TurboMass Software User`s Guide - E

TurboMass Software User`s Guide - E
TurboMass Software
User’s Guide
TurboMass Software User’s Guide
Release History
Part Number
09936767
Release
C
Publication Date
November 2007
For Software Version
5.4
Any comments about the documentation for this product should be addressed to:
User Assistance
PerkinElmer, Inc
710 Bridgeport Avenue
Shelton, Connecticut 06484-4794
U.S.A.
Or emailed to: [email protected]
Notices
The information contained in this document is subject to change without notice.
Except as specifically set forth in its terms and conditions of sale, PerkinElmer makes no
warranty of any kind with regard to this document, including, but not limited to, the
implied warranties of merchantability and fitness for a particular purpose.
PerkinElmer shall not be liable for errors contained herein for incidental consequential
damages in connection with furnishing, performance or use of this material.
Copyright Information
This document contains proprietary information that is protected by copyright.
All rights are reserved. No part of this publication may be reproduced in any form whatsoever
or translated into any language without the prior, written permission of PerkinElmer, Inc.
Copyright © 2007 PerkinElmer, Inc.
Produced in the U.S.A.
Trademarks
Registered names, trademarks, etc. used in this document, even when not specifically
marked as such, are protected by law.
PerkinElmer is a registered trademark of PerkinElmer, Inc.
TurboMass, Clarus 600, and 600 Series LINK Interface are trademarks of PerkinElmer, Inc.
Microsoft is a registered trademark of the Microsoft Corporation.
Windows is a registered trademark of the Microsoft Corporation.
2
Contents
Table of Contents
Table of Contents............................................................................................ 3
Introduction ................................................................................................ 17
Compatibility ................................................................................................ 19
Using this Guide ........................................................................................... 19
Conventions used in this Guide .................................................................... 22
Getting Started............................................................................................ 23
Getting Started.............................................................................................. 25
Starting TurboMass ............................................................................... 25
Quitting TurboMass .............................................................................. 25
General Guidelines for TurboMass Operation ............................................. 26
The TurboMass Top Level Window............................................................. 27
The TurboMass Toolbar ........................................................................ 28
Accessing Menu Commands ................................................................. 28
The TurboMass Desktop .............................................................................. 30
Function Keys........................................................................................ 30
Changing Colors and Fonts ................................................................... 31
TurboMass System Global Parameters ................................................. 34
Processes ............................................................................................... 35
Mass Defect Correction......................................................................... 36
TURBOMASS.INI ................................................................................ 37
Selecting and Viewing Data ......................................................................... 38
The Data Browser.................................................................................. 38
Experimental Record ............................................................................. 41
Deleting a Raw Data File ...................................................................... 42
History Selector..................................................................................... 42
Processed Data Labels........................................................................... 44
Using Explorer to work with Multiple Data Files ................................. 45
Projects .................................................................................................. 47
Directory Structure ................................................................................ 49
Data File Structure................................................................................. 50
Displaying Spectra ................................................................................ 51
Displaying Chromatograms................................................................... 52
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TurboMass Software User’s Guide
The Header Editor ........................................................................................ 54
Determining the Header Information in a TurboMass Window............ 54
Printing Data................................................................................................. 57
Printing a Specific TurboMass Window using the Menu...................... 57
Window Commands ..................................................................................... 58
Getting Help ................................................................................................. 59
The About Box ...................................................................................... 59
TurboMass Overview ................................................................................. 61
Starting TurboMass ............................................................................... 63
Configuring the Inlet System................................................................. 63
Preparing the Mass Spectrometer for use .............................................. 63
Tuning the Mass Spectrometer .............................................................. 64
Calibrating the Mass Scale .................................................................... 64
Setting up your GC................................................................................ 64
Developing your Mass Spectrometer Method ....................................... 64
Setting up your Sample List and acquiring Initial Data ........................ 64
Developing your Quantification Method............................................... 65
Developing your Qualitative Method .................................................... 65
Acquiring Data based on your Method ................................................. 65
Monitoring Data Acquisition................................................................. 65
Manipulating your Data......................................................................... 65
Reporting your Data .............................................................................. 65
Instrument Data Thresholds...................................................................... 67
Selecting the Inlet System ............................................................................ 69
Setting Instrument Data Thresholds ............................................................. 70
Setting Data Thresholding Parameters .................................................. 70
Changing Lab and User Information ............................................................ 78
Communications Status and Diagnostics...................................................... 79
Communications Status ......................................................................... 79
Diagnostics ............................................................................................ 79
Instrument Tuning ..................................................................................... 81
The Tune Page .............................................................................................. 83
The Tune Page Toolbar ................................................................................ 87
Changing Tune Parameter Settings .............................................................. 88
Printing Tune Information ............................................................................ 89
Experimental Record .................................................................................... 90
Saving and Restoring Parameters ................................................................. 91
Saving a Set of Parameters .................................................................... 91
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Contents
Restoring a Saved Set of Parameters..................................................... 92
Modifying the Peak Display ......................................................................... 93
Selecting Peaks...................................................................................... 93
Zooming or Unzooming a Peak............................................................. 94
To Change the Tune Mass, Span or Gain.............................................. 94
UltraTune...................................................................................................... 95
Running Standard UltraTune (DFTPP/BFB) ....................................... 95
Running UltraTune Custom (AutoTune)............................................. 100
To run UltraTune Custom follow this procedure: ............................... 100
Setting Scope Parameters ........................................................................... 105
Changing the Scope Setup................................................................... 105
Changing Inlet Heaters ............................................................................... 106
Setting Gas Controls................................................................................... 107
Turning a Gas On or Off ..................................................................... 107
Vacuum....................................................................................................... 108
Turbomolecular Pump ......................................................................... 108
Pumping Down a Turbomolecular Pump Vacuum System................. 108
Venting the Vacuum System (Turbomolecular Pump) ....................... 108
Diffusion Pump ................................................................................... 108
Pumping Down a Diffusion Pump Vacuum System ........................... 108
Venting the Diffusion Pump Vacuum System .................................... 109
Theory of Diffusion Pump Operation.................................................. 111
Warning Messages in Tune ........................................................................ 112
Resetting the Zero Level............................................................................. 113
Controlling Readbacks ............................................................................... 114
Changing Readback Style.................................................................... 114
Starting an Acquisition from the Tune Page............................................... 115
Mass Calibration....................................................................................... 117
Introduction ................................................................................................ 119
How A Calibration Is Formed .................................................................... 120
Calibration Types ....................................................................................... 121
Overview Of The Calibration Process ........................................................ 122
Check the Instrument Tuning .............................................................. 122
Set the Calibration Parameters ............................................................ 122
Start an Automatic Calibration............................................................ 122
Check the Calibration Report .............................................................. 123
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TurboMass Software User’s Guide
Displaying Calibration Parameters ............................................................. 124
Setting Parameters that Control Calibration ............................................... 125
Setting Automatic Calibration Parameters .......................................... 125
Setting Data Acquisition Parameters................................................... 126
Setting Calibration Parameters ............................................................ 127
Setting Automatic Calibration Check Parameters ............................... 130
Setting Mass Measures ........................................................................ 131
The Calibration Report ............................................................................... 132
Altering the Displayed Range ............................................................. 133
Manually Matching Peaks ................................................................... 133
Other Calibration Facilities......................................................................... 134
Deleting the Instrument Calibration .................................................... 134
Displaying a Calibration Graph........................................................... 134
Displaying a Verification Graph ......................................................... 135
Making a Calibration from a Data File................................................ 135
Recalibrating a Data File ..................................................................... 136
Editing a Reference File ............................................................................. 137
High Mass Calibration................................................................................ 139
Setup Checks ....................................................................................... 139
Tuning and Calibration........................................................................ 140
Manual injection.................................................................................. 141
Saving and Restoring Calibrations ............................................................. 148
Saving a Named Calibration................................................................ 148
Restoring a Saved Calibration ............................................................. 148
GC Control................................................................................................ 151
Overview of TurboMass GC Control ......................................................... 153
The GC Menu ...................................................................................... 154
The GC Status Box.............................................................................. 155
The GC Editor Toolbars and Status Bars ............................................ 155
Configuration.............................................................................................. 156
Configuring TurboMass for GC Control ............................................. 157
Initial GC Configuration...................................................................... 157
Reconfiguring the GC.......................................................................... 162
Changing the Instrument Configuration .............................................. 162
Changing Your Acquisition Port ......................................................... 163
Configuring TurboMass without GC Control ..................................... 164
Configuring User Options ................................................................... 164
Printing Configuration Information..................................................... 167
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Contents
GC Method Editor ...................................................................................... 168
Developing a GC Method.................................................................... 168
Setting Control Options....................................................................... 172
Setting GC Carrier Parameters ............................................................ 177
Entering Descriptive Information for GC Files................................... 185
Printing GC Method Parameters ......................................................... 190
Controlling the GC ..................................................................................... 191
Equilibrating the GC............................................................................ 191
Stopping and Restarting the GC .......................................................... 191
Releasing and Taking Control of the GC ............................................ 192
The Details Window................................................................................... 193
Viewing a Real-Time Plot of GC Detector Data ................................. 193
Viewing Data Acquisition Information ............................................... 194
Viewing Detailed Instrument Information .......................................... 194
Understanding GC Status Messages.................................................... 197
Viewing Error Messages ..................................................................... 199
Working with the GC Interactively ............................................................ 200
Using Hands On .................................................................................. 200
Modifying the Active Method ............................................................. 201
Function List Editor ................................................................................. 203
Introduction ................................................................................................ 205
Function List Editor.................................................................................... 208
Adding a New Function....................................................................... 208
Modifying an Existing Function.......................................................... 208
Removing a Function .......................................................................... 208
Changing a Function's Start and End Times........................................ 208
Setting a Solvent Delay ....................................................................... 209
Saving and Restoring an MS Method.................................................. 210
Setting Up an MS Scan Function ........................................................ 211
Setting Up an SIR Function................................................................. 214
Sample List................................................................................................ 217
Top Level Menu ......................................................................................... 219
The TurboMass Menu Toolbar................................................................... 220
Creating and Editing Sample Lists ............................................................. 223
Adding Sample to the Sample List ...................................................... 231
Sample Injection Information.............................................................. 232
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TurboMass Software User’s Guide
Sample Prep Information..................................................................... 233
Formatting Sample Lists............................................................................. 241
Starting the Analysis................................................................................... 252
Quantify the Data ................................................................................ 254
Report Preview Window ............................................................................ 255
Quantify..................................................................................................... 259
Introduction ................................................................................................ 261
How Does TurboMass Quantify and Report a List of Samples?......... 262
A Step-by-Step Guide to Quantification..................................................... 268
Creating a Sample List ........................................................................ 268
Projects ................................................................................................ 268
Creating a Quantify Method................................................................ 269
Updating of Analyte RTs from Internal Reference ............................. 280
QA/QC Calculations............................................................................ 296
Recoveries ........................................................................................... 297
Matrix Spike/Matrix Spike Duplicate Recovery ................................. 297
Selecting which fields will be displayed in the Quantification
Method Report................................................................................ 302
Starting the Analysis ........................................................................... 304
Quantify the Data ................................................................................ 306
Using the Quantify Window to Examine Results................................ 307
The Summary Window........................................................................ 311
The Graphs Window............................................................................ 316
The Peak List Window ........................................................................ 319
Manually Changing Quantify Results ................................................. 323
Controlling Quantify Reports .............................................................. 328
Files Used During Quantify................................................................. 331
Qualitative Method................................................................................... 335
Introduction to Qualitative Processing ....................................................... 337
Qualitative Integration and Peak Selection ......................................... 337
Qualitative Method Editor .......................................................................... 339
Qualitative Method Editor Toolbar ............................................................ 340
Qualitative Method Editor: General Tab .................................................... 341
The General Tab Fields ....................................................................... 342
Qualitative Method Editor: Search Parameters Tab ................................... 344
The Search Parameter Tab Fields........................................................ 345
Qualitative Method Editor: Library Settings Tab ....................................... 348
The Library Settings Tab..................................................................... 349
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Contents
A Step-by-Step Qualitative Method Summary........................................... 350
1. Create a Sample List........................................................................ 350
2. Create a Qualitative Method............................................................ 351
3. Put the Qualitative Method in the Sample List................................ 356
4. Start the Analysis............................................................................. 357
Data Acquisition ....................................................................................... 361
Starting an Acquisition ............................................................................... 363
Single Sample...................................................................................... 363
Multiple Samples................................................................................. 363
Automated Analysis of Sample List.................................................... 365
Monitoring an Acquisition.......................................................................... 367
GC Status............................................................................................. 367
MS Status ............................................................................................ 367
Chromatogram Real-time Update........................................................ 368
Spectrum Real-time Update ................................................................ 368
Stopping an Acquisition ............................................................................. 370
Automatic Startup....................................................................................... 371
Running Startup................................................................................... 371
Automatic Shutdown .................................................................................. 372
Running Shutdown .............................................................................. 372
Editing the Shutdown parameters........................................................ 372
Running the Auto Control tasks .......................................................... 375
Stopping the Auto Control tasks.......................................................... 375
Saving and Restoring Auto Control Task Lists ................................... 375
Chromatogram.......................................................................................... 377
Getting Started............................................................................................ 379
The Chromatogram Display ....................................................................... 380
The Chromatogram Toolbar ....................................................................... 381
Customizing the Chromatogram Toolbar ............................................ 383
Displaying Chromatograms ........................................................................ 386
Adding or Replacing Chromatogram Traces....................................... 386
Mass Chromatograms.......................................................................... 387
TIC and BPI Chromatograms.............................................................. 389
GC Detector Trace............................................................................... 390
Aligning GC Detector Traces.............................................................. 391
Manipulating the Display ........................................................................... 392
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TurboMass Software User’s Guide
Altering the Horizontal Axis ............................................................... 392
Altering the Range of the Intensity Axis ............................................. 393
Altering the Range of Both Axes ........................................................ 393
Setting Magnified Ranges ................................................................... 393
Setting the Display Range Defaults..................................................... 396
Controlling the Appearance of the Display ......................................... 397
Controlling the Appearance of Peak Labels ........................................ 400
Removing Chromatograms from the Display...................................... 402
Real-time Display of Chromatograms................................................. 403
Changing the Order of Displayed Chromatograms ............................. 403
Adding Text to the Chromatogram Display ........................................ 403
Processing Chromatograms ........................................................................ 405
Processing Multiple Chromatograms .................................................. 405
Subtract................................................................................................ 405
Smoothing Chromatograms and/or Reducing Noise ........................... 409
Integrating Chromatograms................................................................. 411
Editing Detected Peaks........................................................................ 418
Peak Purity .......................................................................................... 420
Signal to Noise .................................................................................... 422
Combine Spectra ................................................................................. 425
Peak Lists.................................................................................................... 427
Creating and Editing a Peak List ......................................................... 427
Reading a Peak List into a Chromatogram.......................................... 428
Automatic Library Searching ..................................................................... 430
Copying to and from the Windows Clipboard............................................ 432
Spectrum.................................................................................................... 435
Getting Started............................................................................................ 437
About the Display................................................................................ 437
The Spectrum Toolbar ................................................................................ 439
Customizing the Spectrum Toolbar..................................................... 440
Displaying Spectra...................................................................................... 443
Adding or Replacing Spectra............................................................... 443
Manipulating the Display ........................................................................... 444
Setting Magnified Ranges ................................................................... 445
Deleting Magnification Ranges........................................................... 446
Changing the Range of Both Axes ...................................................... 447
Restoring the Display .......................................................................... 447
Setting the Display Range Defaults..................................................... 447
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Contents
Displaying a Spectrum as a List .......................................................... 448
Controlling the Appearance of the Display ......................................... 450
Controlling the Appearance of Peak Labels ........................................ 453
Removing Spectra from the Display ................................................... 455
Real-time Display of Spectra............................................................... 456
Changing the Order of Displayed Spectra........................................... 456
Adding Text to the Spectrum Display ................................................. 456
Processing Spectra ...................................................................................... 458
Saving and Recalling Processed Spectra ............................................. 458
Refine .................................................................................................. 459
Combine .............................................................................................. 460
Subtract................................................................................................ 462
Smooth................................................................................................. 463
Center .................................................................................................. 465
Copying to and from the Windows Clipboard............................................ 468
Manipulating Library Spectra..................................................................... 470
Strip and Combine Functions.................................................................. 471
Strip Functions............................................................................................ 473
Creating a Subtracted Data File........................................................... 474
Creating an Enhanced Data File .......................................................... 477
Creating a Clustered Data File ............................................................ 478
Creating a CODA Data File ................................................................ 479
Selecting a Data File to Process .......................................................... 480
Selecting a Data File and Subrange to Process.................................... 481
Selecting a Background Data File ....................................................... 482
Selecting an Output Data File.............................................................. 482
Setting Enhance Datafile Options ....................................................... 484
Setting Cluster Datafile Options.......................................................... 486
Setting Cluster Centroid Options......................................................... 488
Setting CODA Options........................................................................ 489
Stopping a Process............................................................................... 490
Combine Functions..................................................................................... 491
Selecting a Data File and Subrange to Process.................................... 492
Selecting an Output Data File.............................................................. 493
Stopping a Process............................................................................... 494
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TurboMass Software User’s Guide
Library....................................................................................................... 495
TurboMass Library Windows..................................................................... 498
Searching a Library .................................................................................... 499
The Presearch ...................................................................................... 499
The Mainsearch ................................................................................... 499
An Overview of Library Searching ..................................................... 500
Library Toolbar ................................................................................... 501
Selecting Which Libraries to Search ................................................... 502
Selecting a New Search Spectrum....................................................... 504
Setting Library Search Parameters ...................................................... 506
Setting Library Search Filters.............................................................. 508
Starting a Library Search..................................................................... 511
Library Search Results ........................................................................ 511
Automatic Library Search ................................................................... 512
Manipulating the Library Display ....................................................... 514
Printing the Results of a Library Search.............................................. 520
Copying To and From the Windows Clipboard .................................. 521
Refining the Search Spectrum ............................................................. 522
Auto Refine ......................................................................................... 523
Using the Library Compare Process.................................................... 523
Using the Library Subtract Process ..................................................... 523
Creating User Libraries .............................................................................. 525
Creating a User Library ....................................................................... 525
Adding Text Data to the Library Entries ............................................. 527
Indexing a User Library....................................................................... 529
Deleting Library Entries ...................................................................... 530
Using the Library Locator .......................................................................... 532
Map ............................................................................................................ 535
Overview .................................................................................................... 537
How to create a data file map .............................................................. 538
About the Map Display............................................................................... 540
The Map Toolbar ........................................................................................ 541
Selecting a Range to Map from the Data File............................................. 542
Mapping part of the data file of interest .............................................. 542
Manipulating the Display ........................................................................... 544
Changing the Map Intensity Scaling ................................................... 545
Controlling the Appearance of the Display ......................................... 547
Displaying the Status Bar and Toolbar................................................ 549
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Contents
Selecting the Current Cursor Position ................................................. 550
Editing the Header Information........................................................... 550
Printing from Map ...................................................................................... 551
Copying to the Windows Clipboard ........................................................... 552
Molecular Mass Calculator...................................................................... 553
Calculating the Molecular Mass ................................................................. 555
Defining User Elements.............................................................................. 556
Report Method Editor.............................................................................. 557
About the Report Method Editor ................................................................ 559
Report Method Editor Toolbar ................................................................... 561
Selecting an Existing Template .................................................................. 562
Report Template Browser........................................................................... 566
Filtering the Template List ......................................................................... 567
Report Template Filter Toolbar .................................................................. 567
Communiqué Reporting........................................................................... 569
About the Report Method Editor ................................................................ 571
Opening a Report Template........................................................................ 572
Modifying the Template ............................................................................. 575
Adding a Data Object to the Template ................................................ 576
Creating a New Report Template ............................................................... 580
Add a Header and Footer..................................................................... 581
Add Data Objects ................................................................................ 584
Select the Template in the Report Method Editor ............................... 590
Add the Report Method to the Sample List......................................... 595
Environmental Reporting ........................................................................ 597
About Environmental Reporting................................................................. 599
Select Forms Dialog ................................................................................... 601
Report Generation Window........................................................................ 606
Report Generation Window Menu ...................................................... 607
Sample List Tab................................................................................... 613
Form 1 Tab – Organics Analysis Data Sheet ...................................... 616
Form 1 TIC Tab – Tentatively Identified Compounds........................ 619
Form 2 Tab - SMC/Surrogate Compound Recovery........................... 626
Form 3 Tab - Matrix Spike/Matrix Duplicate Recovery ..................... 628
Form 4 Tab - Method Blank Summary ............................................... 630
Form 5 Tab - Instrument Performance Check ..................................... 632
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TurboMass Software User’s Guide
Form 6 Tab – Initial Calibration Data ................................................. 634
Form 7 Tab – Continuing Calibration Check ...................................... 637
Reassign Sample Type ........................................................................ 638
Form 8 Tab – Internal Standard Area and RT Summary .................... 639
Reassign Sample Type ........................................................................ 639
Error Messages and Warnings .................................................................... 641
Error Messages .................................................................................... 641
Warnings ............................................................................................. 643
Form Specific Checks................................................................................. 644
Report Method Usage ................................................................................. 650
Submitter/Task Data Window .................................................................... 652
Submitter/Task List .................................................................................... 654
Report Method Tab..................................................................................... 660
Custom Compounds Tab ............................................................................ 663
Generic TIC Names Dialog ........................................................................ 667
Appendix A TurboMass Security............................................................ 669
TurboMass Security.................................................................................... 671
Security Terminology ................................................................................. 672
Access Rights/Privileges ..................................................................... 672
Administrator....................................................................................... 672
Audit Log ............................................................................................ 672
Group................................................................................................... 672
Group Rights ....................................................................................... 672
Logon Name ........................................................................................ 673
Password.............................................................................................. 673
Right/Privilege..................................................................................... 673
Security Manager ................................................................................ 673
User ..................................................................................................... 673
User Account....................................................................................... 673
Username............................................................................................. 673
Security Model ........................................................................................... 674
Validate Username and Password ....................................................... 674
Access Validation................................................................................ 674
Audit Log Management....................................................................... 674
Security Manager........................................................................................ 675
Security Manager Toolbar................................................................... 678
Setting up an Account Policy .............................................................. 679
Creating a User Account ..................................................................... 680
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Contents
Creating a Group ................................................................................. 682
Managing the Audit Log ..................................................................... 686
Appendix B TurboMass Software Installation ...................................... 691
TurboMass Software Installation................................................................ 693
Installation Summary.................................................................................. 694
Uninstalling the TurboMass Software and all of its Components .............. 694
Installing the TurboMass Software............................................................. 702
Setting the BIOS......................................................................................... 717
Upgrading from v5.3 Using the Service Tool............................................. 719
Installing PerkinElmer NIST/EPA/NIH Library (2002 or 2005) ............... 726
Installing the NIST Library ................................................................. 726
Setting Up NIST 2005 in TurboMass......................................................... 737
Configuring TurboMass for GC Control .................................................... 739
Configuring the GC for the First Time................................................ 739
Appendix C TurboMass Quantify Calculations .................................... 751
TurboMass Quantify Calculations.............................................................. 753
Peak Response ..................................................................................... 753
External ............................................................................................... 753
Internal................................................................................................. 753
Calibration Curve Calculations................................................................... 754
Weighted Calibration Curves .............................................................. 754
Include Origin...................................................................................... 754
Average RF.......................................................................................... 755
Linear................................................................................................... 755
Quadratic and Higher Order Curves.................................................... 756
Peak Amount Calculations ......................................................................... 758
User Specified Response Factor.......................................................... 758
Average RF Calibration Curve............................................................ 758
Linear Calibration Curve..................................................................... 759
Quadratic and Higher Order Calibration Curves................................. 759
User Parameters................................................................................... 759
Calibration Curve Statistics ........................................................................ 760
Coefficient of Determination............................................................... 760
Curve Correlation Coefficient ............................................................. 761
Internal................................................................................................. 761
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TurboMass Software User’s Guide
Appendix D Sample and Compound Table Output Fields .................. 763
Compound and Sample Report Output Fields ............................................ 765
Sample List Data File Structure .......................................................... 770
Appendix E LIMS Import File Example ............................................... 775
Example of a Sample List Import File........................................................ 777
Appendix F Environmental Reporting Calculations............................ 779
About the Calculations ............................................................................... 781
Volatile Organic Compound Analysis........................................................ 782
Water Samples............................................................................................ 782
Soil/Sediment Samples (Low Level) .......................................................... 784
Soil/Sediment Samples (Medium Level).................................................... 785
Semi-Volatile Organic Compound Analysis Water Samples ..................... 787
Soil Sediment Samples ............................................................................... 788
Index .......................................................................................................... 789
Index ........................................................................................................... 791
16
Introduction
1
18
Introduction
Compatibility
This software is designed for use by the following mass spectrometers:
•
Clarus 600 Mass Spectrometer
•
Clarus 560 D Mass Spectrometer
•
Clarus 500 Mass Spectrometers
•
TurboMass Gold Mass Spectrometer
Using this Guide
The TurboMass Software Guide is a step-by-step guide for using TurboMass
software. It is to be used in conjunction with the Hardware Guide and Tutorial
manuals shipped with your instrument when setting up and performing runs on your
Gas Chromatograph/Mass Spectrometer (GC/MS) System.
NOTE: This guide does not cover the installation and configuration of your
computer. If you have purchased a complete system from PerkinElmer,
the computer will already have been configured.
Chapters in this manual cover the following topics:
Chapter 1
Introduction
Software and hardware requirements.
Chapter 2
Getting Started
Navigating the main desktop and performing
some common tasks.
Chapter 3
TurboMass Overview
Overview of the data acquisition process.
Chapter 4
Instrument Data
Thresholds
Preparing the mass spectrometer and setting
instrument thresholds.
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TurboMass Software User’s Guide
20
Chapter 5
Instrument Tuning
Tuning the mass spectrometer.
Chapter 6
Mass Calibration
Calibrating the mass axis.
Chapter 7
Clarus GC Control
Configuring the GC, developing a GC
method, and equilibrating the GC.
Chapter 8
Function List Editor
Managing MS methods.
Chapter 9
Sample List
Developing sample lists for data acquisition.
Chapter 10
Quantify
Entering quantitative parameters into a mass
spectrometry quantification method.
Chapter 11
Qualitative Method
Creating a Qualitative Method to determine
the identity of your sample through the
qualitative processing of sample data.
Chapter 12
Data Acquisition
Initiating and monitoring data acquisition.
Chapter 13
Chromatogram
Working with mass chromatographic data.
Chapter 14
Spectrum
Working with mass spectral data.
Chapter 15
Strip and Combine
Functions
Optimizing data analysis by removing
background noise and combining spectral data.
Chapter 16
Library
Performing library searches.
Chapter 17
Map
Using the 3-D data display Map process.
Chapter 18
Molecular Mass
Calculator
Using the Molecular mass calculator.
Chapter 19
Report Method Editor Enables you to specify a collection of report
definitions (Communiqué report templates
and related parameters) that are printed
sequentially.
Introduction
Chapter 20
Communiqué
Reporting
Using the Report Method Editor and
Communiqué to modify an existing report
template and create a new report template.
Chapter 21
Environmental
Reporting
Using the Environmental Reporting features
to generate reports based on samples collected
with the Clarus GC/MS.
Appendix A
TurboMass Security
Overview of system management procedures.
Appendix B
TurboMass Software
Installation
Reinstalling TurboMass software.
Appendix C
TurboMass Quantify
Calculations
Presents methods for performing quantify
calculations.
Sample and
Compound Table
Output Fields
Defines output table field options and formats.
Appendix E
LIMS Import File
Example
An example of a LIMS file. Sample List for
import.
Appendix F
Environmental
Reporting
Calculations
Equations showing the reporting calculations.
Appendix D
21
TurboMass Software User’s Guide
Conventions used in this Guide
This guide, designed for Windows users, assumes that you will be using a mouse or
similar device to perform TurboMass operations. Many shortcut keys are listed on
the TurboMass menus, and the documentation for your operating system can
provide information about equivalent keyboard procedures. This section discusses
capitalization, terminology, and the way that references are used in this guide.
All menus, commands, and dialog option names appear with initial capital
letters whether or not they are completely capitalized in the user interface.
The names of keyboard items, such as the ENTER key, are capitalized. This
will help you to distinguish these items from narrative or procedural text.
•
Throughout this TurboMass Software Guide, the following terms are used to
refer to program elements and the actions that you perform to carry out tasks:
Click - The term click refers to moving the mouse pointer over a button or
icon on the screen, and depressing the left mouse button.
Select - The term select refers to highlighting an object or item or moving
the cursor focus. Selecting an item prepares it for an action: for example,
when you select text, it appears in reverse video. When you select a dialog
option, you activate the option but the function is not carried out until you
click OK, which closes the dialog and sometimes completes another
operation.
Enter or select - When you use the File Select or File Open dialog to open a
file, the phrase “enter or select” is used to refer to the actions you can take
to open that file. When you enter a filename, you type it in the File Name
field exactly as it exists. When you select a file, you browse for it on your
computer or your network. When you select a file, you will not introduce
typographical errors.
•
22
Unless otherwise indicated, the values in the illustrations of this manual are
examples only. They are not intended to indicate the exact values you will
see or to suggest the values you should use for a specific application.
Getting Started
2
Getting Started
Getting Started
Starting TurboMass
To start TurboMass:
1. Double-click the desktop shortcut
OR
Select from the Windows Start menu.
If TurboMass Security is enabled, the TurboMass Login window opens.
2. Enter your Logon Name and Password, and click OK.
The TurboMass menu bar will appear at the top of the display.
If you have trouble starting TurboMass, there may be a problem with your Security
setup. See Appendix A TurboMass Security on page 669.
Quitting TurboMass
To terminate a TurboMass session, either click the Windows close box, or select
Exit from the TurboMass File menu.
If data acquisition is in progress when you attempt to exit TurboMass, a dialog box
informs you that the data will be lost, and asks if you still want to exit. If you click
Yes, the acquisition stops, and the software shuts down. If you click Cancel, the
acquisition continues.
25
TurboMass Software User’s Guide
General Guidelines for TurboMass Operation
26
•
Always use unique data file names within a Sample List.
•
Always use unique names for Sample Lists before submitting them to a queue
filled with other Sample Lists.
•
Do not stop the Sample List while "General Status" displays "Setting Up".
•
Make sure the GC run is sufficiently long that the autosampler tower has
stopped moving before the run is completed.
•
If the GC autosampler tower has been manually moved, make sure it is returned
to the "home" (full counter-clockwise) position before the next injection.
Getting Started
The TurboMass Top Level Window
The TurboMass top level window includes features that allow you easily navigate
through the software, work with files, and perform tasks.
•
The menu bar includes options that allow you to access a variety of features.
Menus include File, Edit, Samples, Run, View, Quantify, Configure, GC, Tools,
and Help.
•
The GC panel on the left side of the screen includes a run time indicated to
display how long the acquisition method has been running, the Oven
temperature, and status information.
•
The MS panel below the GC pane displays the status of the mass spectrometer.
•
The currently selected Sample List appears in the main pane.
•
An Index of acquisitions queued on the mass spectrometer and the status of each
appears on the lower portion of the screen.
27
TurboMass Software User’s Guide
The TurboMass Toolbar
The TurboMass toolbar includes buttons that allow you to quickly access a variety
of common tasks and options. To see the function of a particular button, roll the
mouse pointer over the icon to display a pop-up definition.
For example, to access Chromatogram from the toolbar, click
.
Accessing Menu Commands
All TurboMass menu commands are accessible by the mouse or keyboard
commands according to standard Windows conventions.
For example, to select the Chromatogram:
Using the mouse
From the TurboMass View menu select Chromatogram
to open the Chromatogram application.
Using the keyboard
Each top level menu will have one underlined letter, the
“key letter.” Press ALT+key letter to display a dropdown menu. For example, press ALT +V followed by C
to open the Chromatogram application.
The sample list pane includes a context-sensitive menu that allows you to apply
options to the queued samples. To access the drop-down menu, right-click an item
or area. The following table describes the options:
28
Pause Process
Right-click an entry and select this option to pause this
entry.
Delete Process
Right-click the Index of an entry and select this option to
delete the entry from the queue.
Getting Started
Priority Process
Right-click the Index of an entry and select this option to
move this entry to the top of the queue.
Refresh Queue
If an entry has been deleted or prioritized, select this
option to refresh the queue display.
Pause Queue
Toggle this option to pause/resume all acquisitions. A
check indicates that a queue has been paused. The
currently running entry will continue to completion, but no
new acquisitions will be started. The queue can also be
paused by selecting Pause Queue from the Run menu or
.
by clicking
Delete Queue
Select this option to delete all entries in the queue.
To open a recently used sample list select one of the four sample lists displayed at
the bottom of the File menu.
29
TurboMass Software User’s Guide
The TurboMass Desktop
TurboMass uses a multiple window system that is controlled from the TurboMass
top level window. Each component of the system, such as the Chromatogram
display or the Tune page, has its own window and menu bar. These frames can be
independently positioned, and in some cases resized. The different components can
be linked together to allow easy data flow around the system. The desktop can be
automated to provide a complete turnkey custom application.
When you exit TurboMass, the current layout is saved in the “Username.ini” file
and reopened the next time you open TurboMass.
Figure 1 A TurboMass multiple window layout
Function Keys
The function keys can be configured by selecting Options from the Sample List
Tools menu. On the Processes tab, use the Add, Edit and Remove buttons to
change function key assignments. By default, the F1 key provides a link between the
30
Getting Started
TurboMass spectrum environment and the optional NIST library search program.
Refer to the NIST manuals for instructions on using the NIST library search
program.
Other function keys can be assigned to other commands (.exe files).
Changing Colors and Fonts
The fonts and colors used to display information in TurboMass windows can be
altered using the Color and Font Editor. To change TurboMass fonts or colors:
1. Select Colors and Fonts from the TurboMass Tools menu.
The Color and Font Editor dialog is displayed.
2. Select a font Type from the list.
The Font or Color button will become active as appropriate.
Select the appropriate button to enter the Font or Color editor
OR
Double-click a Type from the list to open the relevant editor
OR
Double-click a portion of the Current Settings spectrum to open the
relevant editor.
Make any changes required to the fonts or colors of any part of the display.
31
TurboMass Software User’s Guide
Your changes will be reflected in the Current Settings spectrum display.
This gives you the opportunity to experiment before making your changes
permanent.
Click OK to exit the dialog.
Any TurboMass displays affected by these changes are updated.
The Font Editor
The Font Editor allows the font, font style, font size, color, effects, and script to be
changed. Any changes can be viewed in the Sample text.
To change fonts, select the required colors and fonts and click OK.
NOTE: Selecting Cancel in the Colors and Fonts Editor will disregard these changes.
To change data colors, select the required colors and click OK.
NOTE: Selecting Cancel in the Colors and Fonts Editor will disregard these changes.
The color editor displays 48 basic colors:
Data colors 1 to 5 are used for chromatogram traces and spectra.
Data colors 6 to 10 are used in the Map program.
Data color 5 is also used to set the color of tune peaks on the Tune page.
32
Getting Started
To define custom colors:
1. Click Define Custom Colors on the Color dialog.
2. To define the colors, either drag the cross-hairs
and the arrow
OR
Enter Hue, Sat, Lum, Red, Green and Blue values until the required color
appears in the Color|Solid field.
3. Click Add to Custom Colors to display the new color in one of the Custom
colors fields.
4. Click OK.
33
TurboMass Software User’s Guide
TurboMass System Global Parameters
TurboMass includes an option that allows you to specify preferences that apply to a
number of windows. These options are called TurboMass System Global
Parameters. Rather than setting these parameters in every window, you can set the
values at the top level, and the system will automatically apply the settings to all
relevant windows.
To modify the System Global Parameters, select Options from the TurboMass
Tools menu to display the Options dialog.
Display Type
Select either Scan Number or Retention Time. This will determine
the values entered to select spectra in Spectrum and Library.
Axes Labeling
Select Da/e, u/e or m/z to determine axis labeling for spectral displays.
Use Acquired
File as Default
34
Da
represents Daltons (previously called amu).
u
represents atomic mass units.
e
represents the elementary charge.
Select this parameter to always show the last acquired raw file when
the Spectrum or Chromatogram windows are opened.
Getting Started
Processes
External processes can be added to the TurboMass Tools menu. Select Options
from the top level Tools menu, and select the Processes tab.
Adding a process
1. From the Processes tab, click Add to display the Process dialog.
2. Enter the text that will appear on the menu in the Menu text field.
3. Enter the process name and path in the Command field.
will open a browser to help locate the required executable
Clicking
program file.
4. If the process requires arguments that do not change, enter them in the
Arguments field
35
TurboMass Software User’s Guide
OR
For arguments that are variable, select Prompt for arguments.
TurboMass will prompt you to enter the required information.
5. Click OK.
Each process added to the list is assigned an unused function key as a shortcut to
the process. This shortcut key is displayed in the Key field. To run the process,
either select the process from the top level Tools menu or press the shortcut key.
Moving a process
Left-click the Key field of the process to be moved and click
buttons until the process is in the required position.
or
. Move
NOTE: The shortcut keys remain in the same order so some processes may have a new
shortcut key.
Modifying a process
1. Select the key part of the entry you want to modify and click Edit.
2. Modify the required text, and click OK.
Deleting a process
1. Select the key part of the entry you want to delete and click Remove.
2. Click OK.
Mass Defect Correction
Mass Defect Correction can be used to improve quantification and library searches
at higher masses. Select Options from the Sample List Tools menu. In the Options
dialog, select the Mass Defect tab.
36
Getting Started
With the exception of carbon, the masses of all elements are non-integer. Some
elements, such as chlorine and bromine, have larger deviations from integer than
others. These high "mass defects" accumulate, and can cause mass misidentification,
which leads to failed quantification and library searches at higher masses. You can
specify a Mass Defect Correction value to apply a sliding window to correct for this
mass defect. Mass Defect Correction can be applied post-run, so you do not need to
reacquire your data files.
The mass defect is the difference between the exact mass of the ion and that
calculated from the integer nominal masses. The mass defect is used in the mass
calculation as:
nominal mass = (calibrated mass) - (mass defect)*(calibrated mass)
where:
nominal mass is what is displayed in Chromatogram or Spectrum
calibrated mass is from the FC-43 mass calibration file (mass defect n = 0)
mass defect is in mDa/Da
Carbon is defined as 12.00000... Da, or a mass defect of zero. All other elements are
non-integer atomic weight. Chlorine, for example, is 34.9689 Da, a mass defect of
-0.0311 Da, and bromine is 78.9183 Da, a mass defect of 0.0817 Da.
By the time you get to C12Br10, you get 933.1834 Da, instead of (12*12 + 79*10) =
934.0000 Da. The mass defect for this compound is thus -0.8166 Da. The mass
defect correction is:
(934-933.1834)/934 = -8.743e-4 Da/Da = -0.8743 mDa/Da.
By this example, a measured mass of 933.1834 Da gives a nominal mass of:
933.1834 - (-8.743e-4)*933.1834 = 934 Da
TURBOMASS.INI
The TURBOMASS.INI file contains current settings for all TurboMass windows
and dialogs. When a new user logs on, a new Username.ini file is created. Each time
this user uses TurboMass, any changes to the current settings are saved to this file.
37
TurboMass Software User’s Guide
Selecting and Viewing Data
The Data Browser
The Data Browser lets you select a data file to work with. The Data Browser can be
accessed from the TurboMass window by selecting Open Data File from the File
menu, or from Spectrum, Chromatogram and Library programs by clicking
selecting Open from the programs File menu.
or
The data file selected can be in any directory, on any disk, even a network disk. The
browser can access the file header information for every data file and uses it to
display the sample text information and scanning function information for a selected
file. This allows you to find out what is in a data file without having to display a
chromatogram or spectrum.
The Data Browser also holds the history information that gives you access to any
processed data that have been derived from the original data, easing the management
of processed data.
Figure 2 Data Browser
38
Getting Started
Selecting a new raw data file
In the File Name field, enter or select the name of the raw data file you require, and
click OK.
If you do not see the name of the raw data file you want to work with, select a
new drive or directory or double click an item in the File Name list.
Main Data Browser
The main Data Browser appears when you select Open Data File from the
TurboMass top level File menu. It has the following two options that do not appear
on the Spectrum or Chromatogram Data Browsers:
Chromatogram
Automatically opens the Chromatogram window displaying
the chromatogram of the new data file.
Spectrum
Automatically opens the Spectrum window displaying the
spectrum of the new data file.
Spectrum and Chromatogram Data Browsers
The Spectrum and Chromatogram Data Browsers appear when you select File,
Open from Spectrum or Chromatogram. They have the following three parameters
that do not appear on the Main Data Browser:
Add
The data are added to data currently displayed as a new trace in
the same window.
Replace
The data replace existing data in the window.
New
Window
The data are displayed in a new window.
The Chromatogram Data Browser has an additional parameter that does not appear
on the Main Data Browser:
Replace All
If you are displaying the mass chromatograms for a number of
selected masses and select this parameter, when the new file is
opened, traces will be replaced by traces at the same masses.
39
TurboMass Software User’s Guide
Data Browser Fields
File Name
Lists data files in the current directory and provides a field where
you can enter or select a file name. The file name may include a
path if required.
Directories
Lists the directories available on the current drive.
Drives
Lists the other available drives. These will include floppy disk
drives and network drives when available.
Information
Contains information relevant to the currently selected data file.
Sample
Description
Contains the sample description text obtained from the header of
the currently selected data file. This will be information such as
compound name and concentration that was entered during
acquisition.
Acquired
Contains the date and time of data acquisition.
Function
Displays the acquisition function currently selected. The function
description gives the function type, mass range and ionization
mode.
To select a new function, click the arrow at the end of the
Function field and left-click one of the Functions from the list.
History
40
Contains the history of any processing that has been applied to
the current data. When raw data are processed, for example,
Refine or Combine, the processed data can be saved using the
Save Spectrum command from Spectrum File menu. Selecting
History in the History Selector dialog allows you to select one of
the processed data files.
Getting Started
Experimental Record
The Experimental Record window displays information about the selected raw data
file including:
•
Raw data file header information such as sample description, acquisition date
and time.
•
Tune parameters, including the settings on the Tune page and instrument
thresholds.
•
Function description showing the functions set up in the Scan Functions
window.
•
GC information including the GC inlet position, vial number, run log, and GC
method information.
Controlling the Experimental Record display
1. From the Chromatogram Data Brower, click Experiment to open the
Experimental Record window.
2. From the Options menu, select the items that you want to be included in the
experimental record display.
41
TurboMass Software User’s Guide
When an item has been selected, a check mark will appear next to its name. The
options available for inclusion in the experimental record display are Header,
Tune parameters, Function description and GC Information.
Printing a report of the Experimental Record
Select Print Report from the Experimental Record File menu.
The currently displayed Experimental Record will be sent to the printer.
Deleting a Raw Data File
1. Select the data file you want to delete, and click Delete. A dialog will be
displayed asking you to confirm that you want to delete this particular data file.
2. Click Yes to delete the file.
History Selector
The History Selector dialog allows you to access processed data. If no processed
data are selected, raw data is the default. Processes are saved to disk when you select
Save spectrum from the Spectrum File menu.
The History Selector also allows you to delete from disk processes that are no longer
required.
42
Getting Started
Process
History
Displays the full history of all saved processes with the original raw
data at the top of the tree.
Processed data that have been derived from previously processed
data are indented to show the relationship to those data. Each
process is labeled with a unique identification number and the time
and date when it was created. This aids differentiation of similar
processes.
Sample
Displays sample description text obtained from the header of the
currently selected data file.
Function
Displays a description of the currently selected function.
History
Displays full history of the currently selected process. The history
starts with raw data at the top of the list and describes each
processing step made to reach the current process.
OK
Exits the History Selector using the current selection.
Cancel
Exits the History Selector defaulting to the original selection.
Delete
Deletes the currently selected process from the process history tree.
Delete All
Deletes all processes belonging to the current data file function.
Displaying processed data
1. Select the relevant raw data file in the Data Browser dialog, and click History.
The History Selector dialog is displayed.
2. Select the required processed data in the Process History list and click OK.
3. Click OK in the Data Browser dialog.
43
TurboMass Software User’s Guide
Processed Data Labels
Each of the processed data labels is followed by a series of letters and numbers that
describe the parameters used during the process:
Refine
Rf (n1, n2)
Rf
Refined spectrum
n1
Refine window in scans
n2
Refine noise level
Combine
Cm (n1:n2 - (n3:n4 + n5:n6) x n7)
Cm
Combined spectrum
n1:n2
Average range start and end values
n3:n4
First subtract range start and end values
n5:n6
Second subtract range start and end values
n7
Subtract range multiplication factor
Smooth
Sm (s1, [n1x], n2)
Sm
Smoothed data
s1
Smooth type (Mn – mean, Md – median, Sg – Savitsky Golay)
n1x
Number of smooths (not for median)
n2
Smooth window. TurboMass requires that you enter an estimate of the
width of the raw data peak at half height in Daltons, and uses this to
calculate the width of the smoothing window. See “Spectrum” for the
rule used for this calculation.
NR
TurboMass Noise Reduction algorithm
Subtract
44
Sb (n1, n2)
Sb
Spectrum which has been baseline subtracted
n1
Order of polynomial which has been fitted to baseline
n2
Percentage of data points which lie below baseline
Getting Started
Center
Cn (s1, n1, [n2], s2)
Cn
Centered data
s1
Centering method (Top – highest point on peak, Med – Median of peak,
Cen – centroid of peak)
n1
Peak width at half height
n2
Topmost percentage of peak used to calculate centroid
s2
Method used for calculating peak intensities, height ‘Ht’ or Area ‘Ar’
Using Explorer to work with Multiple Data Files
It is also possible to use Windows Explorer to open several TurboMass data files at
once and display them in Chromatogram or Spectrum.
Opening multiple data files
1. Open the Windows Explorer and the TurboMass Chromatogram or Spectrum
application, and arrange the windows so that both are visible.
2. Select the TurboMass data files you want to view in the right side of the
Explorer window.
3. Select more than one file by holding down the CTRL key while you click the
files.
4. Drag the files into the Chromatogram or Spectrum window.
The Chromatogram or Spectrum window will be redisplayed showing the first
function in each data file as a separate trace.
45
TurboMass Software User’s Guide
Deleting multiple data files
1. Open Windows Explorer.
2. Select the TurboMass data folders you want to delete in the right side of the
Explorer window.
3. Select more than one folder by holding down the CTRL key while you click the
folders.
OR
Select a block of folders by clicking the first folder in the block and then
holding down the SHIFT key while you click the last folder in the block.
4. Press DELETE.
You will be prompted to confirm that you want to remove the folder and move
its contents to the Recycle Bin.
5. Click Yes to continue.
NOTE: Files sent to the recycle bin are not deleted from the system; they will stay in the
recycle bin until you delete or retrieve them from there.
46
Getting Started
Projects
TurboMass comes with predefined projects: Default.pro, TutorialQuant.pro,
TutorialReports.pro, Tutorial_VOA.PRO, and Tutorial_SVOA.PRO. All data are
stored in the Default.pro project until a new project has been selected or created.
All TurboMass data storage is organized into projects. When you create a
TurboMass project, TurboMass creates a new directory called ProjectName.pro and
the following sub-directories:
AcquDB
Acquisition settings files
CurvedDB
Quantify calibration curves
Data
Raw data files
MethDB
Quantify methods
PeakDB
Peak lists
QualDB
Environmental Library Search results
SampleDB
Sample lists
Creating a new project
1. Select Project Wizard from the TurboMass File menu.
The Create project dialog is displayed.
2. Enter a Project name and Description in the appropriate fields.
A default location, for saving the project to, appears in the location field.
3. To save the file to a different location, enter a new file name into the field
OR
Click Browse and select a file from the dialog displayed.
4. Click Next to display the next page.
47
TurboMass Software User’s Guide
5. Select one of the following as appropriate: Create New Project, Create Using
Current Project As Template or Create Using Existing Project As Template.
If Create Using Existing Project As Template is selected, the Browse button
will be enabled. Click Browse to display the Select Existing Project dialog
allowing you to select an existing project to use as a template.
If Create Project Using Current or Existing Project is selected, all files in
Acqudb, Methdb, and Sampledb are copied into the new project. If an existing
project is not chosen as a template, all subdirectories will be empty.
6. To create the new project, click Finish.
Clicking Back will display the previous page allowing changes to be made.
Clicking Cancel will discard all information and exit the Project Wizard.
7. For TurboMass to create a new project it must close any TurboMass
applications that are currently running. If you are currently running any of the
TurboMass applications such as Spectrum or Chromatogram, a message will
appear informing you that all applications will be closed. Click Yes to close any
opened applications, and create the new project.
All new data files, sample lists, peak lists, quantify method files and quantify
calibration curves will be saved in this project until you change to a new project.
NOTE: Space on drive C: is normally restricted. It is often useful to place data on other
local drives (for example, d: or e:).
Opening an existing project
1. Select Open Project from the TurboMass File menu.
2. Double-click one of the projects in the list, select one of the projects in the list,
or enter your project name in the Project Name field.
3. Click OK.
For TurboMass to change to a new project it must close any TurboMass
applications that are currently running. If you are currently running any of the
TurboMass such as Spectrum or Chromatogram, a message will appear
informing you that all applications will be closed. Click Yes to close any open
applications and change to the new project.
48
Getting Started
Directory Structure
When TurboMass is opened, a number of default folders will be created that contain
information for different parts of the application. Files can be opened from, and
saved to, any location that you specify, but TurboMass will look in the default
folders for the information first. The following is a list of folders created in the
TurboMass directory.
Folder Name
Type of information stored in the folder
IdenDB
Libraries against which searches are performed. Mass Spectral,
NIST and user defined libraries
Macro
Macros
Ref
Peak list information for Calibration reference files
Shutdown
Shutdown parameters. MS methods for startup before and
shutdown after acquisition
StructDB
Library chemical structures
The following table lists the folders that are created within projects:
Folder Name
Type of information stored in the folder
AcquDB
Acquisition defaults and saved Tune page settings, calibrations
etc. Inlet method files
CurveDB
Quantify calibration curve data
Data
Raw data files
PeakDB
Peak list data
MethDB
Quantify methods
QualDB
Results of Tentatively Identified Compound (TIC) searched
SampleDB
Sample Lists
49
TurboMass Software User’s Guide
When a new version of TurboMass is opened, all files which are no longer
compatible with the new version are stored in subfolders called Old. For example,
old method files will be in the Old subfolder of the MethDB folder. These files can
still be used with older versions of TurboMass but should not be used with the new
version.
Data File Structure
Data acquired from the mass spectrometer are saved into data files on the computer's
hard disk. These data files may contain more than one acquisition function and may also
contain processed data derived from the original raw data, for example, refined spectra.
All files are acquired to the data directory of the current project. For example, if the
file name is specified as test2 then the data files are stored in the directory
c:\TurboMass\currentproject\data\test2.raw. If the data file contains 2 acquisition
functions and 2 sets of processed data then the directory listing will be as follows:
50
_Header.txt
Data file header information
_Funcs.inf
Information on MS functions acquired
_history.inf
Information on how data has been processed
_expment.inf
Experimental record information
_Func001.dat
Data file for first function (one for each function)
_Func001.idx
Data file index for first function
_Func002.dat
Data file for second function
_Func002.idx
Data file index for second function
_inlet.inf
Information on GC method
_proc001.dat
First processed data file (one for each process)
_proc001.idx
Index for first processed data file
_proc002.dat
Second processed data file
_proc002.idx
Index for second processed data file
_Tcfunc1.raw
Data files from the first conventional GC detector
_Tcfunc2.raw
Data files from the second conventional GC detector
Getting Started
Displaying Spectra
There are several ways in which you can ask to display the Spectrum window. The
two most common ways are selecting Spectrum from the TurboMass View menu
or, double-clicking the Chromatogram window.
Selecting a spectrum using the TurboMass menu
Select Spectrum from the View menu.
The spectrum displayed will be the current default spectrum (this will be either
the last spectrum viewed, or, if acquisition is in progress, the last spectrum
acquired). If the Spectrum window is already on display, it becomes the current
window.
If whole rows are selected in the Sample List editor, spectra from the data files
represented by these rows will be displayed.
Selecting a spectrum from Chromatogram
Double-click the chromatogram at the retention time of interest.
The spectrum displayed will be the spectrum closest in retention time to the
position where the mouse was clicked.
If the Spectrum window is already on display, the selected spectrum will either
be added to the one currently on display
OR
Will replace the one currently on display if the
activated
Spectrum toolbar button is
OR
Will be displayed in a new document window of its own if the
toolbar button is activated.
Spectrum
51
TurboMass Software User’s Guide
Removing spectra and document windows
•
To remove a particular spectrum, select the spectrum to make it the currently
selected spectrum, and press DELETE.
Click OK to confirm the deletion.
•
To close a particular Spectrum window, click the Windows close button ⌧.
Displaying Chromatograms
Like spectra, there are several ways in which you can display the Chromatogram
window. The two most common ways are selecting Chromatogram from the
TurboMass View menu, and double-clicking the Spectrum window.
Selecting chromatograms from Chromatogram
Select Chromatogram from the View menu.
The chromatogram displayed will be the Total Ion Current (TIC) chromatogram
of the current data file. If the Chromatogram window is already on display, it
becomes the current window.
If whole rows are selected in the Sample List editor, Chromatograms from the
data files represented by these rows will be displayed.
Selecting chromatograms from Spectrum
Double-click the spectrum at the mass of interest.
The chromatogram displayed will be the mass chromatogram of the mass
indicated by the click.
If the Chromatogram window is already on display, the selected chromatogram
will either be added to the one currently on display.
OR
Will replace the one currently on display if the
button is activated
52
Chromatogram toolbar
Getting Started
OR
Will be displayed in a new window of its own if the
toolbar button is activated.
Chromatogram
Removing chromatogram traces and windows
•
To remove a particular chromatogram trace, select the trace to make it the
currently selected trace, and then press DELETE.
Click OK to confirm the deletion.
•
To close a particular chromatogram window, click the Windows close button ⌧.
53
TurboMass Software User’s Guide
The Header Editor
The Header Editor is used to determine the information displayed in the header for
each of the TurboMass windows.
The TurboMass Window Header can be thought of as a table that has six rows and
three columns. Various pieces of information can be displayed in the header
including your own text. Information can be displayed in lines 1 to 6. On each line,
information can be displayed in three positions: left, center, or right.
There is a graphical representation of the current header at the top of the Header
Editor dialog. The Header Editor areas that are currently displaying information are
shaded in gray. A maximum of eight areas can be used at one time to display header
information.
Determining the Header Information in a TurboMass Window
To open the Header Editor dialog, in most TurboMass windows double-click the
Window header
OR
Select Header from the Display View dialog.
54
Getting Started
Adding information to the displayed header
1. Select the Header areas in which you want to display information.
2. Select the Group, from the drop-down list, that contains the information you
want to append to the displayed header.
3. Select the information required in the Element list.
4. Select the field before which you want to insert the information in the Format
field, and click Add.
To add information at the end of the currently displayed information, select End
and click Add.
5. To add your own text to the header, select [Text] in the Element list and click Add.
The User Text dialog is displayed.
6. Enter your text, and click OK.
Your user text will be shown in the Format list and will be displayed in the
header when you exit the Header Editor dialog.
7. If you want to format the information in the header, select the relevant field in
the Format list, and click Format.
For numeric information you can select the number of Decimal places
displayed in the 0 to 6 range. Some Elements have sub-elements that may be
selected by the Field list.
8. Repeat steps 1 to 6 as required.
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TurboMass Software User’s Guide
A maximum of eight areas can be used at one time to display header
information.
9. Click OK to exit and save the changes.
NOTE: If the information in one of the Header Editor areas overlaps another area, the
overlapped area will not be displayed.
Removing information from the displayed header
1. Select the Header areas from which you want to remove information.
2. To remove a single field, select the information you want to remove in the
Format list and click Remove
OR
To remove all the information from one Header Editor area, select the area and
click Clear
OR
To remove all information from all Header Editor areas, click Clear All.
3. Repeat steps 1 and 2 as required.
4. Click OK to exit and save the changes.
56
Getting Started
Printing Data
TurboMass prints data using the Windows Print Manager, so any printer supported
by your Windows operating system can be used with TurboMass. All of the
operations involved in setting up your printer are controlled by the Windows
Operating System and will be described in the documentation that accompanied that.
The only TurboMass specific procedures to learn are those involved in selecting
what to print.
You can select the printer that you want to use and specify printer setup by using the
Printer Setup command found in each TurboMass File menu, or by using the
Windows Print Manager.
Many of the TurboMass Windows have Print buttons on the toolbar.
Prints current window in portrait format.
Prints current window in landscape format.
Printing a Specific TurboMass Window using the Menu
1. To print a specific TurboMass window using the menu commands, select the
window you want to print, and then select Print from the window's File menu.
2. Select All Windows to print all document windows on display
OR
Select Current Window to print only the currently selected document window.
Trace Width allows you to specify the thickness of the line used to print
chromatogram traces or spectral peaks. Trace Width can be set to values between
1 and 5; a higher value will give a thicker line.
Print All Colors Black will map all the colors in the TurboMass display (except
white) to black. This option is useful when using black and white printers.
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TurboMass Software User’s Guide
Window Commands
Most of the TurboMass program windows have a top level menu command called
Window that contains the standard Windows commands. Those specific to
TurboMass are described here.
Toolbar Button
Menu
Window list
Window list gives a list of available
windows. The currently active
window has a check mark next to its
name. Selecting another window will
make that the currently active
window. In the case of Spectrum and
Chromatogram this becomes a list of
the traces displayed in each window.
Window
Choosing this option causes each
subsequent trace to replace the
currently selected trace.
New Trace
Replace Trace
Window
New Trace
New Window
Window
New Trace
Add Trace
58
Function
Choosing this option causes each
subsequent trace to be displayed in a
new window.
Choosing this option causes each
subsequent trace to be added to those
displayed in the current window.
Getting Started
Getting Help
The TurboMass Help system contains detailed information on how to use
TurboMass. TurboMass Help can be accessed either from the TurboMass top level
menu or from any of the TurboMass program windows.
If you enter Help from the TurboMass top level menu, you will be given a general
index of topics covering the whole of TurboMass. If you enter TurboMass Help
from one of program windows, you will be given help on that particular topic. For
example, if you select Help from Spectrum, you will be given Help on Spectrum.
TurboMass Help also allows you to search for Help on a specific topic or keyword.
For more information on using Windows Help systems, select Using Help from the
Help menu on the TurboMass window. This topic gives detailed instructions on how
to use Windows Help systems.
The About Box
The About TurboMass box gives you information about TurboMass, including the
version number.
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TurboMass Software User’s Guide
60
TurboMass
Overview
3
TurboMass Overview
This chapter describes how to use the TurboMass data acquisition system. It gives
an overview of how to use TurboMass, including mass spectrometer and GC setup,
method development, data acquisition, and data manipulation.
For step-by-step information on how to perform your first run using your mass
spectrometer system, refer to the Clarus GC/MS Tutorial supplied with the mass
spectrometer. In addition, for step-by-step information about how to use TurboMass
with the environmental reporting software, refer to the Clarus GC/MS
Environmental Tutorial, Basic Principles.
Starting TurboMass
1. To start TurboMass, double-click the TurboMass icon
on the Windows
desktop.
If TurboMass Security is enabled, the TurboMass Login dialog displays.
2. Enter your Logon Name and Password.
TurboMass will start and communications with the instrument will be
initialized.
Configuring the Inlet System
1. Choose Select Inlet Interface from the Sample List Configure menu, and select
your interface.
2. Configure your GC as described in Chapter 7: GC Control.
Preparing the Mass Spectrometer for use
Prepare the mass spectrometer for operation as described in the Hardware Guide for
your mass spectrometer.
If in a vented state, it should be pumped down. Then switch it into the Operate
mode.
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TurboMass Software User’s Guide
Tuning the Mass Spectrometer
The instrument must be tuned to obtain the best conditions for ionization according
to the instructions in the Clarus GC/MS Hardware Guide for your mass
spectrometer.
Calibrating the Mass Scale
The mass scale must be correctly calibrated so that the masses reported for
acquired data are correct.
Calibration of the mass scale involves introducing a reference compounds into
the system, acquiring initial data, and then comparing the result with the
expected masses for the reference compound. A calibration curve is produced
and used to correct for any errors in the mass scale.
Setting up your GC
Set up your GC configuration and develop your GC method.
Developing your Mass Spectrometer Method
Develop your mass spectrometer method for scanning the system (referred to as
a Function) in the TurboMass Function List editor.
Setting up your Sample List and acquiring Initial Data
1. Specify your list of samples to be introduced into the system by manual or
autosampler injection.
Your sample list may contain a single sample or a number of samples.
2. Start your run to acquire data to be used for qualitative analysis or quantification
method development.
64
TurboMass Overview
Developing your Quantification Method
If you are performing quantitative analysis, develop a peak detection and location
method based on the results of your initial data acquisition in the TurboMass
Quantify application.
Developing your Qualitative Method
This is a dataset you can specify in each row of the sample list to generate reports
that do not make use of the quantitative results.
Acquiring Data based on your Method
You can now acquire data and apply your quantification method parameters.
Monitoring Data Acquisition
The progress of the acquisition can be monitored by viewing the data acquired in
real time using the Spectrum or Chromatogram displays.
Manipulating your Data
You can manipulate your data in many ways using the TurboMass Chromatogram,
Spectrum, Map, Quantify, Strip, and Combine functions.
Reporting your Data
You can use supplied templates or create your own templates using the
Communiqué template designer to generate custom reports.
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TurboMass Software User’s Guide
66
Instrument Data
Thresholds
4
Instrument Data Thresholds
Selecting the Inlet System
Before you acquire data, you must first configure the software to support the inlet
system selected. You do this from the Select Interface dialog, which displays the
available inlet systems.
1. Choose Select Inlet Interface from the Sample List Configure menu.
The Select Interface dialog is displayed.
2. Select your interface from the displayed list.
The list of inlet options that appears in the Select Interface dialog reflects the
inlet system selected when TurboMass was installed. If, at a later date, you add
a new inlet system or change one of your existing inlets you may need to
reinstall TurboMass to gain access to the control software for the new inlet
system.
3. Select your choice for an inlet to use and click OK to reconfigure the software to
reflect the new inlet system.
The GC Status pane and GC menu item will appear.
NOTE: Once you have selected the inlet system, TurboMass will give you access to the parts
of the acquisition system that are appropriate to the inlet selected and the Tune
application.
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TurboMass Software User’s Guide
Setting Instrument Data Thresholds
TurboMass has Instrument Data Thresholding parameters that allow you to control
how the system preprocesses data before they are sent to the host computer.
Instrument Data Thresholding allows you to specify the type of data you want to
acquire and save to disk, and which type of data you want to discard. Limiting the
amount of data stored on disk can be particularly desirable when acquiring
continuum data and doing long GC runs. Additional options allow you to set the SIR
Baseline Level, the ion counting threshold, spike removal and zero baseline offset.
Setting Data Thresholding Parameters
Changing data thresholding parameters
1. Display the Tune page by clicking
in the MS section of the instrument
status panel in the TurboMass top level window.
2. On the Tune page, select Instrument Threshold Settings from the Options
menu.
The Instrument Threshold Settings dialog appears.
70
Instrument Data Thresholds
3. Set your parameters.
Profile Data
While not normally used for GC/MS, TurboMass can collect
Profile Data that shows mass peak shapes, as in Tune. The
profile data parameters let you control the amount of data
collected during a continuum data acquisition. By default,
TurboMass collects one data point every 16th of a Dalton. For
example, if you scan from mass 50 to mass 1200, you will
collect and save 18,400 data points per scan. As each point
requires 6 bytes of disk space, every scan will require 55.2 KB
of disk space in this example. So, if you use this type of
scanning in conjunction with chromatography, the data file
sizes will grow to be enormous. In addition to the disk space
issue, collecting this amount of data puts a heavy demand on
the computer system, which will ultimately affect the scan
rates at which you can collect data.
The ability to use a threshold with continuum data is therefore
highly desirable as it lets you disregard data that is noise yet
save the complete peak profile for the “real” data. The use of a
threshold with continuum data retains the information in the
data while reducing disk space requirements.
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TurboMass Software User’s Guide
Baseline Level
Raises or lowers the baseline to see more or less noise. The
Baseline Level parameter sets the baseline position above zero
when Ion Counting Threshold is not enabled (set to zero). The
Baseline Level parameter is typically set to 0. If you want the
baseline to appear higher, increase the value of the Baseline Level
parameter.
You can use a negative Baseline Level value to reduce the amount
of noise seen and apply thresholding to 1/16th Dalton type samples.
This thresholding occurs after ion counting and therefore has a less
significant effect.
If you want to see more noise, use a positive value. Do not use a
positive Baseline Level value with Ion Counting Threshold.
Points per
Dalton
Can be set to one of three values, 4, 8 or 16. Selecting 8 points will
allow you to acquire data twice as quickly as selecting 16, and will
(in continuum mode) result in data files that are approximately half
as big as those acquired at 16 points per Dalton (recommended).
Selecting 4 points will allow you to acquire data twice as quickly as
selecting 8, and will result in data files that are approximately half
as big as those acquired at 8 points per Dalton.
Acquiring data at 16 points per Dalton gives the greatest possible
resolution. Acquiring data at 4 points per Dalton gives data with a
smoothed appearance.
Centroid Data
For centroided data (the type most commonly used for GC/MS),
there are two parameters that you can set.
Minimum
centroid
height
The Intensity level below which peaks detected will be ignored.
Typical value is 2. [Should not be changed.]
Minimum
points per
peak
The minimum mass peak width. Typical value is 10 for 16 points
per Dalton. [Should not be changed.]
NOTE: Data is acquired according to the Profile Data criteria before it is centroided.
72
Instrument Data Thresholds
SIR Data - SIR
Baseline Level
Used when Ion Counting Threshold is not enabled (set to
zero). SIR Baseline Level sets the baseline position above
zero. The SIR Baseline Level is typically set to 1. If you
want the baseline to appear higher, increase the SIR
Baseline Level value.
Ion Counting
Threshold
Sets the intensity level below which a data point will be
ignored. The Ion Counting Threshold can be set to values
between 0 and 25; the higher the value, the more data will
be discarded.
NOTE: To disable the Ion Counting Threshold, set the value to zero. If you want to use the
Ion Counting Threshold, a value of 3 is suitable for most data. If you are
performing trace analysis or looking at small isotope peaks, a value from 1 to 3 may
be more appropriate. If you are only looking at large peaks, you can save disk space
with a higher number.
This threshold is applied to all acquisitions, regardless of
scanning mode. It is also the most significant of all of the
data manipulation variables because it is the one applied
first to the raw data.
When an acquisition is started, the instrument performs a
"prescan" with the ion beam turned off so that the electronic
noise level of the acquisition system and its standard
deviation can be measured. The Ion Counting Threshold
level that you enter is multiplied by the standard deviation
of the noise to determine the intensity level to be used. If
you set a value of zero, the intensity level is set so that it sits
in the middle of the noise range, which would mean that
roughly half of the noise data will be acquired. If you set a
value of 20, the threshold would sit well above the noise
level, so very little noise data will be acquired. Conversely,
a value of 1 would place the threshold just above the noise
so almost all of the data will be acquired.
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TurboMass Software User’s Guide
NOTE: When using an Ion Counting Threshold, you
should set the SIR Data SIR Baseline Level and the Profile
Data Baseline Level to zero.
The value of the Ion Counting Threshold should be set
such that background noise is removed without significantly
reducing the intensity of the smallest peaks of interest.
NOTE: When using an Ion Counting Threshold, you should set the Profile Data Baseline
Level and SIR Data SIR Baseline Level to zero.
Profile Data –
Spike
Removal
Spikes are distinguished from real data by the fact that spikes
are very narrow and also very intense when compared to their
immediate neighbors. Data points that are determined to be
spikes are removed by setting the value of each spike data
point to the average of its immediate neighbors.
NOTE: The use of Spike Removal does involve some additional processing during
acquisition, which will reduce the maximum achievable acquisition rates by
approximately 30 %.
Use Spike
Removal
Select this checkbox to perform spike removal during an
acquisition.
NOTE: Spike removal will not be reflected on the Tune page.
Minimum
Spike
Intensity
Sets the intensity threshold below which spikes will be ignored.
Take this value from the Tune page intensities. A very low
intensity signal may include single ion events that can be
combined to produce significant peaks. For this type of data, you
should set the Minimum Spike Intensity to a suitable value such
that these single ion events are not discarded as spikes.
Spike
Percentage
Ratio
Sets the ratio used to determine whether a data point is a spike.
This determination is made by comparing the data point to its
immediate neighbors.
If the Spike Percentage Ratio is set to 30 %, then if at 30 % of
74
Instrument Data Thresholds
its full intensity the data point is still more intense than both its
immediate neighbors, it will be regarded as a spike. To express
this as a ratio, the maximum allowed intensity ratio between a
data point and its immediate neighbors is 3:1.
Spike Percentage Ratio set to 50 % is equivalent to a ratio of 2:1.
Spike Percentage Ratio set to 20 % is equivalent to a ratio of 5:1.
The following examples show the effects of changing the Baseline Level and Ion
Counting Threshold parameters. A series of acquisitions were done using
Heptacosa (FC-43, PTA, PFTBA) and acquiring continuum data. Each data file
contains 18 scans. The data file AB0000 is not thresholded; both Baseline Level
and Ion Counting Threshold were set to zero.
This first example shows the effect of increasing the Baseline Level parameter:
Baseline = 0, Ion Counting = 0
AB0005 2 (0.128) Sm (SG, 2x1.00); Cm (1:18)
576.02
%
Scan EI+
6.61e4
614.06
100
Baseline Level=5
564.03
0
AB0002 2 (0.128) Sm (SG, 2x1.00); Cm (1:18)
Scan EI+
6.03e4
614.06
100
576.02
%
Baseline Level=2
564.03
0
AB0001 4 (0.232) Sm (SG, 2x1.00); Cm (1:18)
Scan EI+
6.19e4
614.06
100
576.02
%
Baseline Level=
564.03
0
AB0000 2 (0.128) Sm (SG, 2x1.00); Cm (1:18)
Scan EI+
4.48e4
614.06
100
576.02
%
Baseline Level=0
564.03
0
Da/e
550 555 560 565 570 575 580 585 590 595 600 605 610 615 620 625 630 635 640 645 650
Figure 3 Effect of increasing Baseline Level on Heptacosa spectrum
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TurboMass Software User’s Guide
The second example shows the effect of increasing the Ion Counting Threshold on
a part of the spectrum that contains only background noise. The bottom trace was
acquired with the Ion Counting Threshold set to zero. For subsequent traces, the
Ion Counting Threshold was set to 1, 2, 4, 6 and 25. As the Ion Counting
Threshold is increased the amount of noise stored is reduced, the normalizing
intensity value at the top right corner of the trace is also reduced.
Baseline = 0, Ion Counting = 25, Data Storage = Compressed
AB0250 2 (0.128) Cm (1:18)
Scan EI+
1
100
%
0
AB0060 2 (0.128) Cm (1:18)
Scan EI+
676
632.03
100
629.36
%
643.54
0
AB0040 2 (0.128) Cm (1:18)
625.63
100
Scan EI+
360
635.89
633.59
639.12
%
0
620
622.71
622
627.99
624
626
628
645.72
640.93
630.11
630
632
634
636
638
640
643.54
642
644
648.51
646
100
629.42 631.35
633.21
625.50
622.46
645.59
638.00
636.63
639.50
643.54
Da/e
650
648
Baseline = 0, Ion Counting = 0
AB0020 4 (0.232) Cm (1:18)
Scan EI+
1.09e3
648.39
646.71
%
0
AB0010 2 (0.128) Cm (1:18)
100
Scan EI+
1.42e3
630.98
626.81
622.52
639.31
636.63
621.46
643.23
648.70
629.67
%
0
AB0000 2 (0.128) Cm (1:18)
100
Scan EI+
648.58 1.65e3
622.52
627.56
636.95
630.54
633.77
643.54
639.81
646.77
645.47
%
0
620
622
624
626
628
630
632
634
636
638
640
642
644
646
648
Da/e
650
Figure 4 Effect of increasing Ion Counting Threshold on noise in Heptacosa
spectrum
The value of the Ion Counting Threshold should be set such that background noise is
removed without significantly reducing the intensity of the smallest peaks of interest.
76
Instrument Data Thresholds
The following example shows the effect of increasing the Ion Counting Threshold
on a part of the spectrum that contains a low intensity peak. As the Ion Counting
Threshold is increased beyond a certain value, the peak becomes narrower, and its
intensity is reduced as the thresholding rejects part of the genuine signal. In this case
an Ion Counting Threshold value of 4 would be suitable.
Baseline = 0, Ion Counting = 4, Data Storage = Compressed
AB0250 2 (0.128) Sm (SG, 2x1.00); Cm (1:18)
Scan EI+
1
100
%
Ion Counting Threshold=25
0
AB0060 2 (0.128) Sm (SG, 2x1.00); Cm (1:18)
614.06
100
Scan EI+
1.53e4
%
Ion Counting Threshold=6
0
AB0040 2 (0.128) Sm (SG, 2x1.00); Cm (1:18)
614.06
100
Scan EI+
2.84e4
%
0
600
Ion Counting Threshold=4
605
610
615
620
625
630
635
640
645
Baseline = 0, Ion Counting = 2, Data Storage = Compressed
AB0020 4 (0.232) Sm (SG, 2x1.00); Cm (1:18)
614.06
100
Da/e
650
Scan EI+
3.98e4
%
Ion Counting Threshold=2
0
AB0010 2 (0.128) Sm (SG, 2x1.00); Cm (1:18)
614.06
100
Scan EI+
4.30e4
%
Ion Counting Threshold=1
0
AB0000 2 (0.128) Sm (SG, 2x1.00); Cm (1:18)
614.06
100
Scan EI+
4.48e4
%
0
600
Ion Counting Threshold=0
605
610
615
620
625
630
635
640
645
Da/e
650
Figure 5 Effect of increasing Ion Counting Threshold on low intensity peak in
Heptacosa spectrum
77
Instrument Data Thresholds
Changing Lab and User Information
TurboMass can save management information with a data file. The information
saved is Laboratory Name, Instrument Identification and User Name. This
information is entered into the Lab and User Info dialog.
This information will be stored with any data that are acquired and can be displayed
as part of the header information of a chromatogram or spectrum when displayed or
printed.
1. On the Tune page select Instrument Name from the Options menu.
The Lab and User Info dialog appears.
2. Make required changes to the information.
3. Click OK.
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Instrument Data Thresholds
Communications Status and Diagnostics
Communications Status
Select Communications Status in the Tune Options menu. A dialog indicates if
the computer and the TurboMass instrument are in communication and the number
of hours. The version of the communications protocol software is displayed.
When done, do not close the System Manager dialog. Click Hide to return to the
Tune page view. Do not click Exit.
Diagnostics
Select Diagnostics Page (a checkmark appears in the menu) in the Tune Options
menu to display diagnostic information for a diffusion pump system or
turbomolecular pump system.
Diffusion Pump - This information includes voltages from the vacuum gauges,
reference voltages (+5 and 0 volts), and the prefilter bias reference voltage.
Turbomolecular Pump - This information includes turbomolecular pump
speed, voltages from the vacuum gauges, reference voltages (+5 and 0 volts),
and the prefilter bias reference voltage.
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TurboMass Software User’s Guide
80
Instrument Tuning
5
Instrument Tuning
The Tune Page
Before acquiring data, you may need to check the tuning conditions of the
instrument, and if necessary, modify one or more of the instrument tuning
parameters. The instrument can be tuned either manually or automatically from the
instrument Tune page.
The Tune page is a configurable paneled display. Use the Ion Mode menu to display
parameters for EI+ (electron ionization), CI+ (positive chemical ionization), or CI(negative chemical ionization), depending on your ionization source. The left side of
the window contains the mass spectrometer tuning parameters. This display will
vary slightly depending if the pump installed in the MS is a turbomolecular or
diffusion pump. The following screen shows a turbomolecular pump system with an
EI+ Source.
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TurboMass Software User’s Guide
The panel displayed in the top right of the window contains the tune peak
information and instrument pressure information.
A toolbar displayed at the top of the Tune page allows you to perform some
common operations with a single click of the appropriate toolbar button.
At the bottom right of the window is the Tune peak display. You can display up to
four masses to tune on. The number of tune peaks displayed is controlled by the four
checkboxes in the top right panel. Any one of the tune peaks can be zoomed so that
it occupies the entire tune peak area. When a tune peak has been zoomed, the
controls for the mass and span for that peak are displayed at the top of the display
window.
Figure 6 Turbomolecular pump Tune Page showing tune and pressure
information
84
Instrument Tuning
Figure 7 Diffusion Pump Tune Page showing Tune and pressure information
The graphic displayed in the panel in the top right shows the vacuum pressure in the
system. It appears as monochromatic for the turbomolecular pump, but for the
diffusion pump it displays the pump status in four colors indicating its operational
status; gray, red, yellow, and green. It also displays the current pressure in the
numerical form. The vacuum gauge colors also correspond to the graphic. The
range colors are:
Red
Atmosphere to 1e-2 Torr
Yellow
1e-2 to 1e-4 Torr
Green
1e-4 to 1e-7 Torr
There is also a Count-Down Timer (Time Remaining) displayed. This displays the
amount of time remaining before the system can be safely vented. The timer starts
counting-down from the time that the diffusion pump heater was turned off.
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TurboMass Software User’s Guide
Displaying the Tune Page
in the MS portion of the instrument status panel in the
Click
TurboMass top level window.
86
Instrument Tuning
The Tune Page Toolbar
The toolbar is displayed at the top of the Tune page and allows you to perform some
common operations with a single click of the appropriate Toolbar button.
Loads the default file.
Selects a data file.
Saves current Tune parameters to disk.
Prints current window in portrait format.
Edits scope settings.
Resets the zero level of the instrument and reinitialize the system.
Activates Standard UltraTune (DFTPP/BFB Tune)
Activates Custom UltraTune (AutoTune)
Pauses an acquisition. Toggles to continue the acquisition. This does
not affect the acquisition of data from samples being processed in the
Sample List.
Stops an acquisition.
Toggles reference gas on/off.
Toggles CI gas on/off.
Accesses online Help.
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TurboMass Software User’s Guide
Changing Tune Parameter Settings
Most of the tuning parameters can be set using the slider bar or by editing a text
field. The tuning parameters can be modified in any of the following ways:
•
by dragging the slider bar using the mouse;
•
by entering a new value directly into the text field;
•
by pressing the left or right keyboard arrows after clicking on the slider bar.
If you change a tune parameter using the slider bar, the value shown in the text field
will update as appropriate.
Other tune parameters only have a text field and can only be changed by direct
typing.
The speed with which the system will respond to changes in parameter settings is
controlled by the speed with which the peak display refreshes. To get the sliders to
be most responsive you should lower the scope scan speed and inter scan time (for
more information, see Setting Scope Parameters on page 105.)
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Instrument Tuning
Printing Tune Information
A report of the tuning parameters can be sent to the printer by clicking
or by
selecting Print from the Tune page File menu. This report contains a copy of the
tune peak information displayed on the screen, along with a record of each
parameter setting.
You can also automatically print out a Tune report by selecting the Print Report
Target Tune option. See UltraTune on page 95.
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TurboMass Software User’s Guide
Experimental Record
Tuning parameters are stored with every data file as part of the experimental record.
The tuning parameters for a particular data file can be viewed or printed from the
Data Browser.
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Instrument Tuning
Saving and Restoring Parameters
Whole sets of instrument tuning parameters can be saved to disk as a named file and
then recalled at a future date.
NOTE: A tune parameter file contains the latest settings for the source parameters for all
supported ionization modes, not just the ionization mode you are currently using.
Tune parameter files also contain settings for the analyzer, and GC inlet line
(transfer line) temperature setpoint.
Saving a Set of Parameters
1. To save the current tune parameters with the existing file name, click
OR
Select Save from the Tune File menu.
To save the current tune parameters with a new file name, select Save As from
the Tune File menu.
2. Enter a new file name under which you want the parameters to be saved, or
alternatively select an existing file from the list displayed.
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3. Click Save.
If the selected file already exists on disk, you will be asked to confirm that you
want to overwrite the existing information. Click Yes to continue or No to enter
a different file name.
NOTE: If you close the Tune page without saving any new settings, the software will prompt
you to save the file.
Restoring a Saved Set of Parameters
1. Click
OR
Select Open from the Tune File menu.
2. Select the tuning parameter set that you want to use, either by entering its name
or by selecting it from the displayed list.
3. Click Open to open the Tune File dialog.
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Instrument Tuning
Modifying the Peak Display
The Tune peak display is modified using either the tune peak parameters, or by
using the mouse directly on the Tune Peak display.
Selecting Peaks
1. Select the number of peaks that you want to display by selecting the appropriate
checkboxes in the top right panel of the Tune page.
For example, if you want to display only the first and second tune peaks, then
select checkboxes 1 and 2, and deselect checkboxes 3 and 4.
2. Click
OR
Select Peak Editor from the Tune Window menu. Then, for each active peak,
select the mass that you want to tune on, the span, and the gain.
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Zooming or Unzooming a Peak
Drag the mouse horizontally or vertically to define a larger area. The peak is
expanded to fill this area.
OR
Click
to return the peak to the original size.
To Change the Tune Mass, Span or Gain
•
Edit the mass, span or gain in the text fields above the peak display.
•
Double-clicking on the borders above or below the peak will increase or
decrease the peak intensity by a factor of 2.
NOTE: The span specifies a small mass window applied centrally about the highlighted
mass. When specifying a mass that is close to either the low mass limit (1) or high
mass limit (1205), you must first enter a span that does not force the mass outside of
the mass limits. For example, to specify a mass of 2, you must first enter a span of 2
or less.
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Instrument Tuning
UltraTune
TurboMass can automatically tune the mass spectrometer by using UltraTune with
an EI ion source. UltraTune ramps the settings for the tuning parameters until they
are optimized to give good intensity, resolution, and peak shape.
Reference Gas and Filament Control
Since reference gas is always required for the UltraTune process, the TurboMass
software will assume control for switching the flow on and off.
Tune History
A ‘tune history’ file is maintained that records the tune parameters following a
successful UltraTune. It is saved in an ASCII, comma–separated format, with one
tune record per line. The file is located in the main ‘TurboMass’ directory. Each
new successful UltraTune will append a new line to the end of the file.
If the tune history file does not exist when a record comes to be written to it, it will
be created. The first line of the file will contain names for each field in the record,
which may be used as column headings when the data are imported into Excel. The
tune history file is named “UltraTuneHistory.CSV” and it is located in the primary
TurboMass path (C:\TurboMass\).
NOTE: The goal of Standard UltraTune is to give a satisfactory, library-searchable
spectrum, not to achieve maximum sensitivity.
Running Standard UltraTune (DFTPP/BFB)
NOTE: If you cancel UltraTune during the data acquisition phase, the instrument will be
restored to the state it was in prior to the start of UltraTune (i.e., previous tune
parameters, reference gas off, etc).
1. Click
OR
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Select UltraTune, followed by Standard (DFTPP/BFB) from the Tune page
Options menu.
You will hear a click when the reference gas solenoid valve opens and
UltraTune begins. The first page of UltraTune is displayed.
2. Click Setup to display the UltraTune Setup dialog.
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Instrument Tuning
3. Select your After UltraTune settings:
Print Report - Automatically prints a tune report after a successful
UltraTune.
Save Alternate Tune Files - Saves the top three UltraTune result sets as tune
files rather than just the top one.
Prompt for Recalibration - Prompts you to perform a mass calibration after
a successful UltraTune.
Evacuate Reference Gas - Automatically pumps out the reference gas
following UltraTune
4. Set the Final Multiplier Setting.
User Set (V) - Check this box if following UltraTune, you want to set the
PMT voltage to the value you enter in the field.
5. When you are satisfied with the UltraTune Setup parameters, choose OK to
exit this dialog.
6. Choose Start to start UltraTune and the following occurs:
•
If the source is not at the set temperature (within normal tolerance) then
the message “Waiting for the source temperature to equilibrate” is
displayed in the UltraTune Status dialog.
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•
Once the source reaches the set temperature, if Operate is Off,
Reference Gas is Off or Pump Out Reference Gas in On, the message
“Waiting for Reference Gas pressure to stabilize” will be displayed.
•
If Pump Out Reference Gas is On it will be turned off, followed by a
delay of 50 seconds.
•
If Reference Gas is Off it will be turned on, followed by a delay of 100
seconds. The “Waiting for Reference Gas pressure to stabilize” message
will then be removed.
•
If Operate is Off it will be turned on, followed by a delay of 5 seconds.
A check is then made to determine if the Electron Energy and Trap
Emission current are at the set values (within ±7 and ±10 respectively).
If either (or both) readbacks are out of tolerance the error message is
displayed is “Electron energy not at the set value.” And/or “Trap
emission current not at the set value” and the UltraTune procedure
stopped.
The UltraTune status dialog is displayed.
The status dialog displays the part of the tuning process that is currently
occurring. The UltraTune status bar is updated to show the progress of
UltraTune.
7. When UltraTune has finished, the UltraTune completed message is displayed.
Click OK.
The tuning parameters determined by UltraTune will be saved to the current
tune parameter file.
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Instrument Tuning
If the Prompt for Recalibration box was checked in the UltraTune Setup dialog, you
will begin to mass calibrate. Refer to Chapter 6, Mass calibration for details.
If you selected Evacuate reference Gas in the UltraTune Setup dialog, UltraTune
turns off the Reference Gas and the pumps out the reference gas.
NOTE: You can verify if it has been done by selecting Reference Gas On from the Gas
menu to remove the check mark ( ) and selecting Pump Out Reference Gas
from the Gas menu and wait about one minute as the reference gas is pumped
away. Select Pump Out Reference Gas from the Gas menu again to remove the
check mark and stop pumping the gas.
8. Select Exit from the File menu.
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Running UltraTune Custom (AutoTune)
TurboMass can automatically tune the mass spectrometer using UltraTune Custom
with an EI ion source. UltraTune Custom ramps the settings for the tuning
parameters until they are optimized to give good intensity, resolution, and peak
shape.
NOTE: The goal of UltraTune Custom is to give a satisfactory, library-searchable
spectrum, not to achieve maximum sensitivity.
To run UltraTune Custom follow this procedure:
1. Turn on the Reference Gas by clicking on
from the Gas menu.
or selecting Reference Gas On
2. Turn on Operate.
3. Click
OR
Select UltraTune, followed by Custom (AutoTune) from the Tune page
Options menu.
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Instrument Tuning
NOTE: The instrument must be in Operate mode and the reference gas must be on before
you can run UltraTune Custom (AutoTune).
4. Click Setup to display the AutoTune Setup dialog and customize your Tune
parameters.
Selects the low mass
and high mass
calibration range.
Prints a report of the
AutoTune results at the
completion of the
AutoTune.
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The default setup parameters (FWHM = 0.6 and masses 69 and 502) for EI
UltraTune are suitable for tuning with Heptacosa. There is no need to alter the
Tune Mass or Peak Width parameters if you are using Heptacosa.
The Level of AutoTune performed can be selected as Maintenance or Full.
A Full AutoTune starts from a default set of tuning parameters, but uses
your current settings for the Inlet Line Temperature and Source
Temperature.
In a Maintenance AutoTune, the software uses your current settings for
Inlet Line Temperature, Source Temperature, Electron Energy and Source
Emission.
A Maintenance AutoTune can be quicker than a Full AutoTune, but
should only be performed if the instrument is reasonably well tuned
already. If the current tuning is too poor, AutoTune will give an error and
ask you to perform a Full AutoTune.
The Tune Masses parameters set a Low Mass and High Mass that will be used
to tune on.
The Peak Width at Half Height parameters set the peak width at half height for
the Low and High Masses being monitored. Typical values are 0.6 for both, but
applications requiring higher mass resolution (for example, the environmental
BFB tune) or more accurate isotope ratios may need higher resolution (for
example, 0.55 or 0.50).
SIR sensitivity may be improved by selecting a number larger that 0.6, but care
must be taken to avoid nearby eluting peaks with ions one m/z above or below
the target ion.
5. When you are satisfied with the AutoTune setup parameters, click OK to exit.
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Instrument Tuning
6. Click Start to start AutoTune.
The AutoTune status bar is updated to show the progress of AutoTune.
AutoTune has sixteen stages. The AutoTune stages are listed here.
1
Checking Instrument Conditions
AutoTune checks that Tune page readbacks
are within acceptable tolerance.
2
Stopping Tune Peak Acquisition
Stops the display of peaks in Tune.
3
Initializing AutoTune
Sets the initial voltages for AutoTune.
4
Acquiring Data
5
Tuning Focus Lenses
Optimizes Lens 1 and Lens 2 voltages.
Values of lenses are ramped to see where the
low mass peak intensity maximizes.
6
Tuning Ion Energy
Iteratively ramps values for ion energy,
repeller, and ion energy ramp for best
sensitivity consistent with lowest values for
these parameters.
7
Tuning Repeller
8
Tuning Ion Energy Ramp
9
Tuning Ion Energy
10
Tuning Repeller
11
Tuning Ion Energy Ramp
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12
Tuning Focus Lenses
Values of lenses are ramped over a narrower
range using the values determined in stage 4
to see where the high mass peak intensity
maximizes.
13
Tuning Resolution Settings
Adjusts peak width at half height and height
of valley between main and isotope peaks to
achieve target values.
14
Adjusting Multiplier
The value of multiplier ramped until the low
mass peak intensity is about 90% of full
scale.
15
AutoTune Finishing
Updates Tune file parameters.
16
AutoTune Completed
When AutoTune has finished, it displays a status message indicating that
AutoTune has been successfully completed.
The tuning parameters determined by AutoTune will be saved to the current
tune parameter file.
7. Click the
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box to close the dialog and return to Tune.
Instrument Tuning
Setting Scope Parameters
Various parameters can be set to control the peak display. You can control the speed
at which the display is refreshed.
Changing the Scope Setup
1. Click
OR
Select Scope Parameters from the Tune page Options menu.
2. Make any required changes to the settings.
3. Click OK.
Scan Time
and Inter
Scan Time
Controls the speed with which the Tune peak display is updated. The
tuning system will behave more responsively if the scan time and
inter scan time are short.
The following options are available by right-clicking on the spectrum plot on the
Tune page.
Grid
Select Horizontal and/or Vertical (a check mark appears in the menu)
to display a horizontal grid and/or vertical grid on the peak display.
Intensity
When this parameter is set to Relative Intensity, the percentage
intensity of the base peak in the active tune segment window is
displayed. When this parameter is set to Absolute Intensity the
absolute intensity of the base peak in the active tune segment window
is displayed. When this parameter is set to Normalize, all peaks are
rescaled relative to the largest peak.
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Changing Inlet Heaters
The GC Interface Inlet Line Temperature setting on the Tune page is used to set the
temperature of the interface between the gas chromatograph and the mass
spectrometer.
Enter the desired temperature (ºC) in the text field.
NOTE: When the Source Temperature or Inlet Line Temperature is first raised after the
mass spectrometer has been vented, there is often a pressure surge from desorbed
air and water. Operate should be kept off until the vacuum gauge shows this surge
has passed.
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Instrument Tuning
Setting Gas Controls
The Gas menu on the Tune page lets you turn gases on or off.
Turning a Gas On or Off
Click the appropriate toolbar button (Ref Gas
or CI Gas
)
OR
Select the required gas from the Tune Gas menu.
If the gas was previously turned off, it will now be turned on. A check mark will
appear next to a gas if it is turned on.
Pump Out Reference Gas should be used for about one minute prior to the first
time Reference gas is selected, to remove the air from the vial. It should also be used
whenever the vial is refilled.
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Vacuum
The mass spectrometer's vacuum system is controlled from the Tune page. Be sure that
this is done in accordance with the information provided in your Mass Spectrometry
Hardware Guide. The following procedures describe a Turbomolecular Pump system
and a Diffusion Pump system.
Turbomolecular Pump
Pumping Down a Turbomolecular Pump Vacuum System
Select Pump/Vacuum System On from the Options menu on the Tune page.
The menu name will change from Pump/Vacuum System On to
Vent/Vacuum System Off, and the system will begin its pump-down
sequence. Once OPERATE is enabled, it remains enabled unless the
Vent/Vacuum System Off command is given.
Venting the Vacuum System (Turbomolecular Pump)
1. Cool the source and inlet to below 100 °C.
2. Select Vent/Vacuum System Off from the Options menu on the Tune
page, and confirm that you want to vent the system.
Diffusion Pump
Pumping Down a Diffusion Pump Vacuum System
Select Pump/Vacuum System On from the Options menu on the Tune
page.
The menu name will change from Pump/Vacuum System On to
Vent/Vacuum System Off, the roughing pump turns on and waits for the
system to achieve a minimum vacuum level of 3.7 x 10-1 Torr. Once that
vacuum level has been achieved, a relay turns on the diffusion pump heater and
a countdown timer starts. A typical vacuum level will stay constant until the
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Instrument Tuning
count down timer reaches 10 minutes, the vacuum drops quickly to 1 x 10-4
Torr, and continue to 4 x 10-5 Torr before the countdown timer ends.
When the timer reaches 5 minutes, the software will enable OPERATE. If
you attempt to use the system prior to achieving a safe operating vacuum
(5 x 10-5 Torr), a warning message will appear.
CAUTION
The software will not prohibit the use of the system prior to reaching
the desired vacuum. The software will monitor the vacuum gauge
pressure to determine when the system has reached the proper
operating vacuum (5 x 10-5 Torr).
Once OPERATE is enabled, it remains enabled unless the Vent/Vacuum
System Off command is given.
Venting the Diffusion Pump Vacuum System
1. Cool the transfer line and source to under 100 °C.
2. Select Vent/Vacuum System Off from the Options menu on the Tune
page, and confirm that you want to vent the system.
The system will start its automatic venting sequence. The software monitors
the temperature of the source and the inlet. When the temperatures of both
of the source and the inlet are less than 100 °C, the software turns off the
diffusion pump heater and starts a 20 minute countdown timer.
During the cooling down period, the countdown timer will display the time
remaining in minutes and seconds. When the count down timer reaches 0,
the backing pump turns off.
Once the backing pump has been turned off, the software will display a
message indicating that the system is now cool enough to vent. The message
also reminds you to turn off the carrier gas.
3. Vent the mass spectrometer by pressing the push-button behind the front
door of the mass spectrometer. It will lock in the pressed-in position and
turn red indicating the vent valve is open.
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CAUTION
If you try to vent a hot diffusion system, oxidation of the pump oil may
occur and cause oil to enter the analyzer tub which will damage the
mass spectrometer.
The depressed push button vent switch lights when the diffusion pump cools to the
proper temperature to allow venting. Before clicking on Pump/Vacuum System
On, make sure the vent switch is closed (i.e., the push button is out and the light is
off)
Never vent when:
• The diffusion pump is hot
• During the 20 minute cool-down period
Always check that the front panel vent button is out and the lamp is off when
starting to pump the system down.
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Instrument Tuning
NOTE: The vent valve will operate if the vent switch is pushed in (on) before the diffusion
pump becomes hot. This includes the first few minutes of Pump/Vacuum System
On. Venting during this period may cause a vacuum fault to occur and risk back
streaming the diffusion oil into the analyzer. It is a good reminder to leave the
instrument front door open whenever the push button switch is pushed in (on).
NOTE: When the diffusion pump is hot, the vent switch is deactivated and will not light
when pushed in (on). Since the vent switch may be left in the depressed position at
any time, you should be careful to avoid closing the instrument door and forgetting
that the push button switch is pushed in. (When the diffusion pump cools, the
pushed in push button switch will light and automatically vent the system).
Theory of Diffusion Pump Operation
The Clarus 600 D MS and the Clarus 560 D MS have an air-cooled oil diffusion
pump. This pump is only available for Electrical Ionization (EI) operation.
1. Pump fluid is heated in the base of the pump to produce a vapor which passes
through the interior of the jet assembly and emerges from the jets as highvelocity vapor streams.
2. These streams entrain eluting compounds and carrier gas, condense on the
cooled pump body wall, and drain into the base of the pump for recirculation.
The entrained compounds are transferred to the fore pump.
3. Vacuum venting is controlled by a front panel pushbutton toggle switch and
a pump temperature sensing switch. The pump temperature sensor prevents
venting when the pump is hot, even if the front panel button is pushed.
4. Depressing the pushbutton opens the vent and illuminates the switch red if
the pump is cold. The vent will not open and the switch will not light when
the pump is hot. When the button is out, the vent is closed and the light is
off.
The temperature sensing switch prevents operation of the vent valve when
the pump is hot. Venting a hot diffusion system may oxidize the pump oil
and cause oil to enter the analyzer tub.
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Warning Messages in Tune
Select Warnings from the Options menu to display a dialog containing a list of
optional warning messages. In most cases, these warnings should all be selected.
You can select the following warning messages when exiting Tune under the
following conditions:
•
The filament on.
•
The reference gas on.
•
The Pump out reference gas on.
•
The CI gas on.
You can select the following warning messages when venting the mass spectrometer
with:
112
•
a hot ion source (> 100 °C);
•
a hot GC transfer line (> 100 °C).
Instrument Tuning
Resetting the Zero Level
The Reinitialize command measures the position of the noise signal so that any
baseline offset caused by the electronics or instrumentation can be compensated for.
It is advisable to reset the zero level whenever the value of the multiplier voltage is
changed.
You can reposition the zero level (or Baseline) by clicking
.
OR
Select Reinitialize from the Options menu on the Tune page.
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Controlling Readbacks
TurboMass allows you to choose how system readbacks will be displayed on the
Tune page. You can ask for readbacks to be displayed continuously, never, or only
when they differ from their associated set points by more than 10 %.
Note that a number of the readbacks are for diagnostic purposes only and thus do not
need to be very precise. Their function is to indicate if the voltage is present or not.
The acceptable variation between the set value and the readback value will vary
depending on the particular tune parameter. If you are concerned about the values,
contact your local service office for advice.
Changing Readback Style
1. Select Readbacks from the Tune Options menu.
2. Select the readback style required.
Selecting Always On will always display readbacks. Selecting Out of Range
will display readbacks when they differ from their associated set points by more
than 10 %.
3. Click OK.
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Instrument Tuning
Starting an Acquisition from the Tune Page
The easiest way to acquire data for a sample is to acquire it directly from the Tune
page. You cannot use inlet programs (for example, GC methods) from the Tune
page, acquire analog data or acquire multiple sample sequences, but you can start
and stop acquisitions and control most of the scanning parameters.
1. Select Acquire from the Tune Window menu
OR
Click Acquire at the bottom of the Tune page.
2. Make any required changes to the settings.
Data File
Name
The name of the data file to which acquired data will be
written. The filename can be up to 128 characters. If the file
exists, you will be asked if you want to overwrite it.
Text
A text area that is used to enter the sample description. The
description can be displayed on any output of the acquired
data and has a maximum length of 80 characters.
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Data
Format
Start Mass
The type of data that will be collected and stored on disk. It
can be Centroid, Continuum or MCA.
Specifies the mass at which the scan will start. The Start
Mass must be lower than the End Mass.
End Mass
Specifies the mass at which the scan will stop.
Run
Duration
Length of the acquisition, measured in minutes.
Scan Time
Specifies the duration of each scan in seconds.
Inter Scan
Time
Specifies the time in seconds between a scan finishing and
the next one starting. During this period data is stored on the
PC.
3. Click Start acquisition.
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Mass Calibration
6
Mass Calibration
Introduction
TurboMass provides a fully automated facility for calibrating the mass scale of an
instrument.
To open the main calibration dialog, select Calibrate Instrument from the
Calibration menu on the Tune page.
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How A Calibration Is Formed
A mass spectrum of a reference compound (a calibration file) is acquired and
matched against a table of the expected masses of the peaks in the reference
compound that are stored as a reference file. Each peak in the reference file is
matched to a corresponding peak in the calibration file. The mass differences
between the reference peaks and calibration peaks are the calibration points. A
calibration curve is fitted through the calibration points.
The vertical distance of each calibration point from the curve is calculated. This
distance represents the remaining (or residual) mass difference after calibration.
The standard deviation of the residuals is also calculated. This number is the best
single indication of the accuracy of the calibration.
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Mass Calibration
Calibration Types
TurboMass requires up to three calibration curves:
•
A static calibration is used to accurately 'park' the quadrupole mass analyzer on
a specific mass of interest (in Tuning and SIR, for example).
•
A scanning calibration enables peaks acquired in a scanning acquisition to be
mass measured accurately.
•
A scan speed compensation calibration compensates for 'lag time' in the system
when the instrument is scanned rapidly.
A separate mass spectrum of the reference compound is acquired for each selected
calibration type.
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Overview Of The Calibration Process
Check the Instrument Tuning
The mass spectrometer should be in Operate mode with Reference gas on. Check
that the peak shape and intensities are correct.
Set the Calibration Parameters
1. Select the appropriate reference file for the calibration reference sample that you
are going to use (typically HEPTA.REF).
2. If required, set the automatic calibration checking parameters in the AutoCal
Check Parameters dialog.
These parameters control how closely the recorded data must match the
reference file.
3. If required, set the Peak Match and Curve Fit parameters in the Calibration
Parameters dialog.
These parameters control the location of reference peaks in a calibration
spectrum, and the drawing of a calibration curve to correct the resulting mass
differences.
4. If you are calibrating continuum or MCA data types you should set the Mass
Measure parameters.
These parameters control peak detection in continuum and MCA data. There is
no need to set these parameters if you are using centroided acquisition, the
typical GC/MS data acquisition mode.
Start an Automatic Calibration
1. From the main Calibrate dialog, click Calibrate/Start Acquisition to open the
Automatic Calibration dialog.
2. Select the types of calibration you want to perform.
Usually, all checkboxes should be selected.
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Mass Calibration
3. Select Acquire & Calibrate to perform automatic calibration.
4. Optionally, select Acquire & Verify.
5. Select Print Report if you want a printed calibration report.
6. Set the data Acquisition Parameters if your mass range or data acquisition
rates are not covered by the defaults.
7. Click OK.
Check the Calibration Report
Examine the calibration report and display the calibration graphs, if necessary, to
satisfy yourself that the calibration is satisfactory.
A good calibration will cover your data acquisition mass range and have a small
(typically less than ± 0.3) error for each calibration mass.
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Displaying Calibration Parameters
The Calibration dialog displays calibration status information, including calibrated
mass range and scan speeds, and the time and date of the last calibration.
1. To open the Calibration dialog, select Calibrate Instrument from the
Calibration menu on the Tune page.
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Mass Calibration
Setting Parameters that Control Calibration
Use the following procedures to set calibration parameters.
Setting Automatic Calibration Parameters
1. Click
in the Calibration dialog to open the Automatic Calibration dialog.
2. Select Static Calibration, Scanning Calibration, or Scan Speed Compensation, as
appropriate.
Usually all checkboxes should be selected.
3. Optionally, select Acquire & Verify to acquire a calibrated mass spectrum of the
reference compound.
4. To automatically print a report of the calibration when the calibration is
complete, select Print Report.
If you choose not to print the report at this stage, you can always print it from
the calibration curve display later. The report contains pictures of the calibration
curves produced, along with calibration statistics such as standard deviation.
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Setting Data Acquisition Parameters
1. Click Acquisition Parameters in the Automatic Calibration dialog to open the
Calibration Acquisition Setup dialog.
2. Specify the acquisition parameters.
Scan From and
Scan To
Specify the scan range for each calibration type.
Run Duration
Specifies the data acquisition time for each calibration
data file. It is usually calculated by the software.
Data Type
Specifies whether data will be acquired in centroid,
continuum or MCA mode. It is recommended that the
calibration uses the same data type as the sample data
you will be acquiring. GC/MS uses the Centroid type
almost exclusively.
3. To acquire data for static calibration, the portion of the mass scale immediately
around each reference peak is scanned.
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Mass Calibration
Static Span
Specifies the distance to be scanned either side of the
reference peak. Typically set to 4.
Static Dwell
Specifies the time taken to scan the static span range.
Typically set to 0.1.
4. To acquire data for scanning calibration, the mass scale is scanned over the
selected range, in a time specified by the Slow Scan Time parameter. This
should be as long, or longer than the slowest rate you will use.
Typically set to 2.
5. To acquire data for the Scan Speed compensation calibration, the mass scale is
also scanned over the selected range, in a time specified by the Fast Scan Time
parameter. This should be as fast, or faster than the fastest scan rate you will use.
Typically set to 0.1.
Inter Scan Delay specifies the time between one scan ending and the next scan
starting. If this is too short (typically less than 0.05 sec), the recorded spectra
may be incomplete depending upon mass range. Typically set to 0.1.
Very fast scanning over wide mass ranges may require verifying that all data are
properly written to the data file. The mass calibration should also be carefully
checked.
6. To reset all parameters to their default values, click Default.
Setting Calibration Parameters
1. Select Calibrate Instrument from the Tune Calibration menu to open the
Calibration dialog.
2. Select Calibration Parameters from the Calibration Edit menu to open the
Calibration Parameters dialog.
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TurboMass Software User’s Guide
3. Specify the Peak Match, Curve Fit, and Display calibration parameters.
128
Perform
auto peak
matching
Select this to turn on auto peak matching. When unselected,
automatic peak matching is turned off.
Peak
window
Specifies the maximum mass difference between the
remaining reference peaks and the expected position of the
corresponding peaks in the acquired spectrum. Normal
operating range for the Peak Window parameter is 0.3 to
1.5 Da. It may need to be large (for example, 4) for very
high mass work.
Initial error
The first reference peak to be matched is chosen to be close
to the center of the calibration mass range. The Initial error
parameter specifies the maximum mass difference between
this reference peak and the corresponding peak in the
acquired spectrum. Normal operating range for the Initial
error parameter is 0.5 to 2.0 Da.
Mass Calibration
Intensity
threshold
Any peak in the acquired spectrum with intensity less than the
specified Intensity threshold will not be used to form the
calibration curve. The threshold is specified as a percentage of
the most intense peak in the acquired spectrum. Normal
operating range for the Intensity threshold parameter is 0 to 5
%.
Polynomial
order
When each peak in the reference spectrum has been matched
with a corresponding peak in the acquired spectrum, the mass
difference
acquired mass - reference mass
is calculated for each pair of peaks. These mass differences are
plotted as points on a graph. Each data point has the mass of the
acquired peak as its x coordinate and the above mass difference
as its y coordinate. A smooth curve is drawn through the points.
The Polynomial order parameter controls the type of curve that
is drawn and can be set to any value between 1 and 5. If
Polynomial order = 1, a straight line is drawn through the points.
If Polynomial order = 2, a quadratic curve is drawn through the
points. If Polynomial order = 3, a cubic curve is used.
For a typical EI calibration where the mass range calibrated
starts below 100 amu and extends up to 650 amu, the
recommended setting for the Polynomial order parameter is 4.
Intensity
weighting
If selected, the curve fit is weighted toward the points
representing the more intense acquired peaks. The weight of
each point is proportional to the square root of the intensity of
the acquired peak.
Calibrate
display
If selected, enables calibration of the peaks in the top (raw file)
graph. This feature allows selection of one peak at a time, with
the display being recalibrated after the selection of each peak,
bringing the other masses in the spectrum into line.
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Setting Automatic Calibration Check Parameters
1. Select AutoCal Check Parameters from the Calibration Edit menu to open the
Automatic Calibration Check dialog.
2. Specify the AutoCal Check parameters, and click OK.
Missed Reference
Peaks
Allows you to enter a number of consecutive peaks
from the reference file that the system is allowed to
miss before a warning is issued to the user.
Maximum Std
Deviation
Performs the same function as Missed Reference
Peaks if the residuals for a particular calibration
exceed the number entered.
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Apply Span
Correction
Applies an extra correction to the mass scale that is
dependent on the mass range being scanned. This
correction ensures that mass assignment will be
correct even if the mass scale that you are working
with is different from the one that the instrument
was originally calibrated over. It is not
recommended that this option be used if the mass
range of interest is less than 1000 amu and includes
the range 0 - 150 amu.
Check Acquisition
Calibration Ranges
If selected, a message is displayed if an acquisition
is started that is outside the range of the current
calibration.
Mass Calibration
Setting Mass Measures
If you are using continuum or MCA acquisition modes to acquire your calibration
data, you will need to tell the system how it should convert the acquired data into
centroided data needed by the calibration process. For more information on Mass
Measure parameters, see Spectrum on page 435.
Setting the Mass Measure Parameters
1. Select Mass Measure Parameters from the Calibration Edit menu to open the
Mass Measure dialog.
2.
Enter the required parameters and click OK.
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The Calibration Report
The peak matching algorithm performed by the calibration may have found wrong
peaks, or missed some peaks. You may need to change the peak match parameters or
adjust the peak matching manually. You can change the peak match parameters by
selecting Peak Match Params from the calibration graph Edit menu. If the peak
matching algorithm has found the wrong peaks, increasing the value of the Peak
window parameter will solve the problem. You should also try reducing the value of
the Intensity threshold parameter (if it is not already zero), before identifying the
peaks in the acquired spectrum by hand.
The top graph shows the calibration spectrum. The peaks matched to reference peaks
are highlighted in a different color.
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Mass Calibration
Altering the Displayed Range
You can alter the range of the spectrum on display by left-clicking at one end of the
range of interest, and dragging the mouse to the other end of the range of interest.
TurboMass indicates the selected range. Clicking Default restores the default
display range.
Manually Matching Peaks
•
You can match a calibration peak to the closest reference peak by positioning the
mouse over the calibration peak in the top window, and right-clicking.
If the closest reference peak is already matched to another calibration peak, the
previous match will be removed.
•
You can also right-click to undo a peak match. Position the mouse over the
matched calibration peak and right-click.
For small peaks, this must be done very close to the baseline.
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Other Calibration Facilities
Deleting the Instrument Calibration
1. Select Delete Calibration from the Calibration Calibrate menu.
This restores the instrument to an uncalibrated state.
2. In the confirmation dialog, click OK to delete all instrument calibration
OR
Click Cancel to abort the operation.
Displaying a Calibration Graph
1. Select From File from the Calibration Calibrate menu to open the Display
Calibration Graphs dialog.
2. Select the desired Calibration Type: Static, Scanning, or Scan Speed
Compensation.
3. Click OK.
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Mass Calibration
Displaying a Verification Graph
You can display the verification graphs for a particular calibration type. Normally an
acquisition would be performed and a calibration made. Use this process to reprocess
the data using the calibration file to verify the accuracy of the calibration.
1. Select Verification From File from the Calibration Process menu to open the
Display Verification Graphs dialog.
2. Select the desired Calibration Type: Static, Scanning, or Scan Speed Compensated.
3. Click OK.
Making a Calibration from a Data File
1. Select From File from the Calibration Calibrate menu to open the Display
Calibration Graphs dialog.
2. Select the Static, Scanning, or Scan Speed Compensation calibration type.
3. Use the default, or click Browse, and select a file.
The default files are STAT.RAW for the static file, SCN.RAW for scanning, and
FAST.RAW for scan speed compensation.
4. Optionally, enter a range of scans to combine From and To.
5. Click OK.
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Recalibrating a Data File
This option allows the current calibration to be applied to a previously acquired data
file.
1. Select Recalibrate Data File from the Calibration Process menu to open the
Display Calibration Graphs dialog.
2. Click Browse and select the data file you want to recalibrate.
3. Click OK.
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Mass Calibration
Editing a Reference File
The table below lists the contents of the file Hepta.ref that is the standard reference
for EI calibration. Calibration reference files consist of two columns of numbers
separated by any number of spaces or TAB characters. The first column contains the
reference peak masses; the second column contains the reference peak intensities. The
reference peak intensities are not at present used by the calibration software and so
can be set to a nominal value of 100. However, you may wish to enter realistic values
here to improve the appearance of the reference spectra.
49.99379
0.73
68.99518
100.00
99.99358
6.31
118.99199
7.80
130.99199
36.31
149.99039
1.29
168.98877
3.24
180.98877
1.31
218.98560
38.07
263.98705
8.38
313.98386
0.32
375.98067
0.38
413.97748
1.64
463.97429
1.02
501.97110
1.90
537.97112
0.13
575.96796
0.32
613.96471
0.64
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You can create or edit calibration reference files using any Windows text editor. To
read the currently selected reference file into the Notepad text editor, select
Reference File from the Calibration Edit menu.
After editing, the reference file can either be saved under the current name by
selecting Save from the Notepad File menu, or saved as a new reference file by
selecting Save as from the Notepad File menu and giving the file a new name.
Textual information or comments can be stored in the reference file. Lines, which are
textual information or comments, must start with a semi-colon ( ; ) character.
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Mass Calibration
High Mass Calibration
Heptacosa’s highest mass peak for calibration is m/z 614. High mass calibration
requires a compound having a higher molecular weight. One compound useful for this
purpose is Tris(perfluoroheptyl)-s-triazine, found in the mass calibration file
Triazine.ref. This compound has calibration ions up to m/z 1185. It is soluble in
methanol and hexane, has a low boiling point, and may be chromatographed easily.
Setup Checks
NOTE: If your mass spectrometer is currently set up and running, skip to Step 8 in Tuning
and Calibration on the next page.
1. Open Tune page (ensure that the transfer line and source are cool: < 100 °C).
2. Make sure the vacuum is 2x10-5 or less (e.g. 1x10-5 or 9x10-6).
3. Check the air and water to be sure the system is leak-free. Refer to Chapter 5 in
the Clarus GC/MS Tutorial for complete procedure.
In a leak-free system, Helium mass 4 should be 100%, water mass 18 should be 10%;
nitrogen mass 24 should be < 10% and oxygen mass 32 should be < 25% of
nitrogen’s response or 5% of mass 4, as shown below.
He2 (carrier gas)
mass 4 = 100%
H2O mass 18 = 10%
N2 mass 28 < mass 18, If N2
is higher than H2O a leak is
present.
O2 mass 32 <
25% of N2
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4. Increase the Clarus MS source and transfer line temperature up to your method’s
operating temperature (for example, 280 °C).
Tuning and Calibration
With a mass spectrometer that is under vacuum, leak-free and at operating
temperature:
1. Open the reference-gas valve (leave Operate off).
2. Select Pump Out Reference Gas with reference-gas valve open (select OK to
the message that appears asking if you want to pump out with valve open) to take
all air and water out of the bulb.
3. After a few seconds, turn off Pump Out Reference Gas, leaving the referencegas valve open.
4. Click on Operate.
5. Run a Custom UltraTune™ (on the option, click on Full).
6. Save the tune file (with a unique name).
7. If necessary, mass calibrate with Heptacosa.
8. Save the calibration file with a notation to designate as a low mass calibration
(Example: date_FC43). Once calibrated and tuned for Heptacosa, release control
of the GC from TurboMass software (in the Sample List window, select Release
Control from the GC menu). On the GC touch-screen interface, apply the
following settings:
• Injector Temperature: 100 °C.
• Carrier Gas: 1.00 mL/min.
• Split: Off during calibration.
• Oven: 125 °C, hold until complete.
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Mass Calibration
Manual injection
1. Before injecting standard, open the Tune page of TurboMass software.
2. Set the software to view m/z 4 (He), m/z 866 and m/z 1166 (Triazine).
3. Enter a Span of 10 and a Gain of 50 for both Triazine ions.
4. Open the Calibration page and select Triazine from the drop-down menu.
Choose masses 866 u and
1166 u to monitor for the
beginning of the Triazine
peak.
From “Edit” menu,
Select Calibration
Parameters
Select Triazine from this
drop down menu before
beginning.
When the m/z 866 ion is
present hit this button to
begin calibration.
One Triazine begins to
elute, a very large peak
will appear in this window.
The major fragment of
Triazine is about m/z 866.
5. Save the file with a name indicating that it is a high mass calibration (for example:
date_tri). Do not overwrite your Heptacosa calibration. Once the GC is ready,
perform a manual injection of the Triazine standard following the procedure
below. Use a 0.5 μL syringe (volume in needle) reserved for that purpose.
6. In the Calibration window select Calibration parameters from the Edit menu
and set the following:
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Perform auto peak matching
Select (check mark)
Peak window (Da)
1
Initial error (Da)
4
Intensity threshold
0.01
4
Deselect (no checkmark)
Polynomial order
Calibrate display
7. Inject about 0.2 μL (make sure that the GC inlet liner is not packed with wool).
8. After injection, return to the Tune page and monitor for the m/z 866 and m/z 1166
ions of Triazine (it is normal for these ions to be shifted from their correct
values, as the system is not yet calibrated). Very quickly (typically under one
minute into the run) the Triazine should begin to elute (the m/z 866 ion will grow
very large). If m/z 866 does not appear within 2 minutes, open your span to 20;
the peak may have shifted outside the current window. Once Triazine is in the
Clarus MS, begin calibration.
9. Once m/z 866 begins to elute, adjust the Repeller, Ion Energy, and Ion Energy
ramp to maximize m/z 866 and 1166.
10. Click on the Start button (►) on the Calibration page, the Automatic Calibration
window appears.
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Mass Calibration
Click to select
appropriate scan range
for calibration.
Once “Acquisition
Parameters” are updated
click “OK” to begin
11. In the Automatic Calibration window, make sure Static Calibration, Scanning
Calibration and Scan Speed Compensation are selected, as well as Acquire &
Calibrate.
Make sure Acquire & Verify are not selected as it will add an additional five
minutes to the acquisition time.
If Print Report is selected, many pages of paper will print out. Only select it if it
is required for laboratory records.
12. At this point, click the Acquisition Parameters button. After clicking the
Acquisition Parameters button, the Calibration Acquisition Setup window will
appear.
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Change the “Scan
to” value to 1200
amu and click “OK”
13. In Calibration Acquisition Setup, change the Scan To value to 1200.
14. Click OK.
15. After changing the acquisition parameters, click OK on the Automatic
Calibration window. The Clarus will begin the calibration process.
This process will run for approximately five minutes. Monitor the m/z 866 and
1166 ions in either the live view of the spectra or chromatogram window. If this
ion decreases dramatically while calibration is running, you will have to start this
process again from Step 1 under “Manual Injection”. Different GC column
phases, lengths or carrier-gas flow rates may require that you decrease the oven
temperature. This will increase the elution time of Triazine, allowing more time
for calibration to run. If calibration fails and a mass shift is still observed after the
calibration file is saved, there is often enough time to run the calibration again.
Save the current calibration and go back to Step 15. Do not open the split vent
or raise the oven and injector temperatures until you have verified a
successful calibration.
16. After you have verified a successful calibration, raise the GC oven temperature to
300 °C (or column maximum), injector port to 300 °C, and open the split vent to
50 mL/min. Allow the GC to bake-out for at least 5 min. to remove residual
triazine.
17. After running the calibration, save the file.
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Mass Calibration
18. Following acquisition, you will verify the calibration from the file.
19. From the Calibration window, click on the Process drop-down menu and select
“Verify from File”.
20. In the Display Verification Graphs window, you will need to verify all three types
of calibration:
• Static: you will select the stat.raw file
• Scanning: you will select the scn.raw file
• Scan Speed Compensation: you will select the fast.raw file
Each Type of
calibration must
be verified.
To select the
appropriate type of
calibration file click
Calibration files are found
in the data folder of your
current project in the
TurboMass Directory.
21. After you select the appropriate file and click OK, a new window (the Select file
for verification window) appears before ion selection.
The spectra shown here has been enlarged to show more detail; the spectra shown
when this window is first opened will show the entire scan range.
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If an ion is not initially identified by
TurboMass it may be manually
selected by the user. To select an
Ion right click on it in the Upper
window you will see the color change
from blue to red and mass notation
will appear above the peak.
22. To verify the calibration, you will want to compare the acquired spectra with the
reference spectra (the above screen shows the acquired spectra on top with the
reference spectra below). As long as most major ions match correctly, the
calibration is good.
23. If the ions do not match correctly, you can modify the peak assignment in the
Calibrate from File menu.
24. To be able to calibrate from file, you will need to manually open each type of
calibration in a similar way as “Verify from File”, described in Step 20. Between
each step you will want to save the calibration file.
25. The window that appears will look similar to the Verify from File window. In this
window, it is possible to reassign peak identification. You can do this by clicking
on an incorrectly-assigned peak and then clicking on the correct peak. You will
see the peak color change from blue to red.
TurboMass software will use the most recently loaded calibration file. If it is
necessary, return to an analysis utilizing a lower mass range. It is generally not
necessary to recalibrate with Heptacosa again. The Heptacosa calibration file, which
was saved under the low mass calibration name in Step 8 of the “Tuning and
calibration” section, can be opened in the Calibration window, allowing TurboMass
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Mass Calibration
software to run using the low mass calibration table. If you are going to be creating a
new project, use the project wizard. This will carry your calibration file to the new
project.
Selection of the ion will change the
color from blue to red, the mass of
this ion will also be assigned. The
mass 769.90 u was measured
before high mass calibration;
following calibration, if measured,
this peak would be assigned a
mass of 770.96 u.
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Saving and Restoring Calibrations
The complete instrument calibration can be saved to disk as a named file and then
recalled at a future date. Static, dynamic, and lag-time calibrations are all saved
together under a common name.
You may find it useful to calibrate the instrument for each of the different types of
experiments that you do and save these calibrations to disk. This means that when you
switch between experiments, you can restore a suitable calibration from disk rather
than having to recalibrate from scratch.
Saving a Named Calibration
1. Click Save As from the Calibration File menu, and enter a new file name.
2. Click Save.
If the selected file exists, you will be asked to confirm that you want to overwrite
the existing information. Click OK to continue or Cancel to enter a different file
name.
Restoring a Saved Calibration
1. Select Open from the Tune File menu.
2. Select the calibration file required, either by entering its name or by selecting it
from the displayed list.
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Mass Calibration
3. Click Open to display the Load Instrument Calibration dialog.
4. Select the desired calibration file.
5. Click OK.
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GC Control
7
GC Control
Overview of TurboMass GC Control
This section contains the software procedures for GC control using the PerkinElmer
Clarus 600 GC as an Inlet Interface example for the GC/MS system. You need to
configure the mass spectrometer for GC control and develop your GC method
before you execute your MS method.
Before you acquire data, you must first configure the software to support the inlet
system selected. You do this from the Select Interface dialog, which displays the
available inlet systems.
1. Choose Select Inlet Interface from the Sample List Configure menu.
The Select Interface dialog is displayed.
2. Select your interface from the displayed list.
The list of inlet options that appears in the Select Interface dialog reflects the inlet
system selected when TurboMass was installed. If, at a later date, you add a new
inlet system or change one of your existing inlets you may need to reinstall
TurboMass to gain access to the control software for the new inlet system.
3. Select your choice for an inlet to use and click OK to reconfigure the software to
reflect the new inlet system.
The GC Status box and GC menu item will appear.
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NOTE: Once you have selected the inlet system, TurboMass will give you access to the parts
of the acquisition system that are appropriate to the inlet selected and the Tune
application.
The GC Menu
All GC commands are located in, or are accessible from, the GC menu in the
TurboMass top level window and Sample List. From the GC menu you set up your
GC configuration, develop your GC method, work interactively with the GC, and
perform all other GC related procedures.
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GC Control
The GC Status Box
You can monitor the GC status from the TurboMass top level window GC Status box.
The GC Status box displays the GC oven temperature and the general GC status. The
general GC status indicates the run status or the GC operational status. For information
on GC status messages, see Understanding GC Status Messages on page 197.
The GC Editor Toolbars and Status Bars
There are two GC editors, the Configuration Editor and the Method Editor. Each GC
editor has a toolbar with buttons that give you quick access to commonly used
commands. When you point to a toolbar button, a tool tip will appear beneath the
button as well as a definition in the status bar at the bottom of the window. The
toolbar is displayed by default. You can hide the toolbar by selecting Toolbar from
the View menu in both GC Editors.
A status bar appears at the bottom of each GC editor that displays a short Help message
explaining the function of the command you highlight in a menu, or the button that the
mouse is positioned over. The status bar is displayed by default. You can hide the
status bar by selecting Status Bar from the View menu in both GC Editors.
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Configuration
When you select Configure… from the GC menu it opens the Configuration Editor
screen and displays information defined during configuration.
156
Name
Your name for the GC.
Type
The GC model or type.
Acq Port
The physical data acquisition port to which the LINK
Interface is connected.
LINK Port
The physical port to which the GC is connected.
Configured
Displays Yes if you have provided all the information
TurboMass needs to configure the GC. Otherwise, the
status is No.
TurboMass Software User’s Guide
IPM
Shows whether or not the Instrument Personality
Module (IPM) for the GC has been downloaded. The
first time you open this window, the IPM will not have
been downloaded.
Once configuration is complete, the area below the
Configuration Editor Summary list displays key GC
information. On the left is information about the LINK
interface including the type (model number), EPROM
version number, memory size available in the interface
(in bytes), and serial number. On the right is a summary
of the GC configuration.
Configuring TurboMass for GC Control
The procedure used to configure the GC depends upon whether you are initially
configuring TurboMass for GC control or are making changes from the GC keypad.
Initial GC Configuration - Use to set up the LINK and GC for TurboMass control
for the first time.
Reconfiguring the GC - Use to make changes from the GC keypad or hardware
changes to the GC without changing the LINK configuration. Reconfiguration is
also required if you add an autosampler.
Initial GC Configuration
There are four steps to configuring TurboMass for GC control for the first time:
•
Confirm a data acquisition port.
•
Confirm the LINK configuration.
•
Set the GC configuration options.
•
Save the configuration.
Each step is described in a separate procedure.
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Confirming a data acquisition port
1. Open the TurboMass application to display the TurboMass top level window.
2. Select Configure from the GC menu to open the Configuration Editor.
3. In the Configuration Editor, select Configure from the Instrument menu to
open the Serial port connected to GC dialog.
4. Select the serial port and click Continue.
The LINK Configuration dialog displays the COM port and instrument name.
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GC Control
Confirming the LINK configuration
1. Select the LINK port for the GC.
For an integral Link, you must select Port A.
2. Select Clarus 600 With or Without Autosampler from the Instrument Name
drop-down list, according to your GC configuration (or if using the Clarus 500
GC select Clarus 500 With or Without Autosampler).
You must select Clarus 600 (or 500) With Autosampler if an autosampler is
installed on your GC. You may exclude use of the autosampler in the GC
Method Editor.
If you make a mistake, click Restart to disconnect the GC and clear the LINK
port. Click Reset to clear all changes and return this dialog to the state it was in
before it was opened.
Setting the GC configuration options
1. In the LINK Configuration dialog, click Configured (next to the port selection)
to open the GC Configuration dialog.
2. To rename the GC to something other than its default name, enter the new name
in the Name field.
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TurboMass Software User’s Guide
3. Under Options, select whether or not you have PPC (Programmable Pneumatic
Control) installed.
Selecting YES activates the other PPC options.
4. Under Inlets, select the Injector setting that matches your GC for Channel A
and/or B.
5. Select the valve type for each valve in the GC.
The PPC split vents will be configured automatically.
6. Select PPC for detector A and/or B if detectors and PPC are installed.
7. Under Detectors, select the Detector, Mode, and Output settings that match
any additional detectors installed on your GC for Channel A and/or B.
8. Under Carrier Pneumatics, select the Pressure units and other options.
9. Select a setting for Carrier A.
PVel
Denotes programmable linear velocity operation. This option is only
available for CAP and PSSx injectors in Cap Control Mode. (You enter
the average values for capillary column linear velocity in the method,
as well as values for column dimensions and vacuum compensation.)
CFlow
Denotes operation at a constant flow rate. (Enter pressure values in the
method.) The pressure is varied by the GC to maintain a constant mass
flow rate through the column as the oven temperature changes. This
mode does not require you to enter column dimensions in the method.
PFlow
Denotes programmable flow operation. (Enter flow values in the
method.)
Press
Indicates direct pressure programmable control in the pressure units
you select.
IFlow
Denotes constant flow operation. (Enter flow values in the method.)
10. If appropriate, repeat the process for Carrier B.
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GC Control
11. Under Auxiliary Pneumatics, select PPC for any auxiliary zone that has a PPC
controller installed.
12. Select the settings to control pressure or flow of the auxiliary zone(s).
13. Click OK.
A check mark in the LINK Configuration dialog indicates that the GC has been
configured.
Saving the configuration
1. Click Finish in the LINK Configuration dialog to save the configuration.
TurboMass creates a configuration file (.CFG) for the GC and downloads the
appropriate IPM. The IPMs available to you are installed during TurboMass
installation.
When you first configure the GC, the Config message appears:
2. If the GC is connected and turned on, click Yes.
3. TurboMass will attempt to check the physical connection with the GC by taking,
and then releasing, control of the GC.
The Confirm Configuration message appears.
4. To compare the configuration options you selected with those that are being
reported by the GC, click Yes.
A series of confirmation messages appear.
5. Respond to each message.
When TurboMass is finished, the Configuration Editor appears.
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Yes appears in the Configured column if your LINK and GC are adequately
configured. If No appears, you need to complete the configuration before you
can acquire data.
Reconfiguring the GC
If you make hardware or other configuration changes to your GC after you have
configured TurboMass for GC control, you can reconfigure the GC settings without
changing the LINK configuration.
However, if you add an autosampler to a GC, you must reconfigure the LINK and
GC as you did when you initially configured your GC. As you are starting with a
configured LINK and GC, you must first disconnect the GC from TurboMass
control and clear the LINK configuration.
1. In the TurboMass top level window, select Release Control from the GC menu
to release TurboMass control of the GC.
Releasing the GC from TurboMass control lets you control the GC from the
keypad. The GC front panel display changes from “External” (TurboMass) to
“Method#” control, where Method# is an internal GC method.
2. Make the required changes from the GC keypad.
3. To update your GC configuration in the TurboMass Configuration Editor, select
Configure from the Instrument menu to open the GC Configuration dialog, and
either click Query Inst for Config to obtain your updated parameters from the
GC, then click OK.
OR
Enter your changes in the GC Configuration dialog, and click OK to update your
GC configuration.
For more information on setting the GC parameters, see Setting the GC
configuration options on page 159.
Changing the Instrument Configuration
1. Select your instrument in the Configuration Editor.
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GC Control
2. Select Disconnect from the Configuration Editor Instrument menu, respond to
the confirmation message that appears, and click OK.
TurboMass clears your LINK port and GC configuration information.
3. To reconfigure your LINK and GC to reflect your new instrumentation, see
Configuring TurboMass for GC Control on page 157.
Changing Your Acquisition Port
You can change the serial port without reconfiguring your LINK and without
opening the Configuration Editor. Before starting this procedure, be sure to
reconnect the serial cable to the appropriate port on your PC.
1. Select Release Control from the GC menu to release the GC from TurboMass
control.
2. Select Change Acquisition Port from the GC menu to open the PortSwitch
dialog.
3. Select the appropriate port (usually COM1), and click OK.
4. In the GC menu, select Take Control to re-establish (TurboMass) control of the
GC.
TurboMass changes the selected COM port and updates your configuration.
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Configuring TurboMass without GC Control
You can configure TurboMass for data reprocessing only or for use with a GC that
is not under TurboMass control.
1. Select Configure from the GC menu to open the Select Interface dialog.
2. To configure TurboMass, for data reprocessing only, select None
OR
For data acquisition but not GC control, select Contact Closure.
Configuring User Options
From the Configuration Editor User menu, you can change the fonts used to print
out the GC method summary and you can set up quick paths.
Changing Fonts
The Font dialog lets you choose the typeface, style, and size of text that will appear
in the Method Editor Summary.
Selecting a Font
1. To open the Font dialog, select Fonts from the User menu
OR
Click the fonts tool.
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The Method Editor Summary is automatically selected in the Select font to
change drop-down list.
2. Select a Font, Font Style, and Size of text.
3. Click OK.
Specifying Quick Paths
Specifying a quick path lets you quickly choose a frequently used path in any file
selection dialog in the GC editors. This provides, for example, immediate access to
your mass spectrometry project file, instead of scrolling and clicking through the
Windows file-selection method.
Adding a path to the Quick Paths list
1. In the Configuration Editor, select Quick Paths from the User menu.
The Quick Paths dialog box appears and lists the current quick paths.
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2. Click Add.
The TurboMass Path-Select dialog opens:
3. Select a path and click Select.
TurboMass will add the path as a quick path and list it in the Quick Paths dialog.
If you want to set a quick path to your project directory, specify the following quick
path to the project subdirectory that contains the GC method:<project path>\acqudb
For example:
c:\TurboMass\myproject.pro\acqudb\
If you do not specify a project directory, TurboMass creates the following project
directory as a default, which you can specify as one of your quick paths:
c:\TurboMass\Default.pro
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Inserting a path in the Quick Paths list
1. In the Configuration Editor, select Quick Paths from the User menu to open the
Quick Paths dialog.
2. Select the path above which you want to insert a new quick path, and click Insert.
3. In the Path-Select dialog select a path, and click Select.
TurboMass will add the path to the Quick Paths list.
Removing a quick path from the Quick Paths list
1. In the Configuration Editor, select Quick Paths from the User menu to open the
Quick Paths dialog.
2. Select the path you want to delete from the Quick Paths list, and click Delete.
Removing all paths from the Quick Paths list
1. In the Configuration Editor, select Quick Paths from the User menu to open the
Quick Paths dialog.
2. Click Clear.
3. If you change your mind, click Reset to replace the original paths.
Printing Configuration Information
The Print command in the File menu lets you print a copy of the LINK and GC
configuration information. Configuration information includes font choices, quick
paths, and GC and interface data.
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GC Method Editor
You use the Method Editor for all GC method operations. When opening the
Method Editor from the GC menu, the Method Summary Window is displayed.
The Method Summary Window contains the data acquisition and GC control
information including the run-time information and control options, such as injector
temperatures, carrier gas settings, and oven program.
Developing a GC Method
To develop a new GC method, set data channels, and set your GC control options.
You can also create a new method by editing an existing method file and renaming it
with the Save As Command.
Creating a new GC method
1. Select Method Editor from the GC menu in the TurboMass top level window
OR
2. Click
in the GC panel.
3. Select Create new method in the Startup dialog, and click OK to open the
Method Editor.
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Opening an existing method
You can open an existing method from two places:
•
From the Method Editor:
Select Method Editor from the GC menu to open the Startup dialog.
In the Startup dialog, select Load method stored on disk, or select Load
recently edited method and select the desired method.
•
From the Sample List:
Right-click the Inlet File cell in the Sample List that contains the GC
method you want to open, and select Open from the drop-down menu
OR
Select Open from the TurboMass Edit menu.
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Setting Data Channels
The Data Channels command in the Instrument menu control how TurboMass
acquires analog and digital data by letting you set the channel or channels for data
collection, the data sampling rate, and the analysis run time. Some of the options
available on the Data Channels tab depend on the type of instrument that you are
using. If not, select None.
NOTE: Setting data channels applies only if you have additional conventional detectors
installed on the GC. If not, choose “None.”
Setting channel options for the GC
1. Select Data Channels from the GC Method Editor Instrument menu to open
the Data Acquisition dialog.
2. Under Data Channel, select channel A, B, Dual, or None.
3. Under Source, select the appropriate additional signal source for the data
channel(s).
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4. Under Set Data Rate, to set the rate at which the GC will sample its detectors
either select By peak width at base, and then enter the number of seconds in
the text field.
With this option, TurboMass acquires data in terms of the width (at its base) of
the narrowest peak that you expect to occur in the run. If you enter a peak width,
TurboMass calculates the optimum sampling rate for that peak width, collecting
at least 20 data points across the peak.
OR
Select By sampling rate, and then enter or select a rate.
With this option, TurboMass acquires data from the GC using the number of
data points per second that you explicitly set (or the nearest available rate to that
value).
5. Under Data Storage, either select Store all data from run to store all the data
from a run.
This option is useful if you don't know the run time because you have not
entered the GC oven program.
OR
Deselect Store all data from run to store only the data collected in a given
time window.
You must specify the relevant times. In the Delay time field, enter the number
of minutes that you want to elapse between the start of the run and when data
analysis starts. In the Run time field, enter the number of minutes for which you
want the interface to collect data. Note that the run time must always be greater
than the delay time.
6. Select Store run log to upload the run log at the end of each run.
When you select this option, TurboMass stores the GC method and run log as
part of the Experimental Record. Store run log is available even when there are
no additional detectors installed on the GC.
7. To save your work and close the dialog, click OK.
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Setting Control Options
The Control Options command in the Instrument menu opens a submenu that has
additional commands for controlling your instruments. When you select a command
from this submenu, TurboMass opens the Instrument Control dialog, which contains
tabs for each major control command.
Setting control options parameters
1. Select Control Options from the Instrument menu and select a command from
the cascaded menu.
The Instrument Control dialog opens to the tab corresponding to the command
that you selected.
2. Select the tab for each control option that you want to complete or edit.
3. Make any changes to the values in the dialog.
4. To save your work and close the dialog, click OK
To save your work without closing the dialog, click Apply
To close the dialog and discard your changes since the last time you clicked
Apply, click Cancel.
The following sections describe how to complete each of the tabs in the Instrument
Control dialog.
The possible tabs in the Instrument Control dialog are:
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•
Autosampler.
•
Oven/Inlets.
•
Carrier.
•
Valves.
•
Detectors.
GC Control
•
Instrument Timed Events.
For a complete definition of each GC parameter, refer to your GC hardware manual.
Setting autosampler parameters for the GC
1. Select the Autosampler tab of the Instrument Control dialog.
2. If you are using manual injection, select Manual
OR
If you are using an autosampler, continue with Steps 3 through 9.
3. Select the Syringe capacity for the syringe in the autosampler.
4. Select the actual Injection volume and an Injection speed.
5. Select the number of Sample pumps that you want to use.
This value specifies the number of times the syringe is filled and emptied before
the final load.
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6. If you are injecting a viscous sample, set the Viscosity delay.
7. Select the Wash/waste vial set that you want to use.
Wash/waste vial set 1 uses vials 1 and 2. Wash/waste vial set 2 uses vials 3 and 4.
8. Select the number of Pre-injection solvent washes that you want to have.
This value determines how many times the syringe is washed with solvent
before each injection.
9. Select the number of Pre-injection sample washes and Post-injection solvent
washes that you want to have.
Setting GC Oven/Inlets Parameters
The Oven/Inlets tab of the Instrument Control dialog controls the oven temperature
of your gas chromatograph, the rate at which the temperature increases, the type of
coolant that you are using, and the zone setpoints for injectors and detectors.
The Ovens/Inlets tab also includes a temperature curve that corresponds to the
values that you enter in the table beneath it. The table has the following columns:
Rate
Represents the rate at which the oven is heated. You can create up
to ten ramps, which are periods during which the temperature
increases. Ramps are in degrees per minute.
Temp
Gives the temperature to which the oven is being raised during the
ramp.
Hold
Represents the period for which the temperature is held before
starting the next ramp. The initial setting is the temperature of the
oven at the start of the run, or throughout the run for an isothermal
analysis.
The Initial Rate field is always 0.0 and you cannot edit this field. To edit the other
fields, click in the field and then enter a value. The Temperature and Hold fields are
disabled until you set the Rate.
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You can also adjust the Temperature and Hold values by dragging the corresponding
points on the curve to the desired position.
1. Select the Oven/Inlets tab of the Instrument Control dialog.
3. From the available program tabs beneath the table, select the tab for the
temperature program that you want to edit.
The curve for the program that you select appears as a solid line. The curves for
all other programs appear as dashed lines.
4. In the Initial Temp field of the table, set the temperature for the start of the run.
5. In the Initial Hold field, enter the amount of time that you want to hold the
initial temperature.
To hold the temperature until the end of the oven program, enter 999.
6. Set the Rate, Temp and Hold values for the other ramp levels.
The time value under Program time changes to reflect the time that is required
to complete the temperature program.
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7. You can also change the values directly on the curve by dragging the points
associated with each ramp level. When you release the points after dragging, the
new values appear in the table.
• To change the rate of a level, select the point that represents the temperature
and drag it horizontally.
• To change the temperature value of a level, select the point that represents
the temperature and drag it vertically.
• To change the hold time duration of a level, select the point that represents
the time and drag it horizontally.
8. Under Cryo, if equipped with the subambient option, select the type of
subambient cooling that you want to use, or set Coolant to Off.
9. If you are using sub-ambient cooling, enter the values for the cryogenic Cut-in
temperature and the oven Timeout in the respective fields.
10. Under Oven, enter the maximum oven temperature allowed.
This value protects the installed column.
11. In the Equil time field, enter the number of minutes that you want the GC oven
to equilibrate at the initial temperature before it becomes READY.
For temperature programming (ramping), typically, the Clarus 600 GC does not
require a temperature equilibration time.
12. Under Heated zone setpoints, if you have non-programmable inlets enter the
temperature for Injector A and Injector B.
If you have programmable inlet type POC or PSS configured in either inlet
program mode or oven tracking mode POCI, PSSI, POCO, or PSSO, select
either On or Off for Injectors A and B.
POCO and PSSO track the oven program temperature +5 °C.
13. If the option is available, enter an Auxiliary zone temperature.
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Setting GC Carrier Parameters
You can use the Carrier tab of the Instrument Control dialog to set carrier
parameters such as the inlet pressure or flow rate for carrier gas.
If the GC has neither carrier nor auxiliary zone configured as a PPC Zone, you can
enter only the pressure and flow values for inclusion in the instrument’s Ready
logic. You must set the actual pressure and flow rate on the GC itself.
Setting carrier parameters without PPC zones
1. Select the Carrier tab of the Instrument Control dialog.
2. Enter the Pressure or flow rate for carrier A and B.
Enter 0.0 if you do not want the actual pressure or flow setting to prevent the
instrument from becoming ready.
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Setting GC Carrier Parameters with PPC Zones
If the GC has either carrier or any auxiliary zones as a PPC zone, you can enter
information about the column, program, inlet split controls, and auxiliary
pneumatics setpoints.
The Carrier tab also includes a pressure/flow/velocity curve that reflects the values
that you enter in the table beneath it. You can switch among different carrier
programs by selecting the program tabs at the bottom of the table. The table has the
following columns:
Rate
Represents the rate at which the carrier pressure/flow/velocity
changes. You can create up to three ramps, which are periods
during which the pressure/flow/velocity changes. Ramps are
shown on the vertical axis of the curve.
Setpoint/Temp
Gives the pressure/flow/velocity to which the carrier is being
changed. When Oven is selected, it displays the temperature
for the oven.
Hold
Represents the period for which the pressure/flow/velocity is
held before starting the next ramp. The initial setting is the
pressure/flow/velocity of the carrier at the start of the run, or
throughout the run.
The Initial Rate field is always 0.0 and you cannot edit this field. To edit the other
fields, click in the field and then enter a value. The Setpoint and Hold fields in a
ramp are disabled until you set the Rate.
1. Select the Carrier tab of the Instrument Control dialog.
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2. From the available program tabs beneath the table, select the tab for the program
that you want to display.
The curve and the table change to reflect the program that you select. The curve
for the program that you select appears as a solid line. The curves for all other
programs appear as dashed lines.
The information under Program time also changes to reflect the selected carrier
values. The color-coded carrier time fields show how much time is required to
complete the pressure/flow/velocity program. Aux Time appears instead of the
carrier time for certain instruments. Oven time shows how much time is
required to complete the oven program.
3. In the Initial Setpoint field of the table, set the flow/pressure/velocity for the
start of the run.
4. If the program you are editing is a constant flow/pressure/velocity program, then
you can only enter an initial Setpoint value in the table.
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5. In the Initial Hold field, enter the length of time to hold at the final
flow/pressure/velocity for this program step.
To hold the flow/pressure/velocity until the end of the temperature program,
enter 999.
6. Set the Rate, Setpoint and Hold values for the other ramp levels.
7. You can also change the values directly on the curve by dragging the points
associated with each ramp level. When you release the points after dragging, the
new values appear in the table.
• To change the rate (flow/pressure/velocity) of a level, select the point that
represents the setpoint and drag it horizontally.
• To change the setpoint value of a level, select the point that represents the
setpoint and drag it vertically.
• To change the hold time duration of a level, select the point that represents
the time and drag it horizontally.
8. If you selected capillary mode during instrument configuration, set the Length
and Diameter of the column under Column.
9. Turn on the Vacuum compensation for the column.
10. If the instrument is configured with auxiliary pneumatics, enter the Auxiliary
Pneumatics setpoints for any auxiliary zones.
11. Under Split Control, select a split control mode.
12. If you select Ratio, enter a split ratio in the Ratio field.
OR
If you select Flow, enter a split flow in the Flow field.
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Setting GC Valves
You can use the Instrument Timed Events tab of the Instrument Control dialog to
enter the initial settings for any valves installed on the GC.
1. Select the Instrument Timed Events tab of the Instrument Control dialog.
The Valves group reflects the system configuration.
2. Under Valves, set the Initial Setting buttons to On or Off for each valve.
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Setting GC Detector Parameters
NOTE: These parameters apply only if you have additional conventional detectors installed
on the GC.
You can use the Detectors tab of the Instrument Control dialog to control the
sensitivity of detection during the analysis as well as the magnitude of any optional
analog output from the GC.
1. Select the Detectors tab of the Instrument Control dialog.
2. In the Temp field, enter a temperature value for the detector.
3. Select a sensitivity setting for the detector from the Range drop-down list.
4. This value is the gain level of the detector output. The values depend on the
instrument and detector type. For example, if you are using a Clarus with an
FID, the lower the Range setting, the greater the detector sensitivity. For a TCD,
the lower the Range setting, the lower the detector sensitivity.
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5. Select a Time constant.
This value sets the detector filter width in milliseconds, which smoothes out the
detector signal. Higher values improve the signal-to-noise ratio but attenuate
narrow peaks.
6. If you are using an FPD detector, set the PMT %.
This value is the percentage of the maximum photo-multiplier voltage and
sensitivity.
7. To make the detector autozero at the start of each run, select Autozero On.
8. If the Value field is available, enter a value to specify an offset.
9. If the Polarity option is available, select Positive or Negative.
10. If the Filament option is available, select On or Off.
11. Under Gases, specify the gas flow rates for the detector.
12. If the GC configuration includes either REC (Recorder) or INT (Integrator)
settings for analog output, set the following options under REC or INT:
• Select an Attenuation value for analog output from the Attenuation dropdown list.
• In the Offset field, enter the amount by which to offset the analog output for
an external recorder.
14. Repeat Steps 2 through 11 for the second detector.
Setting Instrument Timed Events
Use the Instrument Timed Events tab of the Instrument Control dialog to select
one or more timed events from a predefined list, and enter the time at which you
want the event to take place.
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Adding or editing timed events
1. Select the Instrument Timed Events tab of the Instrument Control dialog.
2. In the Time field, enter the time at which you want this event to occur during the
run.
3. From the Event drop-down list, select the event that you want to add.
4. If the event requires a value or setting, the Value field becomes enabled.
5. Depending on the event, use the Value field or list to specify a value for the
event.
6. Click Add to add this event to the Defined Events list.
7. Repeat Steps 2 through 5 to add other events.
TurboMass list the events in the order of the time at which they occur.
Changing the time or value of a timed event
1. Under Defined Events, select the event that you want to change.
2. To change the time, enter a new number in the Time field.
OR
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To change the value, either select one from the list or enter a value in the field.
3. Click Change.
Deleting a timed event
1. Under Defined Events, select the event that you want to delete.
2. Click Delete.
Deleting all timed events
Click Clear.
Entering Descriptive Information for GC Files
From the Method Editor you can enter descriptive information about your GC
method and/or enter audit trail information.
You may enter descriptive information about a method on the Description tab of the
Documentation dialog, and you may enter information about changes made in the
Audit Trail dialog (if auditing is enabled.) One or the other will appear
automatically when you save a file according to the following rules:
•
The Description tab in the Documentation dialog always appears when you
save a new file. If auditing has not been started for a file, then the Description
tab also appears when you use Save As to save an existing file with a new name.
•
If auditing has been started for a file, the Audit Trail dialog appears every time
you save that file with either Save or Save As.
You enable an audit trail by selecting Start audit trail on the Description tab. Once
an audit trail is started, the Description dialog will not appear automatically if you
select Save As. However, you can display it at any time by selecting Description
from the File menu.
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The Description tab in the Documentation dialog
The Description tab opens when you save a new file, and (if auditing is not
enabled) when you select Save As to save an existing file with a new name. You
can also select Description from the File menu to open the Documentation dialog
showing the Description tab.
Entering information in the Description tab
1. Enter any descriptive information about the file that you want to store with it.
To start a new line, press CTRL+M.
2. If you want to start tracking changes to the file, select Start audit trail.
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This will cause the Audit Trail dialog to appear every time you save this file in
the future.
3. Click OK.
Audit Trail Dialog
If you previously enabled auditing for a file, the Audit Trail dialog appears every
time you save the file or select Save As to save it under a new name. This dialog
cannot be opened manually by any menu command or button.
Entering information in the Audit Trail dialog
1. Select a reason for the change(s) in the Reason field.
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2. Enter any information about the change(s) you made to the file in the Comment
field.
3. If you are saving the existing file as a new file (Save As), select Retain Audit
Trail Information if you want to copy the Audit Trail information from the
existing file to the new file and have auditing enabled in the new file.
4. Click OK.
The information you enter in the Audit Trail dialog is saved with the file that
you are auditing.
The Audit Trail
The Audit Trail tab in the Documentation dialog displays a history of changes made
to the audited file. It appears when you select Display Audit Trail from the File
menu. You cannot edit the information in this tab.
Viewing the Audit Trail
1. Select Display Audit Trail from the File menu.
2. When you have finished viewing the information, click OK.
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Printing the Audit Trail
TurboMass displays a print options dialog when you select Print from the Method
Editor File menu. This dialog includes an option to print the Audit Trail for the
current file.
Creating Instrument Notes
The Notes command in the Instrument menu lets you create original text or use the
preset template to record information about the instrument section of the method.
The information you enter has no effect on data analysis. You can view these notes
when you select Print Preview from the Method Editor File menu. You can print
these notes when you print the full method.
Creating or editing header information for the GC method
1. Select Notes from the Instrument menu to open the Instrument Notes dialog.
2. Enter the header text that you want to appear in the printed reports for this
method. To start a new line, press CTRL+M. To erase the contents of the text
field, click Reset.
OR
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Select the CAP-GC template from the Template drop-down list.
3. If you are working with the CAP-GC template, edit the information as
necessary.
4. Click OK to save your changes.
Printing GC Method Parameters
You can print either the specific parameters from a GC method file or the summary
information for a method by using the File menu Print or Print Summary
commands. Two print-related dialogs will appear when you print parameters: one
for method editor options and one for standard printing options.
Printing the parameters from the method
1. Select Print from the File menu to open the Print Options dialog.
2. Select the data to print and click OK.
3. Make any changes in the Print dialog, and click OK.
Printing summary information for a method
1. Select Print Summary from the File menu to open the Print dialog.
2. Make any changes in the Print dialog, and click OK.
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Controlling the GC
Some GC-related menu choices are commands that let you control the GC:
•
Equilibrate.
•
Stop GC and Retry Injection.
•
Take and Release Control.
Equilibrating the GC
GC Equilibration sends the GC method temperature and pressure settings to the GC
to enable the GC to reach those setpoints in preparation for sample injection and
data acquisition.
Equilibrating the GC
Select Equilibrate from the Method Editor menu.
The mass spectrometry sends the GC method temperature and pressure settings
to the GC and begins equilibration.
The GC status in the top level window indicates that MS is equilibrating the GC.
When equilibration is complete, the GC status changes to Ready.
Stopping and Restarting the GC
If there is a problem with the GC setup after a run is started, the Stop command lets
you stop the analysis. Once you have corrected the problem, Retry Injection lets
you restart the GC without stopping and restarting your mass spectrometer method.
NOTE: Stopping the GC from the GC menu does not stop MS data acquisition.
Selecting Stop from the GC menu stops the method that is in the inlet file cell of the
Sample List; however, the mass spectrometer is still acquiring data.
To stop MS data acquisition, select Stop from the TurboMass top level window
Run menu, and respond whether you want to stop the GC as well.
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If you started the MS data acquisition from the Tune page Window menu, stop
the MS data acquisition, and select Stop GC from the Configuration Editor GC
menu if you want to stop the GC also.
Releasing and Taking Control of the GC
The Release command lets you release the GC from mass spectrometer control to
change a setting from the GC keypad or to make a hardware change to the GC. Once
you have completed your change(s), you must re-establish (Take) control of the GC.
Releasing control of the GC
From the GC menu, select Release Control.
The Take Control command in the GC menu allows you to take control of the
GC if its current GC status is Released. Usually, you do not have to select Take
Control because this occurs automatically when you start your MS data
acquisition. However, you may need to select Take Control if you previously
selected Release Control.
Taking control of the GC
From the GC menu, select Take Control.
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The Details Window
The Details command lets you see the GC run and interface status information.
The specific contents of the Details window depend upon whether you are collecting
data from a Clarus detector.
Text appearing in blue on your screen represents information that is changing
dynamically as the GC status changes. Text appearing in gray represents
information that does not apply to this setup.
Viewing detailed status and run information
Select Details from the GC menu to open the Details window.
Viewing a Real-Time Plot of GC Detector Data
You can view a real-time plot of GC detector data, for example a plot from a flame
ionization detector (FID).
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To display the real-time plot:
•
Select Real-Time Plot from the GC menu.
NOTE: The GC method file must be available in order for the software to display the realtime plot.
Viewing Data Acquisition Information
The information that appears in the Details window is grouped into several
categories.
Sample Information
Vial Number
Number of the sample as specified in the Sample List.
Raw Data File Ch A
(Ch B, or both)
The full name of the current raw data file (for each
active channel). This information appears only if data are
being saved from a Clarus detector.
Analysis Information
Instrument Method
The name of the current method used for instrument
control.
Run Time
The total length of time the current cycle is to run.
Delay Time
The amount of time between the start of the run and
when data will be analyzed.
Sampling Rate
The number of data points acquired per second.
Viewing Detailed Instrument Information
The Details window displays information about the state of the GC.
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Current
This section summarizes some of the more important current values.
I/F Status
Status of the interface. For more information, refer to
Understanding GC Status Messages on page 197.
Elapsed Time
The amount of time, in minutes, that the current cycle has
been running.
Aux
Current flow/pressure.
Carr A/B
Current carrier flow/pressure
Inj. A/B
Current injector temperature.
Oven Temp
Current oven temperature.
Program Time
Length of time to run the oven program.
Zones
The setpoint (Init Set) for all zones might change during a run if you have set any
timed events. The column will indicate Ready, Not Ready, Alarm, or N/A.
Injector Temp
Init Set
Setpoint temperatures for injectors A and B.
Actual
Current (actual) temperatures of injectors A and B.
Ready
Whether or not the injector is ready.
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Detector Temp
Init Set
Setpoint temperatures for detectors A and B.
Actual
Current temperatures of detectors A and B.
Ready
Whether or not the temperature zone is ready.
Carrier Pressure/Flow
Init Set
The initial carrier setpoint for channels A and B.
Actual
The current (actual) carrier pressure/flow of channels A and B.
Units
Units configured for the carrier.
Ready
Whether or not the carrier zone is ready.
Detector Flow
Init Set
The setpoint detector flow (two flows can be associated with each
injector).
Actual
The current (actual) detector flow of detectors A and B.
Ready
Whether or not the detector flow zone is ready.
Auxiliary Pressure/Flow
196
Init Set
The initial setpoint pressure/flow for auxiliary zones 1 through 4.
The actual value might differ from the Init value due to timed
events.
Actual
The current (actual) pressure/flow of auxiliary zones 1 through 4.
Units
Units configured for the carrier.
Ready
Whether or not the pressure/flow is ready for the auxiliary zones.
GC Control
Split Flow
Init Set
The setpoint displayed as either flow or ratio depending on
which mode you are using. The actual value might differ from
the Init value due to timed events.
Actual
The current (actual) flow.
Ready
Whether or not the split flow zone is ready.
Understanding GC Status Messages
The status is displayed in the top level TurboMass window in the GC Status area.
The status area displays the general status, the GC status, and the oven status. The
status information changes constantly as you acquire data, modify GC methods, and
perform other actions that affect the GC.
NOTE: The GC status must be either "No Method" or "Run Done" to successfully set up.
Otherwise GC communication lockups may occur.
The General and GC Status messages are color coded as follows:
Green
Indicates that the instrument is ready to start a run (acquire
data).
Blue
Indicates that the interface is active (a run is in progress, or the
interface is uploading data to TurboMass).
Red
Shows that the instrument is not ready to collect data because it
is not connected, it has no method, or it has been paused.
General Status
Active
The interface is collecting data from a current GC run.
Backlog
Data from one or more completed runs still reside in the
interface.
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Detached
Not currently communicating with the interface, possibly due to
communication errors.
Not
Connected
The instrument is not turned on or it is not connected to the
computer.
Init Error
An error occurred during initialization.
Initializing
TurboMass is retrieving initial status information for the
interface.
In Reconfig
The interface is reconfiguring itself, for example, updating the
IPM.
No Method
The interface is turned on and connected to computer but is not
set up, or there is no method downloaded.
Post-Run
Post-run activity is in progress or the autosampler is cleaning up
after the previous injection.
Pre-Run
The autosampler is preparing the next injection.
Ready
The interface is ready to collect data and is waiting for the run to
start.
Run Done
The run is complete. The instrument must be initialized again
for any future analyses.
Run Log
The GC is uploading Run Log information to TurboMass.
Setting Up
The instrument is being initialized with acquisition information.
System
Reconfig
TurboMass is carrying out a system reconfiguration.
TurboMass Software User’s Guide
GC Status
Equil
The GC is equilibrating.
Hold
The GC temperature program is in a hold state.
Not Ready
The GC is not ready.
Off
The GC is turned off.
Oven Off
The GC oven is turned off.
Pre-Run
The GC is executing the pre-run events.
Ready
The GC is ready.
PPC Alarm
The PPC pneumatics are in a fault condition.
During the oven temperature program, the current program step appears.
These are: Initial (temp), Ramp 1, Hold 1, Ramp 2, Hold 2, Ramp 3, Hold 3, and
Cool.
Oven Temperature
Oven temperature is displayed as an integer and may range from -99 to 450.
Viewing Error Messages
When an error occurs during configuration, method setup, or during a run,
TurboMass displays an error message and saves it in the Error Log.
1. Select Error Messages from the GC menu to open the Error Log.
2. To print the Error Log, click Print.
3. To clear the Error Log, click Clear.
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Working with the GC Interactively
There are two commands that let your work with the GC interactively, Hands On
and Modify Active. Hands On lets you change some settings after GC setup.
Modify Active lets you change a downloaded method.
Using Hands On
The Hands On command in the GC menu lets you control certain settings after you
have set up the GC. You can set the GC oven temperature, autozero the detector,
and turn valves (or relays) on and off. You can access Hands On either during or
outside of a run. The actual parameters available depend on whether or not a run is
in progress. The Hands On command is not available until you have initialized the
GC with a method.
Setting controls for the GC
1. Select Hands On from the GC menu, and click Close.
The GC Hands On dialog is displayed, showing the oven temperature and the
current valve settings.
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2. In the Setpoint field, enter the setpoint oven temperature for the GC, and click
Set Temp.
3. Click Autozero, if desired.
4. Select the valves you want to switch by selecting the ON or OFF button as
appropriate.
5. Click Set Valves to implement the settings, and click Close.
You must click Set Temp, Set Valves, or Autozero before clicking Close in
order to change settings.
Modifying the Active Method
The Modify Active command in the GC menu lets you change method parameters in
a method that has been downloaded by selecting Start from the TurboMass top level
window Run menu.
When a method has been downloaded, it is by definition the active method — the
one that is being used in the current run — and the Method Editor opens when you
select the Modify Active command.
The commands and options available in the Method Editor depend on whether or not
a run is in progress. When you modify the active method, the term Modify Active is
displayed in the title bar of the Method Editor.
When you modify the active method with a run in progress, the instrument
parameters that you can modify are limited to those that can be downloaded during a
run. That is, you can modify the oven/inlet and detector parameters.
When you modify the active method and there is no run in progress, you can modify
all method parameters in the active method.
When you finish editing the method, TurboMass downloads the modified method to
the LINK and uses it for the next run.
NOTE: If you select a method that is not the active method, you can modify all parameters
within that method during or outside of a run.
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Modifying the downloaded method
1. Select Modify Active from the GC menu, or double-click the GC portion of the
system icon in the Acquisition Control Panel
OR
Right-click the active method displayed in the Inlet File cell in the Sample List.
The GC method in use appears in the Modify Active (Method Editor) window.
2. In the Modify Active window, select a command from the Instrument menu to
modify the parameters associated with that command.
3. Save your changes after editing method parameters.
Note that the Save As command is not available because you cannot save the
changes as a new method.
4. Close the Modify Active window.
The GC Status field will display different messages, based on the instrument
you are using. While you are modifying the method, the instrument state will be
Paused. It will change to Resumed when you close the Modify Active
window.
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Function List Editor
8
Function List Editor
Introduction
The Function List Editor is used to set up the function(s) that the mass spectrometer
will use to scan the instrument during an acquisition. A function list can be a
mixture of different scanning techniques that can be arranged to run either
sequentially or concurrently during an acquisition. Typical uses for mixed function
acquisitions are to acquire different SIR groups over different retention windows
and the ability to switch MS scan mass ranges during an acquisition.
A function list is produced, saved on disk and then referenced by name when you
start an acquisition.
The simple function list shown might contain only one function, for example, a
centroided mode full scan between 50 and 550 amu using EI ionization.
Immediately above the function bar display is a time scale that shows when the
function will be active from and for how long it will run. In this case the function
starts after 5 minutes and then runs for 35 minutes, terminating after a total elapsed
time of 40 minutes.
To open this dialog, open the MS Method from the Sample list
OR
Click
in the MS panel in the TurboMass main window.
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Figure 8 Function list showing a single function
The currently selected function is highlighted. If the display shows more than one
function, you can select a new function either by selecting it, or by moving to it
using the up or down arrow keys on the keyboard.
A more complicated function list might have four SIR functions, running
sequentially for 10 minutes each.
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Function List Editor
Figure 9 Function List showing multi functions
Up to 32 functions may be created in the function list.
A more advanced technique, Selected Ion and Full Ion Scanning (SIFI) has a mix of
MS scan and SIR functions. As an example, it may have a single full MS scan
method that runs for the entire chromatogram and multiple SIR functions timed for
the elution of specific compounds. This allows both the universality of full scan
analysis, with the ability to library search, and the higher sensitivity of SIR.
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Function List Editor
Adding a New Function
A new function can be added either by clicking one of the function buttons at the top
of the editor, or by selecting MS Scan or SIR from the Functions menu. The editor
for the function type selected will be displayed showing default values. Make any
changes required to the parameters and click OK to add the new function.
Modifying an Existing Function
An existing function can be modified by double-clicking on the function in the
function list. This will bring up the appropriate editor for the function type and allow
you to change the function information. When you have finished editing the
function, the function list display will be updated to show any changes.
Removing a Function
You can remove a function by selecting it and then selecting Delete from the Edit
menu.
Changing a Function's Start and End Times
You can change the start and end times of a function by going into its editor as
described in Modifying an Existing Function on page 208.
The Total Run Time field in the Scan Functions window shows the total run time
for all the functions. Entering a new value in the Total Run Time field and clicking
will set the maximum retention time for the experiment. The ratio of the
functions defined will be maintained. For example, if two functions are defined one
from 0 to 5 minutes and the other 5 to 10 minutes then a Total Run Time of 10
minutes will be displayed. If this value is changed to 20 (and
is clicked) then
the first function will now run from 0 to 10 minutes and the second from 10 to 20
minutes.
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Setting a Solvent Delay
A solvent delay can be set for a function list using the Solvent Delay Time control.
No data is stored during the solvent delay period, which means that solvent peaks
that would normally be seen eluting at this time on the TIC chromatogram of the
acquired data will no longer be seen. The filament in the source is turned off during
the solvent delay to prevent it from being damaged.
The <Enter> or arrow key must be pressed after changing the solvent delay.
Multiple Solvent Delays
There are instances where a chromatogram has several peaks large enough that you
would want to turn off the filament while they are eluting to protect the filament
from burn-out, and then turn it back on afterwards and continue the analysis. The
multiple solvent delay functionality is designed to accommodate this along with the
conventional solvent delay at the beginning of the chromatographic run.
The MS Method editor has a “Solvent Delay” button. When selected, it brings up a
dialog allowing up to four solvent delays to be specified.
Solvent delays are displayed in the method bar as bright green bars at the top of the
Function display, and numbered from 1 to 4. Double clicking on a solvent delay bar,
or clicking the edit button with a solvent delay selected, brings up the solvent delay
dialog. Pressing the “X” delete button or pressing the delete key with a solvent delay
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selected will remove a solvent delay. If it is between other delays, then the delays
are shuffled up.
If just one conventional solvent delay is used, only the top “End” box should be
filled in, with all the other values set to 0. Solvent delays may not overlap, and must
be entered in order of increasing retention time.
Saving and Restoring an MS Method
Saving an MS Method
1. Select Save As from the MS Method File menu to display the Save File As
dialog.
2. Enter a new File Name under which you want the MS Method to be saved, or
select an existing file from the list displayed.
3. Click Save.
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If the selected file already exists, you will be asked to confirm that you want to
overwrite the existing information. Click Save to continue, or Cancel and
specify a different name.
Restoring a saved MS Method
1. Select Open from the MS Method File menu to display the Open dialog.
2. Select the File Name of the MS Method that you would like to use, either by
entering its name or by selecting it from the displayed list, and click Open.
OR
Right-click on the desired MS Method in the Sample List and click Open.
Setting Up an MS Scan Function
The MS scan function editor is used to set up centroid, continuum and MCA
functions.
1. Click MS Scan to open the MS Scan Function Editor.
2. Enter the scan function parameters.
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Start Mass
Specifies the mass at which the scan will start. The Start Mass
must be lower than the End Mass.
End Mass
Specifies the mass at which the scan will stop. Both the start and
end masses can be selected directly from a spectrum displayed in
the Spectrum window. If you right-click and drag the mouse
across a spectrum, TurboMass will automatically enter the start
and end mass values for the selected mass range.
Ionization
Mode
Specifies the ionization mode and polarity that will be used during
the acquisition.
Do not select EI+ if a CI ion source is installed. The filament will not
regulate properly.
WARNING
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Data
Specifies the type of data to be collected and stored on disk:
Centroid — Stores data as centroided, intensity, and mass assigned
peaks. Data are stored for every scan. Almost always used for
GC/MS.
Continuum — Data are not centroided into peaks. Instead the signal
received by the interface electronics is stored regularly to give an
analog intensity picture of the data being acquired. Data are stored
for every scan.
As data is being acquired and continuously stored to disk, even when
there are no peaks being acquired, continuum data acquisition places
some extra burden on the acquisition system as compared to
centroided acquisition. Data file sizes will tend to be significantly
larger than centroided one sided, and the absolute scanning speed
(Da/sec) will be slower. You can set a threshold below which the
data will not be stored to disk, which can reduce these effects,
depending on the nature of the data being acquired.
You can set the threshold so that data considered to be “noise” can be
discarded, thereby improving data acquisition speed and reducing
data file sizes. For more information about setting instrument data
thresholds, see Setting Instrument Data Thresholds on page 70.
Multi Channel Analysis (MCA) — MCA data can be thought of as
“summed continuum” with only one intensity accumulated scan
being stored to disk for a given experiment. As each scan is acquired,
its intensity data is added to the accumulated summed data of
previous scans. An advantage of MCA is that random noise will not
accumulate as rapidly as real data and, therefore will effectively
average out over a number of scans. This will emphasize the real data
and improve the signal-to-noise ratio. A further advantage of MCA is
that as data is written to disk only at the end of an experiment,
scanning speeds can be increased and significantly less storage space
is required. The disadvantage of MCA is that as there is only one
scan, it cannot be used for time resolved data.
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Scans
To Sum
For MCA scans, this defines the number of scans to sum to create a
spectrum.
Start
Time
Specifies the retention time in minutes at which this function will
become active; that is, data acquired and stored.
End
Time
Specifies the retention time in minutes at which this function will
cease to be active; that is, data acquired and stored.
Scan
Time
Specifies the duration of each scan in seconds.
InterScan
Delay
Specifies the time in seconds between a scan finishing and the next
one starting. During this period data is stored, but not acquired.
The total time for a scan = Scan Time + Inter-Scan Delay.
Scan rate = (Start Mass – End Mass) / Scan Time (Da/sec)
Scans/sec = 1 / Scan Time + Inter-Scan time
Setting Up an SIR Function
The SIR (Selected Ion Recording) technique is typically used in those situations
where only a few specific masses are to be monitored during an acquisition. Since
most of the data acquisition time is spent on these masses, the SIR technique is far
more sensitive than “full scanning.” The signal-to-noise ratio increases with the
square root of the dwell time.
The SIR editor is used to enter the masses that you would like to monitor, and their
respective dwell time, span and inter-channel delay time.
When possible we try to monitor ions characteristic of the compound, as high in
mass and intensity as possible. High mass is desirable to minimize the probability of
chemical interference (selectivity). High intensity is desirable for sensitivity. We
also try to choose ions with low baselines for these same reasons.
1. Click SIR in the Scan Functions dialog.
The SIR dialog is displayed.
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1. Specify your parameters.
Most of the parameters are the same as those in the MS Scan Editor. However,
the following are different:
Mass
Specifies the mass to be monitored up to a maximum of 32. A
mass can be entered either by entering its value into the Mass
field and pressing ENTER or by clicking Add. The mass can be
calculated if the chemical formula of the ion is known with the
MW Calculator function in the top level Tools menu. The
mass may also be pulled directly from a spectrum displayed in
the Spectrum window. To do this, display the required
spectrum in the Spectrum window, and right-click the ions that
you wish to monitor. As you select a mass, it will appear in the
SIR masses table.
Dwell
Specifies the length of time in seconds for which the
highlighted mass will be monitored. This is normally set so
that the sum of all the Dwell times for all the target ions gives
about 10 scans across the GC peaks.
Inter
Channel
Delay
Specifies the length of time in seconds between finishing
monitoring the highlighted mass and starting monitoring the
next mass in the function.
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Repeats
This is only relevant for experiments having more than one
function and specifies the number of times we wish to execute
this Function per pass. For example, if we had two Functions
defined by their Start Time and End Time to execute
simultaneously, and the first Function has Repeats = 1, while
the second has Repeats = 3, then the second Function would
execute three times for each time the first Function executed
once. With non-overlapped Functions, better detection limits
will be obtained by increasing the Dwell time rather than the
number of Repeats.
Span
Specifies a small mass window applied centrally about the
highlighted mass. During acquisition this range will be scanned
over the specified Dwell time. This minimizes the chance of
missing the top of the mass peak. A span of zero can be set to
simply “sit” on the specified mass for maximum sensitivity.
Add
Enter values into the Mass and Dwell fields and then click
Add to add the new Mass to the list.
Change
Left-click on a mass in the list and then click Change to
change the Mass or Dwell.
Sort
Sorts the list in order of ascending Mass.
Clear All
Deletes the list of Masses.
Delete
Left-click a mass in the list and then click Delete to delete a
single Mass.
Sample List
9
Sample List
Top Level Menu
The top level desktop includes menus and toolbar buttons that allow you to create
and modify Sample Lists.
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The TurboMass Menu Toolbar
Button
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Menu Equivalent
Purpose
File… New
Create a new Sample List
File… Open
Open an existing Sample List
File… Save, or
File… Save As
Save a Sample List
File… Print
Print a Sample List
Run… Control Panel
Only applicable to previous versions of
software
Run… Start
Start an acquisition
Run… Stop
Stop an acquisition
Run… Pause Queue
Pause the queue of acquisitions
View… Spectrum
View Spectrum
View… Chromatogram
View Chromatogram
View… Map
View Map
Quantify… View Results
View Quantify Results
Tools… Search Library
Perform a Library search
Tools… Combine Functions
Combine Functions
Tools… Strip
Strip Functions
Sample List
Button
Menu Equivalent
Purpose
Tools… MW Calculator
Invoke Molecular Weight Calculator
Help… About TurboMass
Display program information, version
number and copyright
Edit… Cut
Cut the selection and put it on the
clipboard
Edit… Copy
Copy the selection and put it on the
clipboard
Edit… Paste
Paste the contents of the clipboard
Samples… Add
Add samples to the Sample List
Samples… Insert
Insert samples into the Sample List
Samples… Delete
Delete samples from the Sample List
Samples… Field…
Properties
Invoke the Field Properties dialog
Samples… Field…
Customize Display
Invoke the Customize Field Display
dialog
Samples… Field… Remove
Column
Remove a field from the display
Samples… Fill… Down
Fill down
Samples… Fill… Series
Fill series
Samples… Field… Align…
Left
Align text to the left in the current
column
Samples… Field… Align…
Center
Align text to the center of the current
column
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Button
Menu Equivalent
Purpose
Samples… Field… Align…
Right
Align text to the right in the current
column
Samples…Sample List
Wizard
Invokes the Sample List Wizard
The following icons are shown in the TurboMass GC and MS panels
Opens the GC Method Editor
Opens the Tune window
Opens the MS method
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Creating and Editing Sample Lists
NOTE: The Sample List is saved with the .RAW data file when data is acquired. If you change the
Sample ID field in the sample list and try to print environmental reports, the Sample ID
reverts back to the original setting when the files were acquired. You may want to change
the Sample ID field if you modify the sample list to acquire new samples.
Creating a new Sample List
To create a new Sample List:
1. Click
OR
Select New from the File menu to display a Sample List with one default row
displayed.
OR
Create a Sample List using the Sample List Wizard (See the Sample List Wizard
on page
2. Add the desired number of rows to the Sample List by either clicking Add Row
to display the Add Samples dialog, editing the Number to add, and clicking
OK.
OR
Selecting the desired number of rows in the Sample List, and clicking Insert.
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Opening an existing Sample List
1. Click
OR
Select Open from the File menu to display the Open file dialog.
2. Select a data file and click Open.
Creating a Sample List Using the Sample List Wizard
The TurboMass Sample List window is in a spreadsheet format, which allows easy
editing of multiple samples but this becomes unwieldy when there is a lot of
information required for each sample. The Sample List Wizard is a forms-format
equivalent display. It allows for easier editing of the large amount of per-sample
information required of environmental and QA/QC samples.
The Sample List Wizard enables you to select an existing sample list or create a new
one. Only the parameters required for the current type of analysis (VOA, SV, or
QA/QC) and current matrix (water/soil) are displayed. The controls are grouped in a
way to allow efficient entry of sample-specific data. It also provides the ability to
propagate changes made to one row to subsequent rows; a command to update vial
numbers; a command to update sample IDs. Several fields have automatic
incrementing of numeric values, and there are commands to insert, delete, and add
sample rows.
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Sample List
NOTE: All environmental reporting users should use the Sample List Wizard to ensure that all
sample information is entered.
You can enter or modify all of your environmental and QA/QC sample list parameters
using the Sample List Wizard. You can still edit directly from the Sample List.
The recommended approach to using the Sample List Wizard is to create your original
“template” sample list so that all the per-sample information is correctly filled in.
When you run later sets of samples which follow a similar sequence you may then
read in the original “template” sample list, rename it, and make your per-sample
changes in the Wizard or sample list window spreadsheet environment – which ever
you find most convenient for your current task.
More specifically the Sample List Wizard provides:
•
The ability to read an existing sample list template.
•
Only the parameters required for the current analysis (VOA, SV, or QA/QC) and
current matrix (water/soil) are displayed.
•
Grouping of controls for efficient entry of sample-specific data.
•
The ability to propagate changes made in one row to subsequent rows.
•
A command to update vial numbers.
•
A command to update sample IDs with automatic incrementing of numeric values.
Setting Up the Sample List Wizard
The Sample List Wizard dialog (started from the Samples/Sample List Wizard dialog)
provides you with the ability to select and specify an existing sample list or create a
new sample list. The display of editable sample parameters will depend on your
choice of Analysis, Matrix, and Concentration Level.
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The parameters required for the current analysis (VOA, SV, or QA/QC) and current
matrix (water/soil) are displayed. The controls are grouped in a way to allow efficient
entry of sample-specific data. It also provides the ability to propagate changes made to
one row to subsequent rows; a command to update vial numbers; and a command to
update sample IDs, including automatic incrementing of a numeric value. The
parameters are:
•
Sample List
•
Analysis
•
Matrix
•
Concentration Level
NOTE: When you select an existing sample list, the controls in the Analysis. Matrix and Levels
section are disabled and use the values in the last row of that sample list to indicate
the nature of the sample list (assumes all rows use same Analysis, Matrix and Level
settings). If there are no entries for those columns (for example, if it was created prior
to version 5.1) then the Analysis option will be set to QA/QC (and hence the other
options will show no selection).
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Sample List
Sample List
The Sample List section of the dialog provides you with the
options of either selecting a new sample list or editing an
existing sample list.
Existing sample
list
Select this radio button to edit an Existing sample list file.
When selected, the <sample list file name> drop–down list
and Browse button are enabled. All other controls in the
dialog are be disabled (i.e., Analysis, Matrix and Level
selections) as described above.
New sample list
Select this radio button to create a New sample list. When
selected, the <sample list file name> drop–down list control
and Browse button are disabled.
Select a sample list in the current Project from this field by
pressing the down-arrow icon or search for another sample list
by using the Browse button. This field is blank when the New
Sample List option is selected. Clicking the Browse button
displays the standard File Open dialog so that you can search
for a stored sample list. Typically sample lists are found in the
SampleDB directory of your Project directory (*.PRO).
Analysis
The Analysis section of the dialog is enabled when the New
sample list option is selected. There are three radio buttons for
this section: Volatiles, Semi-volatiles, and QA/QC.
Volatiles and Semi-volatiles are environmental sample types.
If either one is selected, the Matrix and Concentration Levels
sections remains enabled. If QA/QC is checked, the Matrix
and Concentration level sections will be disabled.
Volatiles
Select this radio button to indicate that the new sample list will
be used for volatile organics analysis (VOA).
Semi-volatiles
Select this radio button to indicate the new sample list will be
used for semi-volatile (SV) organics analysis.
QA/QC
Select this radio button to indicate the new sample list will be
used for general quality assurance or quality control (QA/QC)
analysis purposes.
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Matrix
The Matrix section is only enabled when you select a
Volatiles or Semi-volatiles Analysis. Other matrices can be
analyzed, but may require the use of additional scaling factors,
custom reporting templates, or external calculations.
Water
Select this radio button to indicate that the new sample list will
be used for the analysis of water samples. This (together with
the Analysis setting) determines the calculations Quantify will
use to produce concentration results. If Water is checked, the
Concentration level section will be disabled.
Soil
Select this radio button to indicate that the new sample list will
be used for the analysis of soil (or sediment) samples. This
(together with the Analysis and Concentration level settings)
determines the calculations Quantify will use to produce
concentration results.
Sample List
Concentration
Level
The Concentration level section is only enabled when you
select a Volatiles or Semi-volatiles analysis and a Soil matrix.
Different equations are used for each.
Low
Select this radio button to indicate that the expected
concentration range of soil samples to be analyzed with the
sample list.
Medium
Select this radio button to indicate that the expected
concentration range of soil samples to be analyzed with the
sample list.
OK
Clicking the OK button displays the Sample List Wizard main
window.
Cancel
Clicking the Cancel button closes the dialog and returns you to
the main Sample List window.
Help
Clicking this button displays the Help window for this dialog.
Building a Sample List
You can build a sample list manually or use the Sample List Wizard. This procedure
describes how to use the Sample List Wizard to build your sample list.
In this example we will show how to use the Sample List Wizard to build a sample list.
1. Click
OR
Select Sample List Wizard from the File menu to display the Sample List dialog.
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You can modify an existing sample list or create a new sample list. This example
shows how to build a new sample list.
2. Click the New sample list button.
3. Select the type of Analysis. Volatiles, Semi-Volatiles or QA/QC
4. Select the Matrix. Soil or Water
5. Select a Concentration level, Low or Medium.
6. Click OK.
The next dialog appears for you to enter the Sample Information and Lab
Information for each of the Samples.
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Sample List
Adding Sample to the Sample List
The Sample List window is a listing of the Row numbers and Sample IDs for the
samples in the current sample list. As long at least one sample exists in the list, a
sample is always selected. The currently selected sample is indicated with a highlight.
You can change the selected row using the up and down arrow keys or with the mouse.
If the Ctrl key is held down, the up arrow will move the currently selected sample row
up one position in the list. Similarly, with the Ctrl key held down, the down arrow will
move the currently selected sample row down one position in the list.
Enter the Sample Injection Information.
This window contains many fields required for environmental and QA/QC data.
Not all fields need to be entered since they are not used for calculations but only
displayed on the reports. They can be ignored or added later on a LIMS system.
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Sample Injection Information
File name - Enter the raw data file name.
File text - Enter additional comments about the sample.
Sample Type - Select the type of sample from a drop-down box. The following
Sample Types are displayed in the order in which they are to appear in the drop–
down list:
• Analyte
• Analyte Dup
• Blank
• QC
• Standard
• Tune Eval
• Init Calib
• Cont Calib
• Meth Blank
• Lab Control
• Spike
• Spike Dup
• Dilution
• Re-Extract
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Analytical sample with unknown concentrations
of target compounds.
Reinjection of an Analyte.
An analytical blank. For environmental and
QA/QC, use Meth Blank instead.
Quality Control sample.
Concentration calibration standard. For
environmental and QA/QC, use Init Calib or Cont
Calib instead.
DFTPP or BFB tuning check.
Initial calibration standard (e.g. one level of a 5level calibration).
Continuing Calibration standard (injected
periodically to validate the initial calibration
curve).
Analytical Method Blank. Contains all Internal
Standards and Surrogates.
Laboratory Control Sample (LCS), typically a
Cont Calib prepared from a different stock
solution to validate the Init Calib and Cont Calib
concentrations.
Matrix Spike sample.
Matrix Spike Duplicate sample.
Dilution of an Analyte. Sample List “Conc”
values for internal standards and Surrogates will
need to be adjusted if they are diluted.
Re-extracted sample.
Sample List
Sample ID - Enter this primary sample descriptor for the environmental reporting
software. This descriptor appears in the Sample List column in this window.
Vial No. - The sample position in the autosampler from which the injection will be
made.
Injection vol - The amount of sample injected into the GC. This value does not
control the injection volume (that value is in the GC Method) but it is used in
calculations.
GC column - Enter information about the GC column used for the analysis. It is
enabled if a GC is configured on the system.
Injector – Select from the drop-down list injection port (A or B) into which the sample
will be injected (this controls the Clarus GC autosampler).
% Moisture - Enter the moisture content determined for a soil sample. This field is
enabled only if the Matrix is Soil.
pH - Enter the pH of the sample.
Sample Prep Information
Date received - Date the sample was received in the lab. The date is displayed in the
short format defined in the Windows Regional settings. Clicking the down arrow
command button displays a calendar control, to enable you to select the Date received.
Dated extracted - Date the sample was extracted for analysis. The date will be
displayed in the short format defined in the Windows Regional settings.
Clicking the down arrow command button displays a calendar control, to enable you to
select the Date extracted.
Sample wt (Sample vol) - The weight or volume (depending on sample matrix) taken
for analysis. This field is enabled if the Analysis type is Volatiles or Semi-volatiles.
If the Matrix setting is Soil the caption is Sample wt and the units displayed are
grams (g).
If the Matrix setting is Water the caption is Sample vol the units displayed are
milliters (mL).
Dilution factor - Dilution factor applied to the sample. (Undiluted is 1)
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Soil extract vol - The total volume of the methanol extract. Enabled only if the
Analysis type is Volatiles, the Matrix is Soil and the Concentration level is Medium.
Soil aliquot vol - Volume of the aliquot of the sample methanol extract. Enabled only
if the Analysis type is Volatiles, the Matrix is Soil and the Concentration level is
Medium.
Extraction type - A text field that indicates how the sample was extracted.
Conc. extract vol. - The concentrated extract volume. Enabled if the Analysis type is
Volatiles or Semi-volatiles.
GPC Cleanup - A drop–down box that indicates whether or not the sample was
subject to a GPC (gel permeation chromatography) cleanup procedure. Enabled if the
Analysis type is Semi-volatiles.
Cleanup - A text field that describes any (non-GPC) cleanup procedure used. Enabled
if the Analysis type is Volatiles or Semi-volatiles.
The following parameters are informational only used for reports
Decanted - A drop–down list that indicates whether or not the sample was decanted.
Enabled only if the Analysis type is Semi-volatiles and Matrix is Soil.
Heated purge - A drop–down box that indicates whether or not a heated purge was
used. Enabled if the Analysis type is Volatiles or Semi-volatiles.
Surrogate lot ID. - A text field allowing identification of the lot number of the
surrogate standard compounds mix. Enabled if the Analysis type is Volatiles or Semivolatiles.
Vol surrogate added - An edit box that indicates the volume of surrogate standard
added to the sample. This field is enabled if the Analysis type is Volatiles or Semivolatiles.
ISTD lot no. - A text field allowing identification of the lot number of the internal
standard compounds mix. Enabled if the Analysis type is Volatiles or Semi-volatiles.
All concentration calculations for target compounds are made relative to an internal
standard
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Sample List
Click the Lab Information tab and enter the Lab Information for this sample. Lab
information displays for each Sample ID in the Sample List. These values typically
do not change on a per-sample basis, so they have been put in this second tab to
simplify the user interface.
Concentrations Display – The concentrations grid (with a horizontal scroll bar)
contains cells for you to enter standard Concentrations A to T (identical with the Conc
A to T values shown in the sample list spreadsheet display). These concentrations
levels are defined for the standard compounds in the Quantify method.
Sample Tracking
Submitter - Drop–down list of the Submitters previously entered in the
Submitter/Task Data window.
Task - Drop–down list of the Tasks previously entered in Submitter/Task Data
window. Optionally defines the list of compounds to be reported, reporting limits, and
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printouts (report methods).
Job - Text field describing the job the sample is associated with.
Contract - Text field describing the contract under which the sample is being
analyzed.
EPA sample No. - Text field defining the EPA sample number.
Case No. - Text field defining the case number.
SAS No. - Text field defining the Special Analytical Services (SAS) number.
SDG No. - Text field defining the Sample Delivery Group (SDG) number.
Lab Code - Text field containing the laboratory code.
Files
GC Method - A drop–down list enabling you to select the GC Method to be used for
the analysis.
MS Method - A drop–down list enabling you to select the MS Method to be used for
the analysis.
Quantify Method - A drop–down list enabling you to select the Quantify Method to
be used for the analysis.
Calibration Curve - A drop–down list enabling you to select the calibration file to be
used for the analysis.
Qualitative Method - A drop–down list enabling you to select the Qualitative Method
(typically the TIC library search) to be used for the analysis.
NOTE: After editing a Sample List, the Environmental Reports generated do not reflect the
Sample List until Quantify is first run on the new list.
NOTE: The Sample List is saved with the .RAW data file when data is acquired. If you change
the Sample ID field in the Sample List and try to print Environmental Reports, the
Sample ID reverts back to the original setting when the files were acquired. You may
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Sample List
want to change the Sample ID field if you modify the Sample List to acquire new
samples.
Saving a Sample List
1. Click
OR
Select Save or Save As from the File menu.
If this is a new Sample List, or the Save As option has been selected, the Save
Sample List dialog is displayed.
2. Enter a name into the File Name field and click Save.
The following characters cannot be used in the filename: / \ & . , : ? “ < >
Editing a Sample List by importing a worksheet from LIMS
The TurboMass software supports text file import for creating a Sample List from a
LIMS worklist and text file export for passing results on to LIMS. The import file
format is compatible with one generated by PerkinElmer LABWORKS™ but it can be
generated by most LIMS systems. See Appendix E
LIMS Import File Example.
The imported file contains one line per sample list row and each line will consist of
some or all of the (functional) parameters that can be defined in a row. The text file
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contains a definition of which fields (columns) the text file is defining for each sample
list row. The names used in this list will be the database field names for the columns.
Text items that contain the defined separator character (e.g. commas) must be enclosed
in quotes “ ”. If quotes are to be included in a string enclosed in quotes, they must
appear twice (e.g. “This string contains not only a comma, but also “”quotes”” within
it”).
The import operation appends the sample rows defined in the text file to the currently
displayed sample list. However, if the current sample list is ‘blank’ (following a
File/New command) the imported sample list will overwrite the blank line and append
subsequent lines. For the purpose of determining a ‘blank’ sample list, the fact that the
File Name cell is empty will be sufficient.
To import a Sample List from LIMS:
NOTE: The key thing to remember is that each Sample List file must have two sections: The
[Variable Parameter List] and the [Variable Parameter Data]. The Number of
Parameters in the [Variable Parameter List] must equal the number of values in the
Data string. For example, if the NumberOfParameters=56 then there should be 56
entries after Data= .
1. On the Sample List page, select Import Worksheet from the File menu.
The Worksheet Names dialog appears.
2. Click the drop-down button next to Look in and search for the directory
containing your files.
3. When you find your desired file, click open.
NOTE: We have provided a sample worksheet for import (Templates_LIMS_import.txt) in the
C:\TurboMass\TutorialReports.pro\SampleDB directory.
NOTE: If an error occurs during generation of the sample list, rows read from the text file that
were valid will be added to the sample list and an error message will be displayed
indicating the error. Further processing of the text file will stop at the occurrence of
an error.
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Sample List
Possible errors and the displayed messages include:
•
First line of text file does not contain column names – “The first line of the import
file must list the columns to be used”
•
Invalid name included on first line – “The first line of the import file contains an
invalid column name: <the invalid name>”
•
Incorrect number of data items on a line – “Incorrect number of items on line:
<line number>”
•
Invalid data type – “Invalid data type on line <line number> : <column name>
(<required data type>)”
Copying a spreadsheet into the Sample List
To copy a spreadsheet created in another application into the Sample List:
1. Click
OR
Select New from the File menu to display a Sample List with one default row.
2. Add rows and columns to the Sample List so that it has the same number of rows
and columns as the worksheet in the other Windows application.
NOTE: If the number of rows and columns displayed in the Sample List is not the same as in
the other Windows application, data may be lost.
3. Select the relevant area in the other Windows application and copy it.
4. To modify currently displayed rows in the Sample List Editor, position the cursor
on the cell at the top left corner of the paste area, and click Paste.
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Printing a Sample List
1. Click
OR
Select Print from the File menu to display the Print dialog.
2. Select the printer, print range, number of copies, and click OK.
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Sample List
Formatting Sample Lists
Column widths can be changed in the same way as any Windows spreadsheet.
There are many different columns of information that can be displayed in the Sample
List.
Selecting columns for display
1. Click
OR
Select Customize Display from the Field option on the Samples menu to open
the Customize Field Display dialog.
2. Select the appropriate checkboxes to include the appropriate fields (columns) in
the Sample List. The following fields can be used for GC/MS.
File Name
The analog of MS data file name.
MS Method (MS_File)
The MS method file name.
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GC Method (Inlet_File)
The GC method file name.
MS Tune File
The name of the file that contains the MS tuning
parameters. If left blank, the current tune file
settings are used.
Injector (Inlet_Switch)
Specifies the GC injector site used to introduce the
sample. “A” is the front Clarus GC injector and
“B” is the rear.
Injection Volume
Not used for TurboMass control only for
quantitative calculations.
NOTE: The injection volume is set in the GC method.
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Inlet Prerun/Postrun
The files that contain the optional GC pre/post run
program parameters.
Parameter File
(Process_Parms)
Optional Process parameter file. Available to external
processes through the MLCURSMP.TXT file.
Process
Optional post-run program to be executed after
acquiring this sample.
Process Options
Optional command line parameters for external
Process when it is executed.
Vial
Specifies the Clarus GC autosampler sample or bottle
number for injection.
Sample List
Sample Type
Sample type used during Quantify: Analyte, Standard,
QC, or Blank.
An Analyte is a sample injection with unknown
concentrations of target compounds.
A Standard is a sample injection with known,
standard concentrations of target compounds.
A QC sample is used as a quality control measure to
compare the calibration curve of the acquired data
against a known concentration. The QC field in the
Sample List has no effect on any calculations
performed. When sample quantification is performed,
the deviation of the analyte concentration is
calculated against the QC concentration and this is
shown as a percentage in the Quantify window under
the heading %Dev. To select this heading, select
Conc. Deviation from the Sample Format menu.
The value determined for a Blank sample is
subtracted from future analyte runs. From the
Quantify Process menu, select Calculate, and then
select Blank Subtract Compounds. The
quantification procedure checks through the Sample
List and subtracts the concentration of each
compound in a Blank from the corresponding
concentration in an analyte. If several blanks are
specified in a Sample List, then the preceding Blank
is used for each analyte. If no Blanks are specified or
there is no preceding Blank for the analyte of interest,
then no Blank Subtraction is carried out. Blank
Subtraction can only be done from the Quantify
window. It cannot be done from the Sample List.
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In addition the following Sample Types are added for Environmental Reporting:
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•
An Analyte Duplicate (Analyte Dup) is used when an Analyte is reprepared and re-analyzed. Typically the Sample ID remains the same.
•
The Tune Evaluation Sample (Tune Eval) is an injection of BFB (4Bromofluorobenzene) or DFTPP (Decafluorotriphenyl phosphine)
used to verify that the mass calibration, mass resolution, and relative
intensity of the mass spectrometer meets EPA-defined standard
conditions. It might only contain the tune evaluation compound, or it
might be part of the Continuing Calibration sample. It is typically
analyzed every 12 hours.
•
The Initial Calibration (Init Calib) is a multi-level calibration used
to establish the quantitative calibration curves. In most environmental
methods it is created when the mass spectrometer is new or cleaned.
Thereafter on a 12-hour basis the Continuing Calibration is analyzed
to verify that the Initial Calibration is still valid.
•
The Continuing Calibration (Cont Calib) verifies that the Initial
Calibration is still valid. It is typically a mid-level calibration sample.
It is typically analyzed every 12 hours.
•
A Method Blank (Meth Blank) sample is a blank used to verify the
complete analytical procedure, including sample preparation. It is
typically analyzed every 12 hours for VOA and every extraction batch
of 20 samples for SV.
•
The Laboratory Control Sample (Lab Control) is often similar to
the Matrix Spike Sample, but spiked into a blank matrix (clean sand
for soils or deionized water for waters) instead of a field sample
matrix. It is typically analyzed every 12 hours.
•
A Matrix Spike (Spike) sample is used to verify the quantitative
extraction (recovery) of selected compounds (surrogates) from the
sample matrix.
Sample List
•
The Matrix Spike Duplicate (Spike Dup) is a duplicate of the Matrix
Spike sample, used to evaluate reproducibility.
•
A Dilution (Dilution) sample is used when a sample’s concentration
exceeds the calibration range of the method. The sample is diluted. The
surrogates are diluted in a SV sample, but not in a VOA.
•
A Re-Extraction (Re-Extract) is a SV sample where the extraction
procedure is suspect, and the sample is re-extracted.
Sample ID
An optional user-defined tracking number assigned to
the sample.
NOTE: This field is filled in prior to acquisition if
needed in the final reports. It cannot be changed after
acquisition occurs.
Conc A-T
The concentration of a designated calibration level of
compounds within a sample. Used during Quantify.
Job
Optional Job designation assigned to the sample.
Recorded in the data file header.
Task
Optional Task designation assigned to the sample.
Recorded in the data file header.
User
Optional TurboMass User identifier. Recorded in the
data file header.
Submitter
Optional sample Submitter identifier. Recorded in the
data file header.
Conditions
User comment on analysis and/or sample preparation
conditions.
File Text
Optional Sample text description. Recorded in data
file header.
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Conditions
User comment on analysis and/or sample preparation
conditions. Recorded in data file header.
User Divisor
Divisor used during concentration calculation stage of
Quantify. Defaults to 1 if not specified.
User Factor 1…3
Multipliers used during concentration calculation
stage of Quantify. Defaults to 1 if not specified.
Spare 1-5
General purpose fields to store extra information
about the sample.
Quantify Method
The selectable method from the drop–down list. The
list is populated with .mdb files from the
<Project>\METHDB directory.
Calibration Curve
The selectable calibration curve file from the drop–
down list. The list is populated with .cdb files from
the <Project>\CURVDB directory.
Qualitative Method
The selectable method from the drop–down list. The
list is populated with .qlm files from the
<Project>\METHDB directory.
Report Method
The selectable method from the drop–down list. The
list is populated with .rme files from the
<Project>\METHDB directory.
3. To change the order in which the fields are displayed, select the name of the
field, and click
or
until a field is in the required position.
4. To view field properties, select a column heading and click
OR
Select Properties from the Field in the Samples menu to display the Field
Properties dialog.
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Sample List
5. To change the name displayed at the top of the column, enter a new name in the
Field name field.
6. To change the alignment of text in the column, select Left, Right or Center
from the Alignment list.
The text alignment in a cell, column, or row can also be changed by selecting
,
, or
, or selecting Left, Center or Right from
the area, and clicking
the Align option in the Field option in the Samples menu.
7. To save a customized Sample List format, select Save Format from the
Samples menu and enter a name in the dialog displayed.
8. To retrieve a previously saved format, select Load Format from the Samples
menu, and select the required format from the list.
Selecting areas
You can select with the mouse, the keyboard, or a combination of both of these
methods:
With the mouse:
To select:
Left-click:
A single cell
The required cell.
A block of cells
The first cell in the block, left-click and drag until the
required cells are selected.
A row
The row number.
A column
The column heading.
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The entire Sample List
The box at the top left corner of the Sample List.
With the keyboard:
Position the cursor at the top left corner of the area to be selected, hold down the
shift key, and use the arrow keys to select an area.
Inserting one or more rows
To insert a single row, click
.
OR
Select Insert from the Samples menu.
OR
Press INSERT.
To insert multiple rows, select the number of rows required and continue as for a
single row.
Editing data in a cell
Do one of the following to edit data in a cell:
1. To select data for copying, replacing data, and other standard editing functions,
select the cell using the mouse or press SHIFT+arrow key.
2. To edit a single cell, use the Cut, Copy, Paste, and standard Windows editing
commands in the usual manner, or right-click to display the following pop-up
menu.
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Sample List
Editing data in a column
The following commands may be used to edit data in a column:
Fill Down
Select an area and click
, or select Down from the Fill
option from the Samples menu to fill the selected range
with the first element in each column.
Fill Series
Select an area and click
, or select Series from the Fill
option from the Samples menu to fill the selected range
with series data. That is, if the first cell in a column is
vial1, the next will be vial2, vial3, and so on.
Insert
Click
or select Insert from the Samples menu to
insert samples into the Sample List. If a row has been
selected, a new row is inserted above the current one. If
more than one row is selected, the same number of rows is
inserted above the first selected row. If a column has been
selected, the same number of rows as were originally in the
column are inserted before the first row. The data inserted
into these new rows will continue the series from the row
above.
For example, selecting the two highlighted rows in the
figure on the left below and clicking Insert will result in
the figure on the right.
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If there is more than one number in a field, only the last number is incremented
when Fill Series is selected. For example, if the ID is Sample1run1, when Fill
Series is selected, the next field will be Sample1run2 etc.
The Cut, Copy and Paste commands can also be used to enter data. Select an area,
Cut or Copy the data and Paste to a new area.
NOTE: The Paste area must be same size as the Cut or Copy area.
Replacing data in a cell
Use one of the following methods to replace data in a cell:
250
•
Use the mouse or the arrow keys to select the cell, and enter or paste new data
into the cell to replace the previous contents.
•
Use the Cut, Copy, Paste and other editing commands, or right-click to display
the following pop-up menu.
Sample List
•
Double-click on a cell, and select an entry from a drop-down list displayed.
•
For Sample Type, select one of the displayed options.
•
Select an entry from the list or enter in a new value.
•
Enter in a new value.
Deleting rows and columns
to delete the selected rows.
To delete a row, click
If the entire table is selected, the cells are cleared not deleted.
To delete a column, select the column and click
.
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Starting the Analysis
Before starting an analysis save any changes made to the Sample List by
selecting Save from the Sample List File menu.
NOTE: The GC status must be either "No Method" or "Run Done" to successfully set up.
Otherwise GC communication lockups may occur.
Acquiring data
1. Select Start from the TurboMass top level Run menu.
OR
Click
Project
252
to open the Start Sample List Run dialog.
The name of the current project appears in this field. To
acquire data to a different project, click OK or Cancel to exit
this dialog, open another project, and restart data acquisition.
Sample List
Acquire Sample
Data
Selecting this option will acquire data for the specified
samples in the list. See the Acquisition Help file (available in
the Help menu) for more information on data acquisition.
Auto Process
Samples
Selecting this option will process the acquired data as
specified in the Process column of the Sample List.
Auto Quantify
Samples
Selecting this option will automatically start sample
quantification at the end of the Sample List.
Qualitative
Calculations
Selecting this option enables Qualitative Method Processing.
Generate
Communiqué
Reports
Selecting this option enables Communiqué report generation.
Preview Reports
Check this box to specify that the Communiqué reports
generated during processing will be displayed in a preview
window prior to printing (or saved to a file or database.
The options above allow you to acquire and immediately process and quantify data as
desired. Or you may choose to process or quantify data at a later time.
Run From Sample
To Sample
Sets the range of samples in the sample list that will be
acquired/and or analyzed. If you highlight a range of rows
before starting the analysis, the first and last rows of the
highlighted region will be displayed here.
Quantify, Qualify and Generate Reports
After Each Run
This indicates specified processing will occur after each row
in the sample List
At End of Sample
List
Indicates specified processing will occur only after the Sample
List is complete.
Process:
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Pre-Run
Specify the name of the process that will be run before the
acquisition of files in the Sample List
Post-Run
Specify the name of the process that will be run after the
acquisition of files in the Sample List.
Quantify the Data
To quantify data after it has been acquired, select Process Samples in the Sample
List Quantify menu.
1. Select the options required and click OK to start the analysis.
254
Integrate Samples
Integrates all the sample data files named in the peak list.
Calibrate Standards
Uses Integration results to form Quantify calibration curves
from all the data files in the Sample List.
Quantify Samples
Uses Integration results and Quantify calibration curves to
calculate compound concentrations from all the data files in
the Sample List.
Print Quantify
Reports
Produces hard copies of the results of integration and
quantification.
Sample List
Report Preview Window
This window displays when the Preview Reports option has been checked in the
Start Sample List Run dialog and a Communiqué report has been generated as part
of data reprocessing.
Only one report is available at a time in the preview window since each report is
displayed when it is generated and further processing of the sample list is paused
until the preview window is closed.
To review a report within this environment:
1. Use the page navigation and display tools to examine each page of the report.
Click the appropriate button to indicate the action settings regarding printing of
the current report and previewing of future reports.
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Main Report Preview Toolbar
Control
Description
The text displays the number of the current
page and the number of pages in the report.
Either side of the text are buttons that
display (from left to right):
•
The first page in the report
•
The previous page in the report
•
The next page in the report
•
The last page in the report.
Displays a single page of the report in the
preview area.
Displays the drop–down palette from which a
multi–page layout can be selected.
Selection of a multi–page option will change
the display in the preview area to that format
(assuming the report contains sufficient
pages).
A drop–down list that enabled the user to
select a zoom factor for the report display.
Displays a standard Windows Save As dialog,
enabling the user to save the current
Communiqué data source as a file, which may
later be loaded into the Communiqué
Designer as preview data when editing
templates.
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Sample List
Report Preview Action Toolbar
Control
Description
A command button that prints the current report
(where ‘print’ is defined within the Report Method)
and closes the preview window. The next report from
the sample list (if any) will be previewed.
A command button that prints the current report,
enables printing for all future reports from the sample
list (where ‘print’ is defined within the Report
Method) and closes the preview window. Future
reports will not be previewed.
A command button that causes the preview window
to close without printing the current report.
Furthermore, future reports from the sample list will
be neither previewed nor printed.
A command button that closes the preview window
without printing the current report. However, the
next report generated from the sample list (if any)
will be previewed.
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258
Quantify
10
Quantify
Introduction
This section describes how to use TurboMass to perform quantitative assays. Many
parts of the system are used to automate the acquisition, integration, quantification
and reporting of data. The Quantify window is used to view the summary of
Quantify results, calibration curves, and lists of integrated chromatography peaks.
TurboMass enables you to form Quantify calibration curves using Standard samples
containing compounds of known concentrations. The calibration curves can then be
used to calculate the concentrations of compounds in Analyte samples. For more
information, see Appendix C TurboMass Quantify Calculations.
The results of Quantify can be viewed in the Quantify Summary window.
Calibration curves can be viewed on the display and a number of Quantify Reports
can be produced. Facilities are also provided for writing Quantify information to the
Windows Clipboard for use by other Windows applications.
The TurboMass automated quantification provides a simple way of quantifying
large numbers of samples within an analysis. Data can be acquired, processed, and
reports printed without user intervention. The whole process is controlled from the
Sample List Editor, which is a very important part of the Quantify system.
You provide a list of the samples and a Quantify method describing how to process
each of the compounds within these samples.
Quantitative Processing for Environmental Analysis
Quantitative processing for environmental analysis is an extension to the TurboMass
Quantify environment. The Communiqué data model is enhanced to support the
additional data items required for environmental calculations.
It is also important to note that not all the calculations are performed by TurboMass
Quantify, and some calculations are specific to certain sample types. Some
calculations are only performed when environmental reports are generated. These
exceptions will be specifically noted.
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Two principal categories of calculations can be identified for both volatile (VOA)
and semi–volatile (SV) organic compound analyses:
•
Matrix–specific concentration calculations
•
QA/QC calculations (values associated with spiked samples
TurboMass Automated Quantification — an Overview
There are six basic stages in automated quantification:
1. Creation of a list of samples using the Sample List Editor.
2. Acquisition of each sample in the analysis.
3. Integration of data file chromatograms.
4. Formation of Quantify calibration curves.
5. Calculation of compound concentrations.
6. Printing reports of results.
How Does TurboMass Quantify and Report a List of Samples?
After data for all of the samples have been acquired, TurboMass must perform
several tasks to get from a list of samples to a printed report of their concentrations.
While you do have considerable flexibility in the control of these processes,
quantification is still a straightforward operation, consisting of the following basic
steps.
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Quantify
Integration of Chromatograms
Sample List
Sample 1
Sample 2
Sample n
Quantitation
Method
All
Compounds
Integrate
Chromatograms
Integrate
Chromatograms
Integrate
Chromatograms
Peak List
Sample 1
Peak List
Sample 2
Peak List
Sample n
Chromatogram integration is made up of two processes: smoothing and peak
detection. You specify how these processes are to be applied in the Quantify
method. The results of the peak detection are stored in a peak list that has the same
name as that of the sample data file being processed.
The Sample List indicates which sample data files are to be integrated.
Each compound in the Quantify method specifies a chromatogram trace that is to be
used to Quantify that compound. The chromatogram for each of the method
compounds is integrated and the resulting peaks are saved to a single peak list.
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Generation of Calibration Curves
A calibration curve is formed for each of the compounds in the method. Samples
that are to be used when forming a calibration are assigned the Standard type in the
Sample List. The Sample List also specifies the concentration of each of the
calibration standards.
The peak, which represents each compound, must be located within a sample's peak
list. A response value for each of the located peaks can then be calculated. For
located peaks, information such as compound name and peak response is saved in
the peak list.
For each compound, one calibration point is obtained from each of the Standard
peak lists. Calibration points are plotted as response against concentration. A
polynomial is fitted to these points to form the compound’s calibration curve. The
calibration curves are saved to a file with the same name as the Quantify Method.
The Quantify Method specifies how to locate peaks, calculate responses, and fit
curves.
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Calculation of Compound Concentrations
TurboMass calculates the concentration of each of the Method compounds for the
samples in the Sample List.
The peak, which represents each compound, must be located within a sample’s peak
list. A response value for each of the located peaks can then be calculated and saved
along with the compound name and other peak information in the peak list.
A concentration is calculated for each of a compound’s located peaks by applying
the compound’s calibration curve. Concentration information is saved in the peak
list.
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Displaying Quantify Results
Quantify displays the results of quantification in three windows.
Summary window Shows a list of results that can be ordered either by compound
or by sample.
Graphs window Shows the calibration curve for each compound in the method with
calculated statistics.
Peak List window Shows the information saved in the peak list for each sample.
The Summary window allows you to thoroughly examine the Quantify results.
To recall integrated chromatograms, double-click on a point in the summary, and
modify baselines as necessary.
Reporting Results
Four printed reports of Quantify results are available:
Quantify Compound Summary Report Displays quantification results for each of
the Quantify compounds ordered by compound.
Quantify Sample Summary Report Displays quantification results for each of the
Quantify compounds ordered by sample.
Quantify Calibration Report Gives calibration curve graph for each Quantify
compound.
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Quantify Sample Report Graphically displays all located chromatogram peaks and
tables quantification results. Report is grouped by sample.
NOTE: The Chromatogram application is opened when producing the report.
The Quantify Toolbar
The Toolbar is displayed at the top of the Quantify window. By choosing the toolbar
buttons, you can perform some common operations.
Prints the current Quantify window display in portrait format.
Prints the current Quantify window display in landscape format.
Shows the previous peak in the Summary window.
Shows current peak in the Summary window.
Shows the next peak in the Summary window.
Arranges the windows in a tiled view.
Arranges the windows in a cascaded view.
Arranges the windows in a stacked view.
Selects the current entry.
Decrements the current entry in the Summary window.
Increments the current entry in the Summary window.
Restores the default display range.
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A Step-by-Step Guide to Quantification
Creating a Sample List
The first thing that you must do when using Quantify is to create a list of samples
that you want to use to perform the analysis. These samples can be acquired
manually, but more often they will be acquired automatically using an autosampler.
The Sample List Editor has various columns such as Filename, vial or bottle
Number and Sample Type that can be filled in for each sample. Each sample is
displayed as one row in the Sample List. The Sample List Editor is part of the
TurboMass top level menu.
You need to tell TurboMass everything that it needs to know about the samples in
the list in order for it to perform a complete analysis. You must describe to the
system what each of the vials in the autosampler contains; that is, whether it
contains a standard, an analyte, a blank or a QC sample, how to acquire it, it and its
concentration(s), if it is a standard. In addition, you must specify the name of the file
in which to store the data. You may also want to add some management information
such as Sample ID, the submitter’s name, or a sample description.
For information on how to create a Sample List, see page 217.
Projects
TurboMass gives you the option to organize your work into projects. Projects are a
very useful way of organizing all of the data files, methods and results for a
particular assay into one directory structure on disk.
When you open a TurboMass project, TurboMass creates a new directory to hold all
the different files associated with this project. The advantage of using projects is that
it becomes very simple to archive everything associated with your assay because
you do not have to hunt around the disk to find the files you need and the chances of
you forgetting to save an important file are greatly reduced. You can save the
following types of files in a TurboMass Project:
•
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Raw data files.
Quantify
•
Peak lists.
•
Sample lists.
•
Quantify methods.
•
Quantify calibration curves.
•
Tuning files.
•
Scanning methods.
•
Instrument calibration files.
•
Inlet (GC) methods.
Projects are created and selected from the TurboMass top level File menu. See
Getting Started on page 23 for instructions on how to create or open a Project.
Creating a Quantify Method
A Quantify Method must be created before Integration or Quantification can be
performed.
The Quantify method describes how a data file is processed to produce calibration
curves and quantitative information. Details must be entered into the method for
each of the compounds being used in the analysis.
The Quantify Method specifies information for performing the following tasks:
•
Integration of a chromatogram trace to obtain peak information.
•
Location of the chromatogram peak relating to a specific compound from the list
of detected peaks.
•
Calculation of a response factor for the located peak.
•
Formation of a Quantify calibration curve.
•
Environmental calculations
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Quantify Method Editor
The Quantify Method Editor creates new methods and modifies existing ones. A
method selected from within the Method Editor will become the current system
method file and is used when performing Quantify operations.
Changes made to the method are not made permanent until they have been saved to
disk. Consequently, the method must be saved before it can be used to perform
quantification. This can be achieved by selecting Save from the File to update the
current method file, or Save As to save to a new method file.
When opened, the Quantify Method Editor contains the current TurboMass method.
If the current method is not available, the editor will contain default values, and the
name of the current method in the editor title bar will be set to [Untitled]. The
current method becomes the current system method file that is used when
performing quantification.
To open the Method Editor dialog select Edit Method from the Quantify menu.
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Setting method parameters:
1. Enter the name of the compound in the Name field.
The compound name can be up to 30 characters in length. The names of the
compounds in the method appear in the Compound list.
2. Select the internal reference compound in the Internal Ref field. Set this
parameter to [None] if the compound is not using an internal reference standard
Only compounds that appear in the compound list can be selected.
3. Select the Data Source of the peak for the selected compound:
•
MS – Mass spectral data will be used
•
GC-A – The GC detector from channel A will be used (i.e., a .raw data file
from this detector).
•
GC-B – The GC detector from channel B will be used (i.e., a .raw data file
from this detector)
If a GC detector is selected, most of the MS specific options will be deactivated
(for example, Quantity Trace, Acquisition Function Number, Relative Retention
Time, REV Fit Threshold, and the Spectrum display).
4. Set Quantify Trace to the trace descriptor of the chromatogram being used to
quantify the compound, as follows:
• A single decimal number for mass chromatograms.
• A range of masses (for example, 280 – 286 will sum the intensity of m/z
280 to m/z 286).
• TIC for total ion current chromatograms.
• BPI for base peak intensity chromatograms.
The Quantify Trace parameter specifies a chromatogram to be integrated when
TurboMass is performing automatic peak detection, and is used during the
locate phase when TurboMass is matching peak list entries against method
compounds.
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Quantification on a selected mass chromatogram is usually preferred for
sensitivity and selectivity. Ideally, the ion should be:
•
Characteristic of the compound
•
Have a high relative intensity
•
A low background level
•
As high in mass as possible - consistent with the previous requirements.
NOTE: TurboMass enters this value automatically if you use the mouse to enter the Peak
Location parameters. Be sure to verify that it is the best choice for avoiding coeluting compounds. See Peak Location parameters in step 7.
5. For multifunction data, select which function number is to be used to quantify
the current compound from the Acquisition Function Number drop-down list.
6. Set the Concentration of Standards parameter to the Sample List column that
contains the compound’s concentration level within each Standard or QC sample.
If the compound is an Internal Standard and it is at the same concentration in all
samples, the Fixed option can be selected.
The software allows up to 20 concentration levels within a single sample. For
example, if one group of compounds is initially at 50 ppb, a second group is at
100 ppb, and a third is at 400 ppb, these three concentration levels can be
defined as Conc. A, Conc. B, and Conc. C. As the standard is serial-diluted,
change the values assigned to Conc. A, B, and C in the Sample List to reflect the
new concentrations.
7. Set the Peak Location parameters to determine how a peak within a peak list is
identified as matching a method compound. A peak can be classified as a match
according to its Retention Time or Relative Retention Time, whether it falls
within the specified Time Window, and whether it satisfies the Peak Selection
criterion.
Retention
Time
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If selected, a peak within a peak list is identified as a match if it
elutes at the Retention Time specified and within the Time
Window specified.
Quantify
Relative
Retention
Time
If selected, a peak within a peak list is identified as a match if it
elutes at the time at which the compound is expected to elute
relative to the compound specified in the Internal Ref text field.
8. Set the Retention Time or Relative Retention Time and Time Window
parameters in one of the following ways:
Using the mouse:
a)
Arrange the TurboMass display so that you can see both the Quantify Method
Editor and the Chromatogram window showing the chromatogram you want to
use.
b)
Select the Compound for which you want to set parameters in the Method
Editor.
c)
Right-click at one end of the chromatogram region of interest, and drag the
mouse horizontally to the other end. As you drag the mouse, TurboMass
indicates the range you have selected. When you release the mouse, the Quantify
Method Editor window will be updated to show the new Time Window and the
Retention Time or Relative Retention Time will be set to the middle point of
the Time Window.
d)
The Quantify Trace parameter will be set to the same type as the chromatogram
selected with the mouse (TIC, BPI, or mass chromatogram).
e)
The Retention Time or Relative Retention Time parameters can also be
selected by right-clicking the chromatogram on the peak apex.
The spectrum may be inserted by copying it from the Spectrum window with
Edit/Copy Spectrum List and then selecting the Edit/Paste Spectrum menu bar
item in the Quantify Method Editor.
If there is a significant degree of chromatographic or spectral background, the
best approach to "purify" the spectrum is as follows:
1. Perform a background subtraction in the Chromatogram window using the
Process/Combine Spectra operations described in Strip and Combine
Functions on page 471.
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2. Edit/Copy Spectrum List in the Spectrum window.
3. Edit/Paste Spectrum in the Quantify window.
To remove specific contamination peaks from the spectrum, paste the spectrum
into a text editor or spreadsheet and edit it before pasting it into the Quantify
window.
Using the keyboard:
a)
If Retention Time is selected, set it to the time in decimal minutes at
which the compound is expected to elute, and set the Time Window
parameter as described in step 7.
b) If Relative Retention Time is selected, set it to the time at which the
compound is expected to elute relative to the compound specified in the
Internal Ref field. The value specified here is a multiplication factor that is
applied to the time at which the internal reference compound elutes. This
can be used to handle situations where some drift may occur in the time at
which compounds elute, but their relative retention times remain constant.
9. If you selected Retention Time, set Time Window to specify by how much the
compound elution time may vary.
The Time Window is applied either side of the predicted retention time to give a
valid window. The Time Window also defines the chromatogram range that will
be integrated.
10. Set Peak Selection to specify which peak should be located where more than
one peak is detected within the time window. By default, the peak Nearest to
the specified retention time will be selected. Other retention time-based options
that can be selected are Largest peak and First peak or Last peak in the
specified time window.
NOTE: The setting for the Peak Selection control will determine the appearance of the lower
part of the window.
•
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Select Spectrum for the best match to the reference spectrum and specify
the Rev Fit Threshold to do a reverse search test in peak selection. Only
Quantify
peaks above the specified Rev Fit Threshold value are considered for the
match. The REV Fit Threshold control will be enabled and the spectrum
display will be visible.
NOTE: Quantify does not perform background subtraction or AutoRefine during Spectral
peak matching. . For example, when using spectrum data objects in a Communiqué
report template, check the Spectrum Properties to make sure the Background
treatment is set to None to match this behavior..
•
When you select Multiple Ion Ratio - to Quantify Trace the spectrum plot
is hidden. The Qualifier Ion table, the Tolerance and the Coelution window
controls will be visible. The REV Fit Threshold is enabled.
•
When you select Multiple Ion Ratio - to Base Peak the spectrum plot
control is hidden. The Qualifier Ion table, the Tolerance, Coelution
window, Quantify Trace Target Ratio and Tolerance controls will be visible.
The REV Fit Threshold is enabled.
•
any other selection - The spectrum plot will be visible (and the multiple
ion controls hidden) but REV Fit Threshold will be disabled.
11. Optionally specify the User RF Value. The User RF Value is used in cases
where there are no calibration standards to plot a calibration curve. It represents
the gradient of a curve and is used as a multiplication factor that will be applied
to peak responses for the current compound to determine concentrations.
12. Optionally set the User Peak Factor. This value is a multiplication factor that
will be applied to all calculated concentrations for the current compound. If the
User Peak Value is left at zero or set to 1, the concentration values will not be
changed.
13. Optionally set the Reporting Threshold value (in concentration units) to filter
quantitative results in reports. This value is passed to Communiqué via the data
source.
IMPORTANT:
The Reporting Threshold value will be used as the Reporting Limit for
the purpose of setting flags on Form 1 and determining what Compounds
to show for Compound on the general environmental Quantitative Report
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(PKIEnvQuant template) if no Custom Compound List (which includes
Reporting Limits) is defined.
14. Optionally set the Standard Concentration Factor (Std Conc Factor). Set this
parameter on a per compound basis and it is used by Quantify to adjust the
concentration values in 'standard' samples in the sample list (including 'Init Calib'
and 'Cont Calib') prior to calibration of the compound.
Because TurboMass only provides for 20 unique concentration values (A thru T) in
the sample list, an alternative mechanism is required for analyses (such as
environmental work) where multi–level calibration of a large number of compounds
can lead to the need for hundreds of distinct standard concentration values. The
Standard Concentration Factor is the factor by which the designated concentration in
the sample list (A thru T) must be multiplied in order to result in the actual
concentration in the standard sample. Since only one Standard Concentration Factor
will be defined for each compound it is requirement that the standards will be
prepared by serial dilution.
Example of usage:
Compound A specifies 'Concentration of Standards' = Conc A and has a
'Standard Concentration Factor' of 1.1155. The Calibration type is Linear Fit.
The processed sample list includes four 'Standard' rows for which the contents
of column A are 10, 20, 50 and 100.
The actual concentration values used in generating the calibration curve (for
graphic displays and for calculating the linear equation) will be:
11.155, 22.31, 55.775 and 111.55.
Setting General Parameters
1. From the Quantify Method Editor dialog, click General Parameters to display
the General Method dialog.
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To use the General Parameters for all compounds in the method, select
Propagate General Parameters from the Quantify Method Editor Edit menu.
A check mark will appear next to this option, and the general parameters will be
copied to all compounds in the method.
Response
Response parameters in the General Method dialog determine
how the response value of a located peak is to be calculated. The
response values are used to form calibration curves for
compounds from standard samples and to calculate the
concentration of compounds within analyte samples.
2. Set the Response Type to Internal (relative) or External (absolute).
Select Internal (relative) if a compound’s response is to be calculated using an
Internal Standard, in which case, the Internal Ref parameters in the Quantify
Method Editor must have the Internal Standard compound selected.
Select External (absolute) if compound does not have an Internal Standard, the
response is then taken as the absolute peak height/area.
3. Select Response Areas or Heights to specify whether the responses for the
compound of interest will be based upon peak heights or areas.
Calibration parameters in the General Method dialog determine how a
compound’s calibration curve is to be formed.
4. Select the type of calibration curve, Average RF, Linear, Quadratic, Cubic or
Quartic, from the Polynomial Type drop-down list.
Average RF
Produces a calibration, which is a straight line through the origin
and through the mean response factor of the calibration points. A
response factor is the response of a calibration point divided by its
concentration. This option should be selected for compounds with
a fixed concentration.
Linear
Performs a linear regression on the compounds calibration points.
Quadratic
Performs a second order regression on the compounds calibration
points.
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Cubic
Performs a third order regression on the compounds calibration
points.
Quartic
Performs a fourth order regression on the compounds calibration
points.
NOTE: There must be one more calibration level than the order of the curve. For example,
a linear curve needs two points, a quadratic curve needs three points, and so on. An
Included or Forced origin counts as one calibration level.
5. Select Point of Origin to Exclude, Include or Force.
At the point of origin it is assumed that zero concentration has a response of
zero. If Polynomial Type is set to RF, this parameter is not used.
Force
The calibration curve will always pass through the origin.
Include
The point of origin will be included in the calibration curve
regression, the curve will not usually pass through the origin.
Exclude
The origin will be ignored when forming the calibration curve.
6. Set the calibration Fit Weighting to None, 1/X, 1/X^2, 1/Y or 1/Y^2.
This parameter is used to give higher priority to calibration points with a low
concentration or response when using regression to fit a calibration curve. This
generally results in the calibration curve being fitted closer to points at low
concentrations, thereby reducing the relative error at these points. Normally, this
parameter is set to None.
7. Set the Axis Transformation parameter to the required option. The available
options are None, LN (Natural Log), Log (Base 10 Log) and Square Root.
The transformation is applied to the concentration and response values before
the calibration curve is fitted. These transformations are useful with very wide
dynamic range data to prevent all the low-concentration data points from being
visually compressed together on the calibration curve.
Axis transformations cannot be used with RF type curves, curves that use point
weighting or curves that include or force the origin.
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8. If required, set the Concentration Units parameter.
The value set here will be used on the concentration axis of calibration curves
and in the concentration column header in the Summary Report.
Mapping of Retention Time to Relative Retention Time
When Retention Time is the selected Peak Location mode and the compound has
an Internal Reference defined, then the software will calculate the appropriate value
for the ‘Relative Retention Time’ field and display it in that (disabled) field to 3
decimal places. The calculated value will be:
RT (Current Compound)
RRT = ——————————
RT (Internal Reference)
When you enter a new value for RT the displayed RRT value will be updated when
focus leaves the RT field.
Similarly, if Relative Retention Time is the selected Peak Location mode and the
compound has an Internal Reference defined, then the software will calculate the
appropriate value for the Retention Time field and display it in that (disabled) field.
The calculated value will be:
RT = RRT (current compound) x RT (Internal reference)
When you enter a new value for RRT the displayed RT value will be updated when
focus leaves the RRT field.
If you change the compound defined as the Internal Reference for the current
compound then the value in the selected/enabled Peak Location field will be used to
calculate a new value to be displayed in the disabled field.
If a compound does not have an Internal Reference defined (or has one which is then
changed to “[None]”) then the RRT radio button will be disabled and the RRT field
will remain disabled and blank.
Both RT and RRT values will be saved in the quantify method file. However, when
the file is opened again in the editor only the ‘active’ data value will be read from
the file, the other value will be calculated as described above.
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Updating of Analyte RTs from Internal Reference
To simplify the process of updating retention times of analytes in complex quantify
methods this option updates RTs of analytes when the RT of their internal reference
peak is modified.
If the current compound is used as an Internal Reference by other compounds then
when its RT is modified and you click the Modify button a dialog will be displayed
asking you if the RTs of the associated analytes should be updated as well.
If you click the ‘Yes’ button then all compounds that use that Internal Reference
(standard) will have their RTs modified according to the equation:
RTa' =
RTi'
× RTa
RTi
Where:
RTa' is the new retention time of the analyte compound
RTi' is the new retention time of the internal reference (standard)
RTi is the old retention time of the internal reference (standard)
RTa is the old retention time of the analyte compound
When the updating is complete a dialog will be displayed indicating the number of
compounds that were updated. This will act as a confirmation to the user that the
action took place.
This same sequence of events will occur if you do not click the Modify button but
respond ‘Yes’ to the ‘Entry has been modified. Keep changes?” dialog displayed
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Quantify
after you have edited the Internal Reference RT and then select another compound
or command.
Setting Multiple Ion Ratios
To set multiple ion ratios:
1. Select one of the ‘Multiple Ion Ratio’ options in the Peak Selection drop–down
list.
•
Multiple Ion Ratio - to Quantify Trace
•
Multiple Ion Ratio - to Base Peak
2. Enter an appropriate REV Fit Threshold or leave the current value.
3. Enter m/z, Target Ratio and ±Tolerance for each of up to four qualifier ions in
the grid,
OR
Paste in a spectrum previously copied from another environment. This action
will automatically add m/z and target ratio values based on the data for the four
highest-intensity ions (excluding the Quant ion). Default values for Tolerance
will also be entered automatically. You may then edit any of these values if
desired.
NOTE: If the ‘Multiple Ion Ratio – to Base Peak’ is selected then Target Ratio and
±Tolerance values must be entered (below the grid) for the Quantify Trace.
4. Accept the default Tolerance type or select the desired alternative from the
drop–down list.
5. Accept the default Coelution Window value or enter the desired value.
Qualifier Ions
Type into the grid to define or modify the qualifier ions but the grid can also be
filled in automatically using AutoBuild or by pasting a spectrum from the clipboard.
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When the AutoBuild process is used (Chromatogram/Library Search Peaks etc.) the
Paste Chromatogram command will have the following effect when the current
setting of Peak Selection is ‘Multiple Ion Ratio – to Quantify Trace’ or ‘Multiple
Ion Ratio – to Base Peak’.
•
The largest peak from the spectrum will be entered as the Quantify Trace, as
occurs currently in TurboMass.
•
The next four largest peaks will be entered as the qualifier ions. The Target
Ratio values will be set according to the ratio of each ion to the quantify ion
from the spectrum. The Tolerances will be set to the default value.
When the current setting of Peak Selection is ‘Multiple Ion Ratio – to Base Peak’
the Quantify Trace ‘Target Ratio’ will be set to its relative intensity in the pasted
spectrum and the ±Tolerance will be set to the default value.
Pasting a spectrum will have the following effect when the current setting of Peak
Selection is ‘Multiple Ion Ratio – to Quantify Trace’ or ‘Multiple Ion Ratio – to
Base Peak’:
•
The largest four peaks, excluding the Quantify Trace, will be entered as the
qualifier ions. The Target Ratio values will be set according to the ratio of each
ion to the ion indicated by the Peak Selection setting (i.e. to the Quantify Trace
or to the Base Peak). The Tolerances will be set to the default value.
m/z- Mass of the qualifier ion, displayed to two decimal places.
Target Ratio- The expected intensity of the qualifier ion to the quant ion (as a
%), displayed to one decimal place.
±Tolerance (%) - The variance permitted in the actual intensity ratio from the
set Target Ratio, displayed to one decimal place. Use of this value is different
depending on the tolerance type set in the Tolerance drop–down list.
Quantify Trace: Controls for defining the Target Ratio and ±Tolerance for the
Quantify Trace (where applicable).
Tolerance - Control to set type of tolerance test applied to qualifier ions.
Coelution Window (sec) ± - Control to set allowed time window for qualifier
ions to maximize.
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Setting Quantify Method Peak Integration Parameters
The Peak Integration parameters are used when automated chromatogram peak
detection is being performed. You can set integration parameters for each compound
or for all compounds within the method.
The facility to set different integration parameters for different compounds can be
useful where peak characteristics such as peak width or shape vary between different
compounds. For more detailed information on integration, see Processing
Chromatograms on page 405.
Small peaks may optionally be removed by setting one of the four available
threshold parameters: Relative height, Absolute height, Relative area, and
Absolute area.
Setting quantify method peak integration parameters
1. To use the same integration parameters for all compounds in the method select
Propagate Integration Parameters from the Quantify Method Editor Edit
menu.
A check mark will appear next to this option and the integration parameters will
be copied to all compounds in the method.
By default, integration will take place over the chromatogram range defined by
the Time Window parameter in the Quantify Method.
2. If you want to integrate over a larger window, select Integrate Window from
the Quantify Method Editor Edit menu to open the Integration Window dialog,
and specify a multiplication factor.
This factor will be applied to the location window to calculate the integration
window and is the same for all compounds in the method.
3. To define the integration parameters, click Integrate Parameters on the
Quantify Method Editor dialog to open the Integrate chromatogram dialog.
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4. Enter the Noise Peak-to-peak amplitude value used by the integration software
to pre-filter the chromatogram by measuring a suitable value directly from a
chromatogram.
5. Right-click and drag the mouse across a section of noise in the chromatogram.
Then manually adjust this value to fine-tune the sensitivity of the integration
algorithm.
OR
Enter a value into the Peak-to-peak amplitude field.
6. Click Copy and Paste as necessary to read and write integration parameters to
and from the Windows Clipboard.
This approach can be used to transfer integration parameters between
Chromatogram and the Quantify Method, which can be useful when
experimenting to find the correct integration parameters using Chromatogram.
Smoothing the chromatogram before integrating
1. Select the Enable smoothing checkbox.
2. To examine and edit the smoothing parameters, click Smooth on the Integrate
chromatogram dialog to open the Smooth chromatogram dialog.
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3. Set the Window size parameter to the half-width of the smoothing window in
scans by right-clicking and dragging the mouse across a chromatogram peak or
by entering a value in the field.
4. Set the number of times the smooth is repeated, by editing the Number of
smooths parameter.
Increasing this parameter gives a heavier smooth.
5. Select a Smoothing method.
Two types of smoothing are available for chromatograms; Moving Mean and
Savitzky Golay. Both methods slide a window along the chromatogram,
averaging the data points in the window to produce a point in the smoothed
spectrum.
Moving Mean takes the arithmetical mean of the intensities of the data points in
the window.
Savitzky Golay takes an average of the intensities weighted by a quadratic
curve. This tends to enhance peak and valley shapes, as well as preserving the
height of the peaks better than the Moving Mean. However, Savitzky Golay
does tend to produce small artifacts on either side of the real peaks.
Setting peak thresholds
1. Click Threshold on the Integrate chromatogram dialog to open the Response
Threshold dialog, and examine or modify these parameters.
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2. Set the required parameters, and click OK.
Relative height
Select if you want to remove peaks whose height is less
than the specified percentage of the highest peak.
Absolute height
Select if you want to remove peaks whose height is less
than the specified value.
Relative area
Select if you want to remove peaks whose area is less than
the specified percentage of the largest peak area.
Absolute area
Select if you want to remove peaks whose area is less than
the specified value.
Setting peak detection parameters
1. You can examine and modify the parameters that control the positioning of
baselines and separation of partially resolved peaks by verticals (droplines) by
clicking Peak detect on the Integrate chromatogram dialog.
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Join
valleys
Affects how baselines for partially resolved peaks are drawn. The larger
the value of this parameter, the more peak baselines will be drawn up to
the valleys between unresolved peaks. The default value for this
parameter is 30 %, and normal operating range is
5 % - 75 %.
Reduce
peak
tailing
Allow control over the positioning of baseline end points. The default
value for the reduce peak tailing parameter is 50 %, and normal
operating range is between 25 % and 300 %. The Raise baseline
parameter prevents the baseline end point from moving too high up the
peak. To prevent the baseline endpoints from moving up the peaks,
reduce the value of this parameter. The default value is 10 %, and
normal operating range is 5 % - 20 %. This parameter is only relevant
when the Reduce peak tailing parameter has a small value (less than
50 %).
and
Raise
baseline
Draw
vertical
Determines how well resolved peaks must be before they are separated
by a dropline (or baselines are drawn up into the valleys, depending on
the value of the Join valleys parameter). If you want poorly resolved
peaks to be separated, increase the value of this parameter. The default
value is 90 %, and normal operating range is 50 % - 100 %.
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Detect
Shoulder
peaks
You can optionally attempt to detect completely unresolved peaks, or
shoulders, by selecting the Detect Shoulder Peaks checkbox. The
algorithm will detect a shoulder if the slope of the shoulder top is less
than the specified percentage of the steepest slope on the peak.
Therefore, to make shoulder detection more sensitive, increase the value
of this parameter. The default value is 30 %, and normal operating
range is 20 % - 90 %.
Setting Environmental Reporting Parameters
The environmental parameters should not have to be changed frequently once
established for the laboratory, however when changes are required it involves
reviewing a large number of compounds. Using the Environmental Parameters
dialogs makes interaction more convenient than the main dialog of the Quantify
Method Editor by placing all the compound-specific environmental parameters in
one place for quick viewing and editing.
The Environmental Parameters dialog displays the parameters based on the type of
the currently selected compound; Target Compound, Surrogate Compound, Spike
Compound, or Internal Standard Compound.
IMPORTANT:
Modifying any part of the Quantify Method may cause calculations to be
invalid and we strongly advise against doing this without completely
reprocessing (integrate, calibrate, quantify) the data.
To set the environmental parameters for compounds:
1. In the Method Editor, select the first compound to be modified and click the
Environmental Parameters button
OR
Choose Environmental Parameters… command in the Edit menu.
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2. If the compound Type setting is not correct, select the appropriate value
from the drop-down list on the right side of the dialog. In the above example
the Type is Surrogate.
3. Modify numeric parameter fields as required.
4. Click Modify to accept the changes for the current component but leave it
selected, or, click Previous or Next to accept the changes and move to a
new component.
5. After making all required modifications, click OK to save the revised
method (or Cancel to abandon all changes and leave the method
unchanged).
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Environmental Parameter Settings
The Environmental Parameters dialog displays when you click the Environmental
Parameters button in the main Quantify Method Editor window (or choose the
Environmental Parameters… command in the Edit menu). The specific form of the
Environmental Parameters dialog depends on the type of the currently selected
compound. If the Type is Internal Standard a dialog appears with the Type, CAS
number and Abbreviation parameters.
If the Type is Target the following dialog appears:
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Compounds: A list view of all compounds defined in the Quantify Method. The
currently selected compound row will remain highlighted. The list displays:
•
The compound number (this will be the same number displayed in the main
Quantify Method Editor window). Clicking on # Sorts the compounds in the
order in which they appear in the Quantify Method main window (or reverse
order if clicked again).
•
The compound type – Target, Spike, Surrogate or Internal Standard. (see also
Type control). Clicking on Type sorts the compounds by type in alphabetical or
reverse alphabetical order (or reverse alphabetical order if clicked again).
•
The compound name, as it appears in the main Quantify Method Editor
window). Clicking on Name sorts the compounds by name in alphabetical (or
reverse alphabetical order if clicked again).
Type - A drop–down list that indicates the nature of the compound: Target,
SMC/Surrogate, Spike, or Internal Standard.
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NOTE: A compound cannot be designated as an internal standard within this dialog. The
use of a compound as an Internal Reference within the main Quantify Method Editor
window defines it as an internal standard and will cause the Int Std selection to be
displayed in this control as read–only.
CAS number - An edit box specifying the Chemical Abstracts Service number for
the compound.
Abbreviation - An edit box specifying the abbreviation to be used for the
compound on Forms 2 and 8 (i.e., this is only used for Surrogates and Int. Stds.)
Maximum in blank - An edit box that indicates the maximum amount permitted
(0.0000 to 9999.9999 or left empty) in the method blank before a ‘B’ flag will be
assigned. If the concentration is larger than this value a ‘B’ flag will be assigned on
Form 1 and Form 1 TIC.
NOTE: “B” flags (indicating blank contamination) are not set when the compound
concentration is less then the MDL. If you do not wish to see the “B” flag, you may
set the Maximum in blank value equal to the Reporting Threshold.
MDL: Water - An edit box to indicate the MDL (minimum detection limit) for the
selected compound in water samples. Concentrations below this value will not be
reported. This control is not available for internal standards.
MDL: Soil - An edit box to indicate the MDL (minimum detection limit) for the
selected compound in soil samples. Concentrations below this value will not be
reported. This control is not available for internal standards.
NOTE: For the purposes of environmental reports, the term MDL is used to indicate the
threshold value for the “U” qualifier flag. Values below this threshold value will
flag the compound with a “U” in the Form 1 report and no concentration value will
be printed.
NOTE: When using a Minimum Detection Limit (MDL) and Reporting Limit values, the
TurboMass software handles the calculations for a straight dilution by using a
dilution factor. However, if you modify the samples (e.g., volumes or weights) then
you should refer to the EPA equations (specified in OLM04.2 or SOM11) to adjust
the MDL and/or Reporting Limits for differences between the nominal (specified in
the method) and the actual sample volumes and weights.
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Response Factors
For each target and surrogate compound you can define:
Minimum RRF - An edit box that defines the minimum acceptable RRF (Relative
Response Factor to the internal standard) for this compound (0.0000 to 9999.9999 or
left empty) in initial and continuing calibrations.
IMPORTANT:
If you change the Minimum RRF value, Maximum % RSD value and/or
Maximum % Difference value, you must reprocess (recalibrate) the
sample list for this new value to be used in the calibration acceptance
testing.
Maximum % RSD (Init Cal) - An edit box that defines the maximum acceptable %
RSD (percentage relative standard deviation, 0.0 to 100.0 or left empty) between
response factors calculated for each concentration level of the initial calibration.
Maximum % Difference [Maximum % Drift For compounds using curve fit] An edit box that defines the maximum acceptable percentage difference between the
RRF calculated for this compound from the continuing calibration and the average
RRF from the initial calibration. For compounds using curve fit (e.g., linear least
squares) this becomes the ‘Maximum % Drift’ – the acceptable difference between
the concentration calculated for the compound in the continuing calibration standard
using the calibration equation and the known concentration.
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Surrogate/SMC
This dialog contains all of the above parameters plus the following:
Concentration - An edit box that defines the amount of the compound used to spike
the sample.
Low Recovery limits: Water and Soil - An edit box that defines the minimum
acceptable recovery percentage for the compound (spike or surrogate) in a Water
sample and a Soil sample.
High Recovery limits: Water and Soil - An edit box that defines the maximum
acceptable recovery percentage for the compound (spike or surrogate) in a Water
sample and a Soil sample.
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Matrix Spike
This dialog contains all of the above parameters plus the following:
RPD Limit for Water - An edit box that defines the maximum acceptable RPD
(relative percent difference) value between the matrix spike and matrix spike
duplicate recoveries, for water samples.
RPD Limit for Soil - An edit box that defines the maximum acceptable RPD
(relative percent difference) value between the matrix spike and matrix spike
duplicate recoveries, for soil samples
To Set QA/QC Limits
The QA/QC limits are a set of values that apply to all compounds (global
parameters) in the method. For this reason the QA/QC Limits dialog is accessed
from the Method Editor Edit menu rather than from a button in the compound list
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section of the Method Editor since all items in this dialog are global to the method
and not compound-specific.
To set QA/QC Limits:
1. From the Method Editor, select QA/QC Limits from the Edit menu.
2. Make the following entries then click OK.
Internal Standard Area Lower Limit (% – ) - The value (from 0 to 100) that
defines the acceptable lower limit of the area measured for each internal
standard peak in a sample, compared to that in the most recent continuing
calibration, or mid–level of the initial calibration if no continuing calibration has
yet been performed.
Internal Standard Area Upper Limit (% + ) - Enter a value (from 0 to 100)
that defines the acceptable upper limit of the area measured for each internal
standard peak in a sample, compared to that in the most recent continuing
calibration, or mid–level of the initial calibration if no continuing calibration has
yet been performed.
Internal Standard RT Limits (min ± ) - Enter a value (from 0.00 to 999.99)
that defines the acceptable limits for the actual retention time of each internal
standard peak in a sample, compared to that in the most recent continuing
calibration, or mid–level of the initial calibration if no continuing calibration has
yet been performed.
QA/QC Calculations
The following equations apply to both volatile and semi–volatile organics,
and to all matrix types.
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Recoveries
The recovery calculation shall be performed for each system monitoring
compound/surrogate standard in all samples, blanks, matrix spikes and matrix spike
duplicates.
% Recovery =
Concentrat ion (amount) found
× 100
Concentrat ion (amount) spiked
where:
Concentration (amount) found is calculated using the appropriate matrix specific
equation
Concentration (amount) spiked is taken from the Quantify Method
Matrix Spike/Matrix Spike Duplicate Recovery
These calculations require that three data files be identified:
•
An analyte sample (Analyte or Analyte Dup sample type in the
sample list)
•
A spiked sample that was prepared from the original analyte sample
(Spike sample type in the sample list)
An optional third sample can also be identified.
•
A second spiked sample prepared independently from the original
analyte sample (Spike Dup sample type in the sample list)
NOTE: Because these calculations require that the user has indicated unambiguously
which three data files are involved, they will only be performed during the process
of environmental report generation.
The concentration of the matrix spike compounds is calculated using the same
equations as used for the target compounds. The percentage recovery shall then be
calculated as follows:
Matrix Spike Recovery =
SSR - SR
× 100
SA
where:
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SSR
SR
SA
Spiked sample result - calculated concentration from the Spike (Matrix Spike) or
Spike Dup (Matrix Spike Duplicate) sample
Sample result - calculated concentration from the unspiked Analyte sample
Spike amount added - taken from the Quantify Method
The relative percent difference (RPD) of the recoveries of each compound in the
matrix spike and matrix spike duplicate shall be calculated as follows:
RPD =
abs(MSR - MSDR)
× 100
½(MSR + MSDR)
where:
MSR
MSDR
Matrix spike recovery - calculated from the Spike and Analyte sample pair
Matrix spike duplicate recovery - calculated from the Spike Dup and Analyte
sample pair
Since the numerator is calculated from the absolute value of the difference between
the recoveries, the RPD is always expressed as a positive value.
AutoBuild: Automatically Building a Quantification Method
After a chromatogram is labeled with the desired names, the names, retention times,
spectra, and largest ion can be automatically used to build a quantification method.
See the following procedure.
1. In Chromatogram, expand the time axis to the range of interest by dragging the
left mouse button.
2. Select Integrate from the Process menu. Drag the right mouse button over a
background range of the chromatogram to set the noise peak-to-peak amplitude.
3. Click OK. This will integrate the chromatogram.
4. Select Lib Search Peaks from the Process menu. Click OK when asked to
print.
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NOTE: To save paper, you can pause the printer, and later delete the contents of the print
queue. See Avoiding Printout of Library Search Results on page 401.
5. When library searching is complete, return to Chromatogram and select Copy
Detected Peaks from the Edit menu.
NOTE: If Display Peak Name is selected, the peak name, if available, will be displayed
above the peak. (To select Display Peak Name, select Peak annotation from the
Chromatogram Display menu.) For more information on using names to label the
chromatogram, see Annotation Type Parameters on page 400.
6. Open the Quantification method by selecting Edit Method from the Sample List
Quantify menu.
It may be a new or existing method.
7. Enter the Time window you wish to use.
8. Select Paste Chromatogram from the Edit menu.
The library search name, the largest ion, the retention time, and the spectrum
will be entered into the method.
9. You may now enter any compound-specific information, such as Internal Ref.
Verify that the Quantify ions are those you wish to use.
10. Save the method.
AutoUpdate: Automatically Updating Retention Times in the Quantify
Method
To automatically update the retention times in the Quantification method:
1. In the Sample List, select View Results from the Quantify menu.
2. In Quantify, select View from the Display menu.
3. Select Show Summary Window and List by Sample in the Summary section,
and then click OK.
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4. Select the data file of interest by pressing the left or right arrow icons.
5. Remove any undesired peaks by double-clicking on the peak name and pressing
DELETE, and then click OK.
6. When you are ready to update the Quantification method with the retention
times in the list, select Update Retention Times from the Process menu.
CAUTION
The update is immediate and irreversible.
Creating a new Quantify method
1. Select New from the Quantify File menu.
The editor parameters are set to default values, and the Compound list is empty.
The name of the current method in the editor title bar is set to [Untitled].
2. Add the desired compounds as described below.
3. Select Save As from the Quantify File menu. Enter the name of the new method
into the Save As dialog.
Selecting an existing Quantify method
1. Select Open from the Quantify File menu.
2. Select the required method file from the file selection dialog, and click Open.
The compounds within the method appear in the Compound list. The first
compound in the method is selected.
Propagating general parameters to all compounds
To use the same integration parameters for all compounds in the method, select
Propagate General Parameters from the Quantify Method Editor Edit menu.
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A check mark will appear next to this option and the general parameters will be
copied to all compounds in the method.
Propagating integration parameters to all compounds
To use the same integration parameters for all compounds in the method, select
Propagate Integration Parameters from the Quantify Method Editor Edit
menu.
A check mark will appear next to this option and the integration parameters will
be copied to all compounds in the method.
Adding a new compound
1. Enter the required information for a new compound.
2. Click Append to add the new compound to the end of the compound list.
Inserting a new compound
1. Select the entry in the compound list before which the new compound is to be
inserted.
2. Enter the required information for the new compound, and click Insert.
Modifying information for an existing compound
1. Select the entry in the compound list that is to be modified.
2. Enter the updated information, and click Modify.
Deleting a compound
1. Select the entry in the compound list that is to be deleted.
2. Click Delete or press DELETE to remove the selected compound from the list.
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Deleting all compounds in the method
1. Select Delete All Compounds from the Method Editor Edit menu.
2. Click OK to delete all compounds in the method.
Printing a Quant Method Report
You can print out Method data in two compressed formats.
1. Select Print Table from the Quantify File menu.
2. Select the desired options in the Print Method Report dialog:
Sort By
The table may be sorted by retention time, compound name,
internal reference standard, or the quantify trace ion.
Report Type
The Compact format displays the compound data in paragraph
format, taking as many lines for the compound as required. The
Extended format displays one compound per line.
Compound
Select Current to display the current compound. Select All to
display all compounds
OR
Select Range and enter the compound range in the text field.
3. Optionally, enter text for the headers and footers on the report.
4. Select Page Numbers to add page numbers to the report.
Editing the Compound Format in the Quantification Method Report
Selecting which fields will be displayed in the Quantification Method Report
Select Edit Compound Format from the Quantify Edit menu to display the
Report Format dialog.
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The fields present in the Method Report are shown in the Displayed Fields list in
the Report Format dialog. Other fields that can be added to the Method Report are
displayed in the Available Fields list.
The Method Report will display up to the maximum number of columns that will fit on
one page. To include more columns, print in landscape mode instead of portrait mode.
Appending new fields to the Method Report
1. Select the field you want to append in the Available Fields list box.
2. Click Append.
3. Repeat steps 1 and 2 as required.
4. Click OK to save the changes.
Inserting new fields in the Method Report
1. Select the field you want to insert in the Available Fields list.
2. Select the field before which you want to insert the new field in the Displayed
Fields list, and click Insert.
3. Repeat steps 1 and 2 as required.
4. Click OK to save the changes.
Removing a field from the Method Report
1. Select the field you want to remove in the Displayed Fields list.
2. Click Remove.
To remove all the fields in the Method Report, click Remove All.
3. Repeat steps 1 and 2 as required.
4. Click OK to save the changes.
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Formatting the display of a field in the Method Report
1. Select the field whose display settings you want to change in either the
Available Fields or Displayed Fields lists.
2. Change the Header field to display the heading you want to display above this
column.
3. Change the Justification setting to Left, Right or Center as required.
4. Change the Field Width and Decimal Places as required.
5. Repeat steps 1 through 4 as required.
6. To change the settings for all fields back to default values, click Default.
7. Click OK to save the changes.
Starting the Analysis
Before starting an analysis save any changes made to the Sample List by
selecting Save from the Sample List File menu.
NOTE: The GC status must be either "No Method" or "Run Done" to successfully set up.
Otherwise GC communication lockups may occur.
Acquiring data
2. Select Start from the TurboMass top level Run menu.
OR
Click
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to open the Start Sample List Run dialog.
Quantify
Project
The name of the current project appears in this field. To
acquire data to a different project, click OK or Cancel to exit
this dialog, open another project, and restart data acquisition.
Acquire Sample
Data
Selecting this option will acquire data for the specified
samples in the list. See the Acquisition Help file (available in
the Help menu) for more information on data acquisition.
Auto Process
Samples
Selecting this option will process the acquired data as
specified in the Process column of the Sample List.
Auto Quantify
Samples
Selecting this option will automatically start sample
quantification at the end of the Sample List.
Qualitative
Calculations
Selecting this option enables Qualitative Method Processing.
Generate
Communiqué
Reports
Selecting this option enables Communiqué report generation.
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Preview Reports
Check this box to specify that the Communiqué reports
generated during processing will be displayed in a preview
window prior to printing (or saved to a file or database.
The options above allow you to acquire and immediately process and quantify data as
desired. Or you may choose to process or quantify data at a later time.
Run From Sample
To Sample
Sets the range of samples in the sample list that will be
acquired/and or analyzed. If you highlight a range of rows
before starting the analysis, the first and last rows of the
highlighted region will be displayed here.
Quantify, Qualify and Generate Reports
After Each Run
This indicates specified processing will occur after each row
in the sample List
At End of Sample
List
Indicates specified processing will occur only after the Sample
List is complete.
Process:
Pre-Run
Specify the name of the process that will be run before the
acquisition of files in the Sample List
Post-Run
Specify the name of the process that will be run after the
acquisition of files in the Sample List.
Quantify the Data
To quantify data after it has been acquired, select Process Samples in the Sample
List Quantify menu.
2. Select the options required and click OK to start the analysis.
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Integrate Samples
Integrates all the sample data files named in the peak list.
Calibrate Standards
Uses Integration results to form Quantify calibration curves
from all the data files in the Sample List.
Quantify Samples
Uses Integration results and Quantify calibration curves to
calculate compound concentrations from all the data files in
the Sample List.
Print Quantify
Reports
Produces hard copies of the results of integration and
quantification.
Quantify From
Sample To Sample
Sets the range of samples in the sample list that will be
quantified.
Using the Quantify Window to Examine Results
The Quantify window contains three windows: the Summary window, the Graphs
window, and the Peak List window. You can turn each of these on and off as required.
NOTE: If a peak is missed in Quantify because of retention time or ion ratios, it is necessary
to manually integrate it before the Quantify/View Results/Process/Update Retention
Times/Ion ratios can be used for it.
Displaying the Quantify window
Select View Results from the top level Quantify menu.
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Controlling the appearance of the Quantify display
1. Select View from the Quantify Display menu to display the Quantify Display
dialog.
2. Specify the Quantify windows you want to display by selecting the appropriate
checkboxes.
You can choose to display any combination of the following: the Graphs
window showing calibration curves, the Graphs window showing residuals, the
Summary window, and the Peak List window.
3. Choose whether you want to display the Summary window listed by compound
or by sample, by selecting the relevant setting from the Summary Format dropdown list.
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A user configurable header can be displayed at the top of the Graphs or the Peak
List windows. In the default display the header is not displayed.
4. To open the Header Editor dialog, click Edit Header from the View dialog.
OR
Open the Header Editor from outside the View dialog by selecting an existing
header.
See The Header Editor on page 54 for more information about using the Header
Editor.
Controlling the appearance of the Quantify Chromatogram display
1. To display a particular peak list entry in the Chromatogram window select the
desired entry in the Summary window or the Peak List window entry.
2. To display a particular calibration standard peak, select the desired calibration
point in the Calibration Curve window. This allows manual adjustment of
integration results.
3. To control the appearance of the Chromatogram window, select Chromatogram
from the Quantify Display menu to open the Quantify Chromatogram Display
dialog.
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4. Edit your parameters.
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Show Internal
Reference
If selected, the internal reference peak (if specified)
will be shown with the current peak.
Add to existing
chromatograms
If selected, each new chromatogram will be added to
those already displayed.
Show Edit Quantify
Peak Dialog
If selected, the dialog enables you to edit the Quantify
Peak.
Display Range
Can be set to Integration to use the integration range,
Keep Current to keep range currently displayed, or
Acquisition to use the acquisition range.
Quantify
The Summary Window
The Quantify Summary window gives a summary of the results of quantification.
The results in the Summary window can either be listed by compound or by sample.
If no peak has been located for a compound entry, the peak information fields will
be left blank.
Use the Quantify toolbar buttons to display information about a new
compound/sample.
Shows previous compound/sample in Summary window.
Shows the next compound/sample in Summary window.
The Quantify Toolbar buttons can be used to display integrated peaks in
Chromatogram.
Shows the previous peak in the Summary window.
Shows the current peak in the Summary window.
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Shows the next peak in the Summary window.
The Summary window format also determines the format of printed Summary
Reports. Two Summary Reports can be printed: the Summary Report listed by
sample, and the Summary Report listed by compound.
There are many different columns of quantification information that can be
displayed in the Summary window. You can select which columns are currently
displayed. Use the horizontal and vertical scroll bars, if available, to move around
the Summary window.
The format of the Summary window listed by sample and listed by compound can
be changed independently.
The fields present in the Summary window are shown in the Displayed Fields list in
the Compound Report Table Format dialog. Other fields that can be added to the
Summary window are displayed in the Available Fields list.
Any changes made in the Compound Report Table Format dialog will be reflected in
the Summary window display and in the Summary Reports. The Summary Reports
will display up to the maximum number of columns that will fit on one page. To
include more columns print in landscape mode instead of portrait mode.
Selecting which fields will be displayed in the Summary window and
Summary Reports
Select the Summary window column headers, Output Compound Format, or
Output Sample Format from the Quantify Edit menu to display the Compound
Report Table Format dialog.
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Appending new fields to the Summary window
1. Select the field you want to append from the Available Fields list.
2. Click Append.
3. Repeat steps 1 and 2 as required.
4. Click OK to save the changes and update the Summary window.
Inserting new fields in the Summary window
1. Select the field you want to insert from the Available Fields list.
2. Select the field before which you want to insert the new field in the Report
Format list, and click Insert.
3. Repeat steps 1 through 2 as required.
4. Click OK to save the changes and update the Summary window.
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Removing a field from the Summary window
1. Select the field you want to remove in the Report Format list.
2. Click Remove.
To remove all the fields in the Summary window, click Remove All.
3. Repeat steps 1 and 2 as required.
4. Click OK to save the changes and update the Summary window.
Formatting the display of a field in the Summary window
1. Select the field whose display settings you want to change in either the
Available Fields or Displayed Fields list.
2. Change the Header field to display the heading you want to display above this
column.
3. Change the Justification setting to Left, Right or Center as required.
4. Change the Field Width and Decimal Places as required.
5. Change the Not Found parameter as required.
Not Found determines what will be printed in the Quantify report for this field
if the peak is not found. The options available are Blank, Zero, Dash, Not
found or n/a.
6. Repeat steps 1 through 5 as required.
7. To change the settings for all fields back to default values, click Default.
8. Click OK to save the changes and update the Summary window.
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Reviewing Target Compound Data (Interactive Data Review)
To review target compound data:
1. Open the Quantify window by choosing the View Results… command from
the Quantify menu.
2. With the Summary window (by Sample) displayed, double–click on a peak
to view the chromatogram, spectra and qualifier ion plots associated with
that peak.
3. To view data for the next (or previous) peak click the toolbar button:
(or
)
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To modify peak data:
1. Double-click on the compound name in the Summary window you wish to
manually integrate.
2. If the Edit Quantify Peak dialog is not displayed, select Chromatogram from
the Display menu in Quantify and make sure the Show Edit Quantify Peak
dialog is selected. Then try step 1 again.
3. Perform manual reintegration, if necessary. See Manual Peak Integration on
page 323
4. Click OK to accept the changes made and have the results display updated.
Saving the Summary window
In the Summary window, select Save Summary by Compound or Save Summary
by Sample from the File menu.
The Graphs Window
The Quantify Graphs window contains a graphical display of the current calibration
curve and/or its residuals plot. Statistical information on the calibration curve is
displayed above the graphs. A user configurable header can be displayed at the top
of the window.
The Graphs window is available if you selected Curve and/or Residuals in the
Quantify Display dialog.
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The current calibration curve file holds a calibration curve for each of the
compounds being analyzed. The toolbar within the Graphs window allows you to
easily select other calibration curves by clicking
or
.
The calibration curve graph displays concentration against response value. The
vertical axis is labeled as a percentage of the maximum response. The horizontal
axis is labeled with the concentration units specified in the method. The displayed
calibration curve shows the response value expected for particular concentrations.
Crosses mark the calibration points used to form the curve.
The residual plot displays concentration against delta concentration at the calibration
points. This shows the difference between the concentration predicted by the
calibration curve and the actual concentration at the calibration points.
Selecting another calibration curve
To select another calibration curve from within the current file, use the following
tool buttons:
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To show the previous calibration curve.
To show the next calibration curve.
To open a dialog where you can enter the number of the desired
calibration curve. Curve number 1 is for the first compound, curve
number 2 the second, and so on.
Changing the display range of the calibration curve
Both the horizontal and vertical display ranges of the Graphs window can be
expanded.
1. Left-click and drag the mouse horizontally, vertically, or diagonally from one
end of the region of interest to the other.
As you drag the mouse, TurboMass indicates the range you have selected. When
you release the mouse, the selected range will be redisplayed to fill the current
window.
Repeat this operation as often as required.
2. To restore the display to the default range, click
.
Viewing another calibration curve file
1. Select Calibration from the File menu to open the File Open dialog.
2. Select a file, and click Open.
Displaying more information about a particular calibration point
1. Select a calibration point to update the Summary and Peak List windows to
display the calibration point as the current entry.
2. Double-click on a calibration point to display the peak list entry, display the
corresponding chromatogram, and open the Edit Quantify Peak dialog.
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3. Manually adjust the baseline assignment as necessary.
4. Add any Comment that you want to store in the peak list for the selected peak.
For more information, see Manual Peak Integration on page 323.
The Peak List Window
Select Show Window from the Quantify Display View menu to display the Peak
List window.
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The Quantify Peak List window lists all the peaks in the current peak list with the
current peak selected. You can configure the columns displayed in the Peak List and
the header displayed at the top of the Peak List window.
The Peak List window displays all the information for a peak list entry. To
accommodate display space restrictions, you can select which columns are to be
displayed and the order in which order they are to appear.
Configuring the displayed Peak List columns
To select Configure Peak List columns:
1. Select Peak List Display Format from the Quantify Display menu to open the
Format DB List dialog, and then select the desired column(s).
OR
Use the mouse to select the desired column headings in the Peak List window.
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Appending new fields to the Peak List window
1. Select the field you want to append from the Fields list.
2. Click Append.
3. Repeat steps 1 and 2 as required.
4. Click OK to update the Peak List window.
Inserting new fields in the Peak List window
1. Select the field you want to insert from the Fields list.
2. Select the field before which you want to insert the new field in the Format list.
3. Click Insert.
4. Repeat steps 1 to 3 as required.
5. Click OK to update the Peak List window.
Removing a field from the Peak List window
1. Select the field you want to remove from the Format list.
2. Click Remove.
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To remove all the fields in the Peak List window, click Remove All.
3. Repeat steps 1 and 2 as required.
4. Click OK to update the Peak List window.
Formatting the display of a field in the Peak List window
1. Select the field whose display settings you want to change in either the Fields or
Format list.
2. Click Justification to open the List Field Justification dialog.
3. Change the Field Name to show the heading you want to display above the
column.
4. Select the Justification setting to Left, Center or Right as required.
5. Edit the Field Width, Significant Figures (SF) and Decimal Places (DP) as
required.
6. Click OK to update the Peak List window.
Changing the Current Peak List file
To view another Peak List, select Peak List from the File menu to display the
File Open dialog, and select a peak list.
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Displaying Peak List Chromatograms
To display the chromatogram and peak associated with a Peak List window
entry, double-click on the desired entry.
Manually Changing Quantify Results
Although TurboMass can perform a complete automated quantification analysis
from setting up a Sample List and acquiring data to printing Quantify Reports, it is
also possible to repeat individual Quantify processes and to manually edit results
including:
•
Manual editing of peak baselines.
•
Editing calibration curves to exclude erroneous calibration points.
•
Performing Quantify Locate compounds, Calculate calibration curves or
Quantify compounds processes.
Manual Peak Integration
If the automated peak detection is not determining peak baselines satisfactorily, it is
possible to define the baselines manually. This can be achieved by modifying the
peak information held in the Peak Lists or by creating them from scratch.
1. To display an integrated peak in Chromatogram, select the desired entry in the
Summary window or the Peak List window entry.
Figure 10 Chromatogram showing peak used for a calibration point
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2. To display calibration standard peaks, double-click on the desired calibration
point in the Calibration Curve window.
TurboMass opens the Chromatogram window with the relevant peak displayed.
Also, the Edit Quantify Peak dialog is opened. This displays detailed peak
information and from which you can manually adjust the baseline.
3. To modify the peak baseline, select the handles that appear at either side of the
baseline, and adjust the baseline as required.
TurboMass will update the Peak Information displayed in the Edit Quantify
Peak dialog.
4. When you are satisfied with the manual integration, click OK to save the new
peak integration information.
5. Optionally, add a Comment to be stored in the peak list for the selected peak.
The comment can be included in the printed report.
6. If no peak was detected, the chromatogram that should have contained the peak
can be displayed by using the mouse to select the appropriate Summary window
entry.
7. To add a baseline, right-click at one end of the chromatogram region of interest,
and drag the mouse horizontally to the other end.
As you drag the mouse TurboMass indicates the selected range. When you
release the mouse, a baseline will be drawn.
8. To delete the current peak, click Delete and then OK in the Edit Quantify Peak
dialog.
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The peak list and associated windows will be updated. If the peak is a
calibration standard, you will be asked if you want to recalculate the calibration
curve. If a new curve is calculated, all compounds will be requantified.
The Summary window can be formatted to include the Detection Flags for each
peak. The Detection Flags give information about the start and end points of the
peak and can have the following values:
b
Peak baseline starts or ends on the chromatographic curves
v
Peak starts or ends as a valley dropline between two peaks
s
Peak baseline starts or ends as a shoulder dropline between two
peaks
M
Peak start or end point has been manually assigned
t
Peak end was not detected within the retention time window
X
Calibration point has been excluded from the calibration curve
The default Chromatogram display range can be controlled by selecting
Chromatogram from the Quantify Display menu. For more information about
setting the default Chromatogram display range, see Controlling the Appearance of
the Display on page 397.
Excluding erroneous calibration points
If, once the calibration curves have been formed, a calibration point is seen to be
erroneous, it can be removed from the calibration as follows:
1. Select Calibration Curve from the Quantify Edit menu to open the Calibration
Curve Edit dialog.
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The Calibration Curve Editor will display a list of the calibration points used to
form the calibration curve. Each point is displayed with Peak List name,
standard concentration, residual error %, and a label to indicate whether the
point has been included or excluded from the current calibration curve.
2. To exclude a point that is currently being used to form the calibration curve,
select the calibration point in the list and click Exclude.
The label for the point will change from Include to Exclude.
3. To include a point that is not currently being used to form the calibration curve,
select the calibration point in the list and click Include.
The label for the point will change from Exclude to Include.
4. When you have finished making changes, click OK to save the changes.
You will be asked if you want to quantify compounds according to the new
calibration curve.
5. Click Yes to quantify compounds or No to keep the existing calculated
concentrations.
The calibration curve will be replotted using only the included calibration
points. Excluded points are denoted by a circle around the point. Excluded
points are denoted in the Summary reports with an X in the Detection Flags
column.
Excluding a complete sample from being used to form the calibration curve
If, once the calibration curves have been formed, all calibration points from a
particular standard sample are seen to be erroneous, the sample can be removed
from the calibration as follows:
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1. Determine which sample produced the erroneous calibration points.
2. In the Sample List Editor, find the row that contains the erroneous sample and
set the Type field to Blank. Alternatively, remove the row from the Sample List.
3. Click Start, and select the Calibrate, Quantify and Print Report options. There
is no need to integrate again.
4. Click OK to start the analysis.
Performing any of the Quantify processes
1. Select Calculate from the Quantify Process menu to open the Quantify Process
dialog.
2. Select the Quantify processes you want to perform:
Locate Compounds
Locates peaks for all compounds in the current
method.
Calculate
calibration curves
Plots calibration curves for all standards.
Quantify
compounds
Calculates concentrations for analyte samples using
the current calibration curves.
Blank subtract
compounds
When a sample defined as a blank is encountered,
the value is saved and subtracted from subsequent
samples until the next blank is encountered, this
new value is saved and subtracted from the next set
of samples.
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3. Click OK to exit.
Controlling Quantify Reports
Four printed reports of quantification results are available:
Quantify Compound Summary Report: Displays quantification results for each of
the Quantify compounds ordered by compound.
Quantify Sample Summary Report: Displays quantification results for each of the
Quantify compounds ordered by sample.
Quantify Calibration Report: Gives calibration curve graph for each Quantify
compound.
Quantify Sample Report: Graphically displays all located chromatogram peaks
and tables quantification results. Report is grouped by sample.
NOTE: The Chromatogram application is opened when producing the report.
Printing Quantify reports
1. Quantify Reports will be automatically printed at the end of a sample list
analysis if Print Quantify Reports is selected when a sample list analysis is
started.
OR
Select Print Report from the Quantify File menu to open the Quantify Reports
dialog.
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2. Choose the reports you want to print by selecting the appropriate checkboxes.
3. Click OK to save changes and open the Print dialog.
4. Set the print and print setup parameters as required.
The Quantify Report margins can be changed by clicking Margins.
5. Click OK to print the Reports.
Changing the format of the Quantify reports
1. To open the Quantify Report Format dialog, either select Report Format from
the Quantify File menu.
OR
Select Print Report from the Quantify File menu to open the Quantify Reports
dialog, and then click Format.
2. Enter the required text in the Header and Footer fields to create a customized
header and/or footer that will appear on each page of the Quantify Reports.
3. Select or deselect Page Numbers to turn page numbering on or off as required.
4. Set the Sample Report parameters to specify the number of Horizontal graphs
and Vertical graphs you want to display on one page of the Sample Report.
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5. If you want to print out a summary table of the sample results as well as the
graphs, select Display Table.
6. Set the Orientation to Portrait or Landscape for each part of the Quantify
Report.
7. Click OK to exit and save the changes.
Selecting which fields are displayed in the Quantify Summary Reports
Select Output Compound Format or Output Sample Format from the
Quantify Edit menu.
For more information about formatting Summary Reports, see Selecting which
fields will be displayed in the Summary window and Summary Reports on page
238.
Selecting the Chromatogram display range for the Quantify Sample
Report
The Quantify Sample Report uses the Chromatogram display parameters.
1. To set the Chromatogram display parameters, select Chromatogram from the
Quantify Display menu.
The Quantify Chromatogram Display dialog is displayed.
2. Select Show Internal Reference if you want the internal reference peak shown
with the current peak.
3. Select Add to existing chromatograms to display each new chromatogram to
those already on display.
4. Set the Display Range to Integration to use the integration range or to
Acquisition to use the acquisition range.
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If the Display Range is set to Keep Current, TurboMass will use the acquisition
range.
Printing Quantify windows
1. Select Print from the Quantify File menu.
2. Select to print All Windows or Current Window and click OK to print the
Quantify windows.
Printing Quantify windows using the Quantify toolbar
Prints the current Quantify window display in portrait format.
Prints the current Quantify window display in landscape format.
Writing Quantify Summary to the Clipboard
Quantify allows the equivalent of the Quantify Summary Report to be written to the
Clipboard. From there, the information can be pasted into other applications, such as
a spreadsheet. Quantify uses the currently selected Sample List, Method and Peak
List files.
The Quantify Summary Report can either be ordered by compound or by sample.
To write the Quantify summary information to the clipboard, select Copy Summary
By Compound or Copy Summary By Sample from the Quantify Edit menu.
Files Used During Quantify
Four types of files are used by the Quantify program: Sample List, Method, Peak
List and Calibration Curve. The current file of each type can be selected from the
Quantify File menu. It is recommended that you use the Projects option when doing
quantification as this allows you to organize and access your data more easily. For
more information, see Projects on page 47.
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The Sample List (.SPL) File
Three items in the Sample List are required for quantification.
File Name: Specifies the sample data file name, which will be the same name as the
corresponding Peak List file.
Type: Specifies the type of sample. This should be set to Standard if the sample is to
be used to form a calibration curve, Analyte if the concentration of the compounds
within the samples is to be calculated, QC if it is a quality control sample, or Blank
if the sample does not contain any analyte compounds.
Concentration: Only required if the sample is a standard and is optional for QC
samples. Specifies the known concentrations of the compounds within the standard.
This does not apply to compounds whose concentration has been specified as being
constant, (fixed), within all samples.
The Sample List files are normally stored in the \SAMPLEDB directory.
The Quantify Method (.MDB) File
The Quantify Method contains an entry for each of the compounds being analyzed
determining how the data are to be processed. The same method is applied to all the
samples in the analysis. For more information, see Creating a Quantify Method on
page 269.
The Method files are normally stored in the \METHDB directory.
Peak Lists (.PDB) File
A Peak List contains peaks that were detected when integrating chromatograms.
Further information gathered as a result of running Quantify, such as compound
name and concentration, is also saved in the peak list.
Peak lists are produced as a result of running the TurboMass automated Quantify
software or by the Chromatogram application. One peak list should be formed for
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each of the samples in the analysis. The peak list will have the same name as the
sample from which it was formed.
For more information on examining, modifying and creating peak lists, see
Chromatogram on page 377.
The peak list files are normally stored in the \PEAKDB directory.
Calibration Curves (.CRV) File
Stores the Quantify Calibration Curves that are produced for each of the compounds
within the method. The Calibration Curve file has the same name as the method
used to create it.
The Calibration files are normally stored in the \CURVEDB directory.
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Qualitative Method
11
Qualitative Method
Introduction to Qualitative Processing
You can determine the identity of your sample through the qualitative processing of
sample data. To do this you create a Qualitative Method of the data (that you can
specify) in each row of the Sample List. This defines the parameters required for
generating reports that do not make use of quantitative results. The parameters fall
into two main categories:
1. Definition of input data for generating a peak data set
2. Library search parameters
Qualitative processing can have one or two stages:
1. Integration of one of more defined chromatograms to generate a peak list.
2. Automatic library searching of the peak spectra and reporting of potential
‘hits’ The first step will always be carried out if a qualitative method is
specified in the Sample List. The output of this process will be a collection of
peak data which can be made available to Communiqué as a data source for
qualitative reports and/or used as input to the automatic library search.
The first step will always be carried out if a qualitative method is specified in the
Sample List. The output of this process is a collection of peak data which can be
made available to Communiqué as a data source for qualitative reports and/or used
as input to the automatic library search.
Qualitative Integration and Peak Selection
Only the number of peaks specified by the ‘Report largest n peaks’ parameter in the
Qualitative Method will be included in the data source. The steps in the processing
are:
1. Integrate each chromatogram.
The specified trace (TIC or mass) will be extracted from the specified
acquisition
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function. Peak detection and integration are carried out in the manner it is done
in the TM Chromatograms environment. Threshold values will be taken from
the Qualitative method. Integration is made with: Smooth off, Peak detect Join
= 30, Reduce = 50, Raise=5, Draw vertical = 90, detect shoulders = off.
2. Calculate Area% and Norm% values for each peak.
These values are calculated for each chromatogram separately. The peak data set
associated with a specific chromatogram is supplied via the AddData function to
any Qualitative Plot control plotting that chromatogram.
3. Combine the peaks from all chromatograms and sort the peaks in retention time
order.
•
If more than one peak maximizes within ±2 scans, eliminate all but the one
with the largest area, or the first one if there are two with equal area.
•
If ‘Exclude target compounds’ is set in the method, remove peaks that
maximize within ±2 scans of the actual retention time of the target
compound taken from the quantification results. This setting is ignored if no
quantification results are available. If this option is not checked and
quantification results exist then these results (compound name,
concentration and concentration units) will be associated with the
appropriate peak in the data source. However, Area% and Norm% results
will always come from the qualitative processing.
4. Sort in descending area order.
5. Eliminate all but the largest (by area) n peaks (where n is the ‘Largest peaks’
parameter from the qualitative method).
6. Re-sort in retention time order.
7. Add the peak data to the data source.
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Qualitative Method Editor
The main window consists of menu bar, tool bar, and three tabs of parameters.
•
General
•
Search Parameters
•
Library Settings
The General parameters are needed for all qualitative reports that require a peak data
set. Since Search Parameters and Library Settings are only required when a library
search is to be performed these have been placed on secondary tabs.
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Qualitative Method Editor Toolbar
The Toolbar is displayed at the top of the Qualify window. By choosing the toolbar
buttons, you can perform some common operations.
Creates a new qualitative method.
Opens an existing qualitative method.
Saves the current qualitative method.
Saves the qualitative method with a new name.
Prints the qualitative method.
Closes the Qualitative Method Editor.
Displays the help associated with this screen.
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Qualitative Method Editor: General Tab
To define parameters for creation of a qualitative peak data set:
•
Specify the chromatographic data sets which are to be subject to peak
detection and integration. The options are:
The full chromatogram from start to end
OR
One to four segments with specified start and end times.
•
Each chromatographic data set can be the TIC, the BPI chromatogram,
or a mass chromatogram defined with the usual TurboMass expression.
•
Define the threshold parameters for each chromatographic data set.
•
Define the default peak-to-peak noise amplitude value.
•
Set the desired number of peaks to be reported and optionally exclude
Quantify target compounds (where applicable).
•
Set a ‘coelution window’ parameter to ensure reliable identification of
target compounds within the qualitative chromatograms when the
Quantify Trace and qualitative peak do not maximize at the identical
retention time (default 1 second).
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The General Tab Fields
342
Full chromatogram
Integrate the full chromatogram to create a peak list
Window 1
Use the first data segment in creating a peak list
Window 2
Use the second data segment in creating a peak list
Window 3
Use the third data segment in creating a peak list
Window 4
Use the fourth data segment in creating a peak list
grid
Defines time segments and integration thresholds. The first
two cells in the first edit row (alongside Full Chromatogram)
are always disabled and cannot be selected.
Peak–to–peak noise
amplitude
Sets the maximum noise expected on the signal
X-Axis units:
Time - Selects Time units for setting the ‘From’ and ‘To’
values in the grid.
Qualitative Method
Scan - Selects Scan numbers for setting the ‘From’ and ‘To’
values in the grid.
Report largest n
peaks
The number of peaks to be reported.
Exclude target
compounds
Do not include target compounds in the peak list.
Coelution window
(sec) ±
Time window for qualitative and Quantify Trace peaks
to maximize and still be considered same compound.
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Qualitative Method Editor: Search Parameters Tab
To define the criteria for library search operation:
Select the treatment to be applied to the spectrum before initiating the search.
Select the thoroughness of the search (the 'Spectrum search type') and its options.
More thorough searches take longer.
Optionally select the 'Reverse search' option to improve the matching capability
when there are contaminant peaks in the mass spectrum.
Optionally restrict the mass range of the searched reference spectra if he has some
prior knowledge of the compound molecular weight. This will improve matches
where the reference spectra may have peaks outside the acquired range.
Optionally restrict the range of the matched compounds, if he has some prior
knowledge of the compound molecular weight. This will improve the match quality
by only returning results with molecular weights within this range.
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The Search Parameter Tab Fields
Spectrum Treatment
None
AutoRefine
Background
subtracted
Use original spectrum scan for search.
AutoRefine the spectrum prior to search.
Average the top 3 apex scans, and subtract the scan prior
to GC peak start.
The 'Window size' and ‘Noise threshold’ fields are enabled only when ‘AutoRefine’
option is selected.
Window size
Window size parameter for Refine algorithm.
(scans)
Noise threshold
Noise threshold parameter for Refine algorithm.
Spectrum Search Type
Identity
Specifies an Identify type search.
Specifies a Similarity type search.
<drop–down list> Defines the specific Identify or Similarity search mode.
(Contents of the drop–down list change depending on the selection made with
the radio buttons.)
Similarity
Spectrum Search Options
Reverse search
Penalize rare
compounds
Default
Off
Use Reverse Search scoring
Penalize a match by up to 50 points (out of 1000)
depending on how common the compound is.
Normal operation, use presearch screening before
spectrum-by-spectrum match factor calculation
Search the entire database using only the detailed
match algorithm
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Limits
Apply limits
Constrain the possible matches with the selected
limits. State of check box does not affect
accessibility to other controls in the group.
Set Defaults
Set all limits to Default values. (Clicking this
button restores the settings in the Limits group to
default values.)
Minimum abundance
Determines whether the minimum abundance limit
<drop–down list>
will be used.
<text box> - Smallest peak that will be used in comparison. Used to
force small peaks in the target spectrum to be ignored. The value is only
enabled when ‘Minimum abundance’ drop down list is set to ‘On’
Minimum m/z <drop–
down list>
Determines whether or how the minimum m/z
limit will be used.
<text box> - Used to determine the lowest m/z used for match factor
calculation. Without this specification, the matching algorithm starts
comparison at the HIGHER of the minimum m/z values in the target or
the library spectra. The value is enabled when ‘Minimum m/z’ drop–
down list is not set to ‘Off’
Maximum m/z
Determines whether the maximum m/z limit will
be used.
<text box> Peaks above the specified mass are ignored. Use to exclude
spurious high mass peaks in the search spectrum. The value is only
enabled when ‘Maximum m/z’ drop-down list is set to ‘On’.
Minimum match
Determines whether the minimum match value
will be used.
<text box> - Only compounds with a match value above the entered
value will be included in the ‘hits’ list. The value is only enabled when
‘Minimum match’ drop-down list is set to ‘On’.
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Molecular weight constraints
Between
and
Lower limit for library compound molecular weight.
Upper limit for library compound molecular weight.
Reporting
Reporting
Maximum hits Text
Maximum hits Plots
The maximum number of hits for which text information
will be provided for reporting.
The maximum number of hits for which plots will be
available for reporting.
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Qualitative Method Editor: Library Settings Tab
You may have several mass spectral libraries on your computer. Some are from
NIST (mainlib, the main library, and replib, a smaller library of replicate spectra
(same compounds, different spectra) which can improve the chances of finding the
right compound. There can also be other commercial libraries (e.g. the PflegerMauer-Weber drug library) or user-created libraries.
This tab allows you to select which libraries to search, and in what order.
Restricting the number of libraries (spectra) searched increases speed in a linear
fashion. Searching libraries which have only the target compounds with few
"unlikely" matches also increases the chance of a correct match. For example,
someone doing drug analyses might search a drug library, but would not want to
search a flavors and fragrances one.
Compounds in mainlib (the primary NIST library) have flags indicating which
databases they originally came from or in which industry-standard lists of
compounds they occur. If the unknown compound is expected to be in one of these
databases or lists, the speed and accuracy of the search can be improved by
restricting results to members of those databases or lists.
About NIST Results
•
•
•
•
The names in the Qualitative Results may come from the Library
Search results, or the Quantify results (if they exist).
If a peak has both Qualitative and Quantify results, the Quantify name
is used.
NIST Library Search results are in upper case, Quantify can have
upper or lower.
NIST results should use the fonts “NIST Serif” or “NIST Sans Serif”
to permit display of Greek letters.
NOTE: To prevent library searching during Qualitative Calculations, make sure the
Included libraries field is empty.
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The Library Settings Tab
Unused/Included libraries
Unused libraries
Included libraries
>
<
>>
<<
Libraries not being searched. The order in which
items appear in the ‘Unused libraries’ list is
alphabetical order.
Libraries being searched. The order in which items
appear in the ‘Included libraries’ list is the order in
which they were moved over (i.e. new items are
appended to the list).
Search selected libraries
Do not search selected libraries
Search all libraries
Remove all libraries from search list
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Compound must appear in database
A list of other databases that the compound must be in. The list is processed as a
logical OR, that is if 5 of the databases are checked, the compound is found if it is
either of the five databases. All of these are only enabled when ‘Compound must
appear in database’ is checked. These states are remembered from the last setting.
EINECS
EPA
Fine
HODOC
IR
NIH
RTECS
TSCA
USP
European Index of Commercial Chemical Substances
US EPA Environmental Monitoring Methods Index
Commercially Available Fine Chemical Index
CRC Handbook of Data of Organic Compounds
NIST/EPA Gas Phase IR Database.
NIH–NCI Inventory File
Registry of Toxic Effects of Chemical Substances
Toxic Substances Control Act Inventory
U. S. Pharmacopoeia/U.S.A.N.
A Step-by-Step Qualitative Method Summary
•
Create a Sample List
•
Create a Qualitative Method
•
Put the Qualitative Method in the Sample List
•
Start the Analysis
1. Create a Sample List
The first thing that you must do is to create a list of samples that you want to use to
perform the analysis. These samples can be acquired manually, but more often they
will be acquired automatically using an autosampler. The Sample List Editor has
various columns such as Filename, vial or bottle Number and Sample Type that can
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be filled in for each sample. Each sample is displayed as one row in the Sample List.
The Sample List Editor is part of the TurboMass top-level menu.
You need to tell TurboMass everything that it needs to know about the samples in
the list in order for it to perform a complete analysis. You must describe to the
system what each of the vials in the autosampler contains, i.e., whether it contains a
standard, an analyte, a blank or a QC sample, how to acquire it, its concentration(s),
if it is a standard or has internal standards. In addition, you must specify the name of
the file in which to store the data. You may also want to add some management
information such as Sample ID, the submitter's name, or a sample description, and
the Report Method template used.
For more information on how to create a Sample List, see Creating and Editing
Sample Lists on page 223.
2. Create a Qualitative Method
A Qualitative Method is required for most Communiqué reporting (an exception is
when you just report the chromatogram plot or acquisition conditions).
NOTE: The Quantify Method is required for Calibration and Quantification curves.
The Qualitative method describes how a data file is processed to produce calibration
curves and qualitative information. Details must be entered into the method for each
of the compounds being used in the analysis. The Qualitative Method specifies
information for performing the following tasks:
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1. Qualitative Peak integration and Reporting parameters.
2. Library Search parameters (Spectrum treatment, search type, search options
and limits; molecular weight constraints; and reporting parameters).
3. Library Selections.
To create a Qualitative Method, follow this procedure:
1. Select Qualitative Method Editor from the Tools menu
The Qualitative Method Editor appears:
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Qualitative Method
The General parameters are needed for all qualitative reports that require a
peak data set. Since Search Parameters and Library Settings are only
required when a library search is to be performed, these have been placed on
secondary tabs.
2. Specify the chromatographic data sets which are to be subject to peak detection
and integration.
The options are: The full chromatogram From start To end.
OR
One to four segments (Windows 1-4) with specified start and end times.
NOTE: Enter the peak integration parameters in the same manner as you have done in
Chromatogram or Quantify.
3. Enter a From value. A blank cell indicates the chromatogram segment will start
from the beginning of the data. The From value must be less than the To value
(unless either is blank).
4. Enter a To value. A blank cell indicates the chromatogram segment will end at
the end of the data. The To value must be greater than the From value (unless
either is blank).
5. Enter a Relative height threshold (Rel Ht) of the peak in the chromatogram.
(default is 0).
6. Enter an Absolute height threshold (Abs Ht) of the peak in the chromatogram
(default is 0).
7. Enter a Relative area threshold (Rel Area) of the peak in the chromatogram
(default is 0.0).
8. Enter an Absolute area threshold (Abs Area) of the peak in the chromatogram
(default is 0.0).
9. Enter a mass (m/z)or mass function (Func) for the segment (enter TIC, a
selected ion, or a valid mass chromatogram equation).
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10. Enter the Peak-to-peak Noise amplitude value for integration.
11. Select the X-Axis units Time (min) or Scan.
Time - Selects Time units for setting the ‘From’ and ‘To’ values in the grid.
Scan - Selects Scan numbers for setting the ‘From’ and ‘To’ values in the grid.
12. Enter the number of largest peaks you want to report.
13. Set a ‘coelution window’ parameter to ensure reliable identification of target
compounds within the qualitative chromatograms.
Peaks identified in the quantitative results can be missed in the qualitative report
if their retentions do not exactly match those found by the qualitative report
method. This can occur because two specific masses in a peak may maximize
one or two scans away from each other (of the TIC) due to noise and scan-rate
induced ‘spectral skewing”.
14. Click on the Search Parameters tab.
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15. Select the Spectrum Treatment to be applied to the spectrum before initiating
the search. For example, Background Subtracted.
16. Select the thoroughness of the search (the Spectrum search type) and its
options. Keep in mind that more thorough searches take longer.
17. You can select the Reverse search option to improve the matching capability
when there are contaminant peaks in the mass spectrum.
18. You can leave the rest of the settings as their default values or optimize as needed.
19. Click the Library Settings tab.
You may have several mass spectral libraries on your computer. Some are from
NIST (mainlib, the main library, and replib, a smaller library of replicate
spectra (subset of compounds, different spectra) which can improve the
chances of finding the right compound (Refer to the NIST2002 Software
Manual on the NIST2002 CD). There can also be other commercial libraries
(e.g., the Pfleger-Mauer-Weber drug library) or user-created libraries.
This tab allows you to select which libraries to search, and in what order.
Restricting the number of libraries (spectra) searched increases speed in a
linear fashion. Searching libraries which have only the target compounds with
few "unlikely" matches also increases the chance of a correct match. For
example, someone doing drug analyses might search a drug library, but would
not want to search a flavors and fragrances one.
Compounds in mainlib (the primary NIST library) have flags indicating which
databases they originally came from or in which industry-standard lists of
compounds they occur. If the unknown compound is expected to be in one of
these databases or lists, the speed and accuracy of the search can be improved
by restricting results to members of those databases or lists.
NOTE: If no libraries are selected, no library search will be performed. This is the default
method for only picking Qualitative Peaks.
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20. Click Save or Save As from the File menu, then name and save the method.
This method name will now be available in the Sample List under the
Qualitative Method column.
3. Put the Qualitative Method in the Sample List
After creating and saving a Qualitative Method, enter it in your Sample List.
1. Display your Sample List.
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2. Move the slider on the bottom of the Sample List window to the right until you
can view the Qualitative Method column.
3. Double-click in the cell and select your Qualitative Method.
4. Start the Analysis
Before starting an analysis save any changes made to the Sample List by selecting
Save or Save As from the Sample List File menu.
To begin acquiring data or perform post-run reporting:
1. Choose Start from the TurboMass top-level Run menu
ORto open the Start Sample List Run dialog box.
Choose
The Start Sample List Run dialog appears:
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2. Enter values or check boxes in this dialog. (The order in this dialog indicated the
order of execution. For Example, you Acquire Sample Data, then Auto
Process Samples, Auto Quantify Samples, perform Qualitative
Calculations, and Generate Communiqué Reports.)
Project - The name of the current project appears in this text box. To acquire
data to a different project, choose OK or Cancel exit this dialog box, open
another project, and restart data acquisition.
Acquire Sample Data - Selecting this option will acquire data for the specified
samples in the list.
Auto Process Samples - Selecting this option will process the acquired data as
specified in the Process column of the Sample List.
Auto Quantify Samples - Selecting this option will automatically enable
sample quantification..
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Qualitative Calculations - Selecting this option will enable Qualitative Method
processing
Generate Communiqué Reports - Selecting this option will enable
Communiqué Report generation.
Preview Reports - Check this box to specify that the Communiqué reports
generated during processing will be displayed in a preview window prior to
printing (or saving to a file or database).
NOTE: The five options above allow you to acquire and immediately process and quantify
data as desired. Or, you may choose to process or quantify data at a later time.
Run: From Sample n To Sample m - Sets the range of samples in the sample
list which will be acquired/and or analyzed. If you highlight a range of rows
before starting the analysis, the first and last rows of the highlighted region will
be displayed here.
Quantify, Qualify and Generate Reports: After Each Run - Indicates
specified processing will occur after each row in the Sample List.
At End of Sample List - Indicates specified processing will occur only after
the sample list is complete.
Process: Pre-Run - Specify the name of the process that will be run before the
acquisition of the files in the Sample List.
Post-Run - Specify the name of the process that will be run after the
acquisition of the files in the Sample List. For example, to switch the
instrument out of the operate mode and turn off various gases.
NOTE: If you want to run a process after each sample in the Sample List has been acquired,
format the Sample List to display Process and enter the name of the process to be
run for each of the samples. If you want the process to automatically operate on the
data file that has just been acquired, select Options from the Sample List Tools
menu, then deselect the Use Acquired File as Default parameter on the System tab.
3. When all are entered, click OK.
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12
Data Acquisition
Starting an Acquisition
There are two ways of starting an acquisition, a single sample acquisition from the
Tune page or a multiple sample one from the TurboMass top level screen.
Single Sample
Starting a single sample acquisition
1. Click Acquire on the Tune page.
2. Set the required parameters.
3. Click Start to begin data acquisition.
Note that this method of starting an acquisition does not have a solvent delay
time or specify a GC method. It is best for recording background and calibration
gas spectra.
Multiple Samples
The TurboMass top level window contains a Sample List Editor for defining
multiple (one or more) samples that may be used together to perform a quantitative
analysis. The list of samples is set up using the spreadsheet style editor, which can
be tailored to suit different requirements.
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Starting a multi-sample acquisition
1. Set up a Sample List as described on page 217.
2. Select Start from the Sample List Run menu
OR
Click
to display the Start Sample List Run dialog.
3. Select the Acquire Sample Data checkbox.
Select Auto Process Samples to automatically process data with macros once
it has been acquired. Select Auto Quantify Samples to automatically perform
quantification at the end of the sample list.
4. Enter values in the Run From Sample and To Sample fields.
The default is all samples in the list.
5. Click OK.
6. Repeat steps 1 to 5 as required. Sample Lists will be added to a queue and will
run sequentially.
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7. A green dot will display next to the sample in the Sample List that is currently
being acquired.
NOTE: Filenames in a Sample List must not be duplicated, and Sample List names in a
queue must not be repeated.
Process
The Process parameters allow you run processes before and after
the Sample List.
Pre-Run
Specify the name of a process that will be run before acquisition
of the files in the sample list.
Post-Run
Specify the name of a process that will be run after acquisition of
the files in the sample list, for example, to switch the instrument
out of the operate mode and to turn off various gases.
If you want to run a process after each sample in the sample list has been acquired,
format the Sample List to display Process and enter the name of the process to be
run for each of the samples. If you want the process to automatically operate on the
data file that has just been acquired, select Options from the Sample List Tools
menu, then deselect the Use Acquired File as Default parameter on the System tab.
Automated Analysis of Sample List
1. Select Process Samples from the Quantify menu to display the Quantify
Samples dialog.
2. Select the checkboxes required and click OK.
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The Quantify Samples dialog allows you to automatically process data files once
they have been acquired. To integrate samples, calibrate standards, quantify
samples, and print quantification reports, select the appropriate checkboxes. For
more information on automated sample list analysis refer to Quantify on page 259.
Integrate Samples
Integrates all the sample data files named in the Sample
List.
Calibrate Standards
Uses integration results to form Quantify calibration
curves.
Quantify Samples
Uses integration results and Quantify calibration curves
to calculate compound concentrations.
Print Quantify Reports
Prints the results of integration and quantification.
Project
Displays the project into which data will be acquired.
If you want to change the project into which data will
be acquired, you can cancel the acquisition and create a
new project by selecting Project Wizard, or open an
existing one by selecting Open Project from the
Sample List File menu. Note that this means that data
may only be processed from one Project at a time.
Make sure that all data files you might want to process
at the same time are acquired to the same Project.
Quantify From Sample n
To Sample n
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Sets the range of samples in the Sample List that will
be analyzed.
Data Acquisition
Monitoring an Acquisition
Acquisition status is shown on the TurboMass top level display.
GC Status
If GC control is configured, the GC run time is shown on the GC panel along with
the oven temperature, General Status, and GC Status.
General Status refers to the PC communications with the GC while GC Status refers
to the state of the GC, usually with respect to the current run. Both are described in
GC Control on page 150.
The scan status, sample number, and scan number are shown in the Status bar at the
bottom of the window.
MS Status
If a GC is not configured, the MS run time is shown on the MS panel, and the scan
status, sample number, and scan number are shown on the Status bar at the bottom
of the window.
The MS status displays several states:
State
Operate
Pressures
Color
Meaning
Green
High voltages are on, data acquisition is
possible
Red
High voltages are off, data acquisition is
not possible
Green
High vacuum pump is up to speed
Red
High vacuum pump is not up to speed
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Filament
Green
Operate is on, filament is on
Red
Operate is off, filament is off - possible
open filament
Chromatogram Real-time Update
To view the chromatogram that is currently being acquired in real time:
In the Chromatogram window, click
OR
Select Real-Time Update from the Display menu.
The chromatogram display will be updated as the acquisition proceeds.
Spectrum Real-time Update
To view the spectrum that is currently being acquired in real time:
1. Open the data file from the Chromatogram window
OR
Use the TurboMass Data Browser.
2. In the Spectrum window, click
OR
Select Real-Time Update from the Display menu.
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To turn on Real-Time Update, select Enable Real-Time update; to turn it off,
deselect Enable Real-Time update. When Real-Time Update is turned on, the
display will continually be updated with spectra from the current acquisition.
The actual information displayed is determined by selecting one of the options.
Real-Time Update can also be turned on and off by clicking the Real-Time
spectrum toolbar button.
Latest scan
Displays the last acquired scan. This is the default
option.
Average all
scans
Updates the display with spectra formed by averaging
all the spectra that have so far been acquired.
Average latest
scans
Updates the display with spectra formed by averaging
the last n scans acquired, where n is specified in the
associated field.
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Stopping an Acquisition
To stop an acquisition, do one of the following:
•
From the Tune page, click
•
From the TurboMass top level window, select Stop from the Run menu
.
OR
Click
.
Data acquired up to this point will be saved.
TurboMass will ask whether you want to stop the GC as well. Respond
appropriately.
If you stop the GC, you will need to select Retry Injection from the top level GC
menu to restart the GC.
For more information on starting and stopping the GC, see Stopping and Restarting
the GC on page 191.
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Automatic Startup
TurboMass includes a Startup facility that can be used to startup an instrument to
perform an acquisition. Startup can be used in any ionization mode.
The Startup facility will do the following:
•
Switch the instrument into Operate mode.
•
Load the Tune page and the startup Tune parameters.
•
Turn off Operate at the end of the Sample List and shut off the CI gas.
Running Startup
Startup uses the current Tune page settings. To change these settings, open a new
file on the Tune page. Startup can be run in any of the following ways:
•
Select Startup from the TurboMass Run menu.
•
Start an acquisition from the Tune page.
•
Start a Sample List run.
•
In the Sample List Run menu, select Edit Shutdown. In the Shutdown dialog,
select Startup from the Control List menu.
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Automatic Shutdown
TurboMass includes a Shutdown facility that can be used to shut down the mass
spectrometer at the end of a Sample List. Shutdown can be used in any ionization
mode.
The Shutdown process will do the following:
•
Switch the instrument to Standby mode.
•
Open the appropriate Autoshutdown Tune file and apply the shutdown
parameters.
•
Wait for a user-specified delay time.
Running Shutdown
Shutdown can be run in either of the following ways:
•
Select Shutdown from the TurboMass Run menu.
•
In the Sample List Run menu, select Edit Shutdown. In the Shutdown dialog,
select Shutdown from the Control List menu.
Editing the Shutdown parameters
1. Select Edit Shutdown from the TurboMass Run menu to display the Edit
Shutdown dialog.
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2. Select the appropriate checkboxes to enable startup before and/or shutdown after
a batch run, or on error. Enter the time in minutes when shutdown should start
after a Sample List batch run.
NOTE: Selecting a shutdown time that is too short could cause premature shutdown.
3. Set up an Auto Control Task timetable.
NOTE: The original parameters are carefully selected. Be cautious about changing them.
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Task
A drop-down list of all the tasks that can be controlled from
this page. The list of Tasks will vary depending on the
system configuration.
Pre Delay
Time in seconds to wait before this task is run.
Post Delay
Time in seconds to wait after this task is run.
Ion Mode
A drop-down list of Ionization modes. Enabled when Ion
Mode is selected from the Task list.
File Name
Enabled when Tune File is selected from the Task list.
Click
to display the Open file browser and select the
required Tune file.
Control
Tasks
•
To add a Task, select a Task from the drop-down list,
enter a Pre Delay or Post Delay time and click
•
To delete a single Task, left-click on the Task in the
timetable and click
.
•
To delete all entries, click
•
To modify a Task, select the required entry in the
timetable. The values will then be displayed in the edit
fields and can be altered as appropriate. Once changed,
click
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.
.
to modify the values in the timetable.
Data Acquisition
Running the Auto Control tasks
Select Run List from the Control List menu
OR
Click
.
Stopping the Auto Control tasks
Select Stop List from the Control List menu
OR
Click
.
Saving and Restoring Auto Control Task Lists
To save the settings, select Save or Save As from the File menu
OR
Click
and enter a file name in the dialog displayed.
To restore settings, select Open from the File menu
OR
Click
and select the required file.
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13
Chromatogram
Getting Started
Chromatograms are displayed in the TurboMass Chromatogram window.
Displaying the Total Ion Current (TIC) chromatogram
Select Chromatogram from the TurboMass View menu.
OR
Click
.
Displaying a summed mass chromatogram around a peak in a
spectrum
Select a peak in a spectrum to display the summed mass chromatogram centered
around the selected peak and 1Da wide.
OR
Click
to display the Mass Chromatogram dialog. Enter the mass required
in the Description field, and click OK.
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The Chromatogram Display
The chromatogram application runs in a window that has a menu bar at the top.
Under each of the headings on the menu bar is a pull-down menu, and every feature
of the chromatogram application can be accessed from this menu structure.
At the top of the chromatogram window is the toolbar. The toolbar provides a quick
way of performing common operations.
The top level window may contain one or more chromatogram windows, and each
can contain one or more chromatogram traces.
The current chromatogram window is identified by having a colored title bar. To
select another window to be the current one, either left-click on any part of the new
window, or select one from the bottom section of the Window menu.
When there is more than one trace in a window, the current one is identified by a
colored square to the left of the trace. To select another trace to be the current one,
left-click on any part of the trace, select a trace from the Traces option on the
Chromatogram Display menu, or use the up and down arrow keys on the keyboard.
The chromatograms in each chromatogram window share a common time axis. To
display chromatograms on different time axes, you must put them in separate
windows.
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The Chromatogram Toolbar
The toolbar is displayed at the top of the chromatogram window and allows you to
perform some common operations by clicking the appropriate toolbar button. The
default Chromatogram toolbar contains the buttons listed below. It is also possible to
customize the toolbar and add additional buttons for other Chromatogram
operations.
Opens a data file.
Prints the current window in portrait format.
Prints the current window in landscape format.
Sends a picture of current window to the Clipboard.
Copies a list of points in the chromatogram to the Clipboard.
Copies a list of detected peaks to the Clipboard.
Pastes the contents of the Clipboard onto the display.
Selects a mass chromatogram.
Performs peak integration.
Combines spectra scans across a chromatogram peak.
Compares BFB and DFTPP spectra to US EPA method criteria.
Performs automatic library searches.
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Select to process all traces in the current window.
Writes text onto a chromatogram.
Toggle to display each subsequent chromatogram or chromatogram process in
a new window, or to add to the current one.
Click to cause each subsequent chromatogram or chromatogram process to
replace the currently selected trace. Note that
chosen.
is unavailable when
is
Toggles real-time chromatogram update on and off.
Switches between overlay and non-overlay mode.
Increases the magnification of the current range.
Decreases the magnification of the current range.
Deletes the current magnification range.
Resets the display to a TIC trace.
Decrements the currently displayed scan in the spectrum window.
Increments the currently displayed scan in the spectrum window.
Toggle between the previous display range and the default display range.
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Customizing the Chromatogram Toolbar
The Chromatogram toolbar can be customized to:
•
Add other buttons for the operations that you use most frequently.
•
Remove buttons you do not require.
•
Determine the order in which the toolbar buttons are displayed.
Customizing the Chromatogram toolbar
Select Customize Toolbar from the Chromatogram Display menu, and add or
remove buttons as appropriate.
The additional buttons that can be added to the default Chromatogram toolbar
are:
Edit integrated peaks.
Display analog chromatograms.
Smooth.
Subtract.
Tile windows.
Cascade windows.
Stack windows.
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Adding buttons to the toolbar
1. In the Available Buttons list, select the button you want to add
2. In the Toolbar Buttons list, select the toolbar button before which you want to
insert the new button.
3. Click Add to add the new button.
Steps 1 to 3 can be repeated as often as required.
4. Separators can be inserted between toolbar buttons to divide them into logical
groups. To add a separator, repeat steps 1 to 3 selecting Separator in the
Available Buttons list.
5. Click Close to exit and save changes.
Removing buttons from the toolbar
1. In the Toolbar Buttons list, select the button you want to remove.
2. Click Remove to remove the button.
Steps 1 and 2 can be repeated as often as required.
3. Click Close to exit and save changes.
Changing the order in which toolbar buttons are displayed
1. In the Toolbar Buttons list, select the button you want to move.
2. Click Move Up or Move Down to move the toolbar button.
Steps 1 and 2 can be repeated as often as required.
3. Click Close to exit and save changes.
Resetting the toolbar to default settings
1. Click Reset.
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2. Click Close to exit and save changes.
Displaying/hiding the toolbar in the Chromatogram display
Select Toolbar from the Chromatogram Display menu to display/hide the
toolbar in the display. This command is a toggle. A check mark will appear next
to this menu item when it has been selected.
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Displaying Chromatograms
You can display various types of chromatograms in the Chromatogram Window:
mass chromatograms, TIC, and BPI chromatograms. You can also display
chromatograms in several ways.
Adding or Replacing Chromatogram Traces
TurboMass gives you a number of options for displaying any new chromatogram
traces. New chromatogram traces can be generated by:
•
Opening a new file.
•
Processing chromatogram traces (subtract, smooth, integrate, etc.).
•
Selecting mass chromatograms with the mouse or by using the Display Mass
menu command.
To display each new chromatogram trace in a new window, click
. To cancel
again. When new
this mode and display new traces in the same window, click
traces are displayed in the same window, you can choose whether to add the new
trace to the traces currently displayed or to replace the current trace with the new
trace. Click
to replace the currently selected trace with each subsequent
chromatogram or chromatogram process. Click
a second time to add each
subsequent chromatogram or chromatogram process to the traces on display. Up to
16 chromatogram traces can be displayed in one window.
NOTE:
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is unavailable when
is chosen.
Chromatogram
Mass Chromatograms
The following procedure describes how to display a summed mass chromatogram.
1. Click
OR
Select Mass from the Chromatogram Display menu to open the Mass
Chromatogram dialog.
2. If required, select a function from the Function drop-down list.
3. Enter the description of the mass chromatogram you want to generate using one
of the following formats:
110
The summed chromatogram of masses 109.5 to 110.5
110+340
The summed chromatogram of masses 109.5 to 110.5
and 339.5 to 340.5
110-340
The summed chromatogram of masses 339.5 to 340.5
subtracted from the summed chromatogram of
masses 109.5 to 110.5
110_340
The summed chromatogram of all masses from 110
to 340 inclusive
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You can generate more than one mass chromatogram trace at a time by
separating individual descriptions with commas. For example:
110, 150
The two mass chromatograms centered around 110
and 150
110_150, 340
The summed mass chromatogram of all masses from
110 to 150, and the mass chromatogram centered
around 340
4. If you want to add the mass chromatogram to the current chromatogram
window, select Add trace. If you want the mass chromatogram to replace the
currently displayed chromatogram trace, select Replace trace. If you want the
mass chromatogram to have its own chromatogram window, select New
window.
5. Click OK.
6. Mass Chromatograms can also be generated from a spectrum display. A single
right-click on a peak in the spectrum generates a chromatogram centered around
the nearest peak. The vertical height at which the mouse is clicked is also taken
into account. The peak chosen will be the nearest peak of equal or greater
intensity. A right-click-and-drag operation generates a chromatogram for the
selected range.
Displaying the same mass chromatograms for a new data file
1. Select Open from the Chromatogram File menu to load the Chromatogram Data
Browser.
2. Select the new data file you want to display.
3. Select Replace All to replace the existing data file and also any mass
chromatograms that are on display.
4. Click OK.
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TIC and BPI Chromatograms
The Total Ion Current (TIC) chromatogram is the default chromatogram displayed
when you start the chromatogram module or when you select a new data file using
the File Open command. The intensity plotted at each point in the TIC is the sum of
all the intensities in that scan. You can also obtain the TIC by selecting TIC from the
chromatogram toolbar.
A BPI (Base Peak Intensity) Chromatogram plots the greatest intensity at each scan,
whereas the TIC is the sum of the noise and the sum of signal at each scan. The BPI
chromatogram exhibits a greater apparent resolution and signal-to-noise, but will
only contain contributions from the most intense components. Therefore, it is
possible that some peaks in the TIC chromatogram may not be visible in the BPI
chromatogram. Alternatively, the BPI chromatogram may separate some
components that coelute in the TIC.
Displaying a TIC chromatogram using the toolbar
Click
to update the Chromatogram display to show a single TIC
chromatogram for the currently selected trace.
Displaying a TIC or BPI chromatogram using the menu
1. Select TIC from the Chromatogram Display menu.
2. If you require a BPI chromatogram, select BPI Chromatogram.
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3. If you want to add the new chromatogram to the current chromatogram window,
select Add trace. If you want the new chromatogram to replace the current
trace, select Replace trace. If you want the chromatogram to have its own
window, select New window.
4. Click OK to save changes.
GC Detector Trace
This dialog enables you to display the GC chromatograms previously acquired from
GC detectors (such as an FID) run in parallel to the MS within the Chromatogram
window. You may also specify the GC detector chromatogram as the Quantify
Trace for a compound within the TurboMass Quantify Method.
1. Select GC Detector Trace from the Chromatogram Display menu to open the
GC Detector Chromatogram dialog.
Next to File is the name of the currently selected TurboMass raw data file.
Select from the drop–down list the GC detector data channel (A or B) to display.
Enter an Offset (positive or negative) to be applied to the GC detector
chromatogram display to help align it with the mass spectrometer chromatogram.
For example, a positive offset of 0.15 minutes would cause the plot to start at 0.15
minutes on the time axis. If the X-axis display is changed to ‘scans’ the previous
offset (in minutes) will continue to be used for the GC detector trace.
Select one of the following:
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•
Add trace: A radio button that indicates the new chromatogram will be
added to the current window, in stacked or overlay mode.
•
Replace trace: A radio button that indicates the new chromatogram will
replace the active chromatogram in the current window.
•
New window: A radio button that indicates the new chromatogram will be
displayed in a new window.
If necessary, select a new TurboMass raw file by clicking the File button. If a new
file is selected the ‘File:’ name displayed will be updated and the ‘Channel’ control
will also be updated appropriately.
Aligning GC Detector Traces
Data from the GC detector may be slightly out of phase with data from the mass
spectrometer as there may be a time lag between analyte arrival.
You can specify an offset to the time axis of each GC trace to allow you to manually
align it with another. A different time offset can be applied to each of the GC
detectors acquired. Only the display is affected; the data on disk remain unchanged.
NOTE: This only works if the horizontal axis is displayed as time and not scans.
Aligning two chromatograms
1. Select a chromatogram.
2. Select Align from the Display/Range dialog.
3. Enter the Offset time that is required to line up the two chromatograms, and
click OK.
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Manipulating the Display
You can alter the displayed ranges of the horizontal and vertical (intensity) axes and
set the magnification ranges.
Altering the Horizontal Axis
Do one of the following to alter the range of the horizontal axis.
Altering the range of the horizontal axis (zoom)
•
Use the mouse: Left-click at one end of the region of interest, and drag the
mouse horizontally to the other end. A line appears across the range you have
selected. Do not go beyond the bounds of the axis. When you release the mouse,
TurboMass redisplays the selected region to fill the current window.
Repeat this operation as often as required.
•
Use the menu:
1. Select Range From from the Chromatogram Display menu.
2. Enter new From and To values for the horizontal axis.
3. Click OK.
Centering the display around a point on the horizontal axis
1. Select either Range, Center, On Scan or Range, Center, On time from the
Chromatogram Display menu.
Only one of these items will be on the menu, depending on the units displayed
on the horizontal axis.
2. Specify the scan number or retention time you want to center on.
3. Specify the half-width of the display range in the Window text field.
4. Click OK.
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Centering the display around a peak list entry
1. Select Range, Center, Peak List Entry from the Chromatogram Display menu.
2. Specify the peak list entry you want to center on.
3. Specify the half-width of the display range in the Window text field.
4. Click OK.
Altering the Range of the Intensity Axis
You can alter the range of the intensity axis with the mouse.
Left-click at one end of the region of interest, and drag the mouse vertically to
the other end. A line appears across the range you have selected. Do not go
beyond the bounds of the axis. When you release the mouse, TurboMass
redisplays the selected range to fill the current window.
This operation can be repeated as often as required.
Altering the Range of Both Axes
You can alter the range of both axes with the mouse.
Left-click at one corner of the region of interest, and drag the mouse to the
diagonally opposite corner. A box appears around the region you have selected.
Do not go beyond the bounds of the axis. When you release the mouse,
TurboMass redisplays the selected region to fill the current window.
This operation can be repeated as often as required.
Setting Magnified Ranges
Use the following procedures to set the magnification ranges.
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Creating single or multiple magnification ranges
To create single or multiple magnification ranges do any of the following:
•
If you have a three-button mouse, middle-click at one end of the region of
interest and drag the mouse horizontally to the other end. A line appears across
the range you have selected. When the mouse is released, TurboMass redisplays
the selected range with an initial magnification factor of 2.
•
Hold down the SHIFT key, and left-click and drag the mouse across the region
of interest.
•
To expand the chromatographic range of interest, left-click and drag the mouse,
and click
Click
•
as many times as required to achieve the desired magnification.
to restore the original chromatographic range.
Set parameters from the Chromatogram Magnify menu.
Creating single or multiple magnification ranges using the Magnify
menu
1. Select Magnify from the Chromatogram Display Range menu to open the
Chromatogram Magnify dialog.
OR
Double-click the magnify range indicators for an existing magnified range.
2. Enter the range to magnify in From and To. Enter the magnification factor you
want to apply in By.
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3. To define more than one magnification range, select a new range in Range and
repeat step 2.
You can define up to five different magnified regions of the chromatogram.
4. Click OK to redisplay the chromatogram with the data in the selected region
magnified by the requested factor.
The magnified regions are-displayed in a different color and labeled with the
magnification factor.
Magnifying the range of the intensity axis using the Toolbar
Click
to increase the magnification of the current range.
The current magnification factor is multiplied by 1.5 and rounded up to the
nearest even number to give the increased magnification factor. If the initial
magnification factor is 2, this will give subsequent magnification factors of 4, 6,
10, 16 etc.
to decrease the magnification of the current range.
Click
The current magnification factor is divided by 1.5 and rounded down to the
nearest even number to give the decreased magnification factor. If the initial
magnification factor is 16, this will give subsequent magnification factors of 10,
6, 4 etc.
Changing the magnification of a particular range
Double-click the magnification description of the magnification range to display
the Chromatogram Magnify dialog. Enter the new magnification factor and click
OK to exit.
Deleting magnification ranges
1. To delete a single modification range, select the magnification description that
appears above the range, and click
. The description will change color to red
to indicate the currently selected range.
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2. To delete all magnification ranges, select Magnify from the Chromatogram
Display Range menu. Click Default to delete all magnification ranges.
3. Click OK to exit.
Restoring the display
Click
to toggle the display between the previous display range and the
default range.
OR
Selecting Default from the Chromatogram Display Range menu toggles the
display between the previous display range and the default range.
These operations do not remove magnification ranges.
Setting the Display Range Defaults
The display range default settings specify both the effects of choosing and adding a
new chromatogram to the display.
Changing the default display
1. Select Range, Default from the Chromatogram Display menu.
2. Make any changes.
Default graph If there is more than one chromatogram in the same window, this
option specifies whether the default time/scan range for that window is made
large enough to include the time/scan ranges of All the chromatograms, or large
enough for the Current chromatogram only.
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Chromatogram
Automatic range default If this option is selected, the display range will return
to the specified default (see Default graph) when a new chromatogram is added
to a chromatogram window. If this option is not selected, the display range will
remain unchanged when a new chromatogram is added.
3. Click OK.
Controlling the Appearance of the Display
Each chromatogram window has its own set of display parameters that determines
the appearance of the chromatogram display. You can inspect and alter the
parameters for the current chromatogram window from the Chromatogram Display
View dialog.
Changing the display parameters
1. Select View from the Chromatogram Display menu to open the Chromatogram
Display View dialog.
2. Make any changes.
Normalize Data To
These parameters specify the scale on the intensity axis.
Largest
If selected, the vertical axis is scaled such that the largest
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Peak
peak on the display is at 100 %.
Intensity
If you select Intensity and specify a normalizing intensity
in the text field, the vertical axis is scaled such that your
specified intensity is at 100 %.
Baseline at
Zero
If selected, the vertical axis is scaled from 0 %.
Baseline
If you select the Baseline parameters and specify an
intensity offset in the adjacent text field, the vertical axis is
scaled from your specified intensity. This option can be
useful for displaying chromatograms that have a raised
baseline.
Lowest
Point
If selected, the display is automatically scaled such that the
lowest point on the trace is at the bottom of the display.
Link Vertical
Axes
When comparing two chromatograms by overlaying them,
it may be useful to plot both chromatograms on the same
intensity scale. The Link Vertical Axes parameter allows
you to do this. If selected, all axes in the current window
will be given a common vertical scale.
Axis Label
The Horizontal Axis parameter allows you to specify the
units of the horizontal axis to be either time or scans.
Style
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Overlay
Graphs
If selected, multiple traces in the same window will be
superimposed on the same axis. If not selected, the traces
will be drawn on separate axes, arranged vertically. When
chromatograms are overlaid, only the currently selected
trace is annotated.
Fill Trace
If selected, the area under the chromatogram trace will be
colored.
Fill Detected
If selected, then peaks detected by integration are colored.
Chromatogram
Peaks
Graph
Header
The Graph Header parameter allows you to turn off the
header information normally displayed at the top of the
chromatogram, in order to produce data for publication. If
selected, the header will be displayed; if not selected, the
header will not be displayed.
Process
Description
Each process performed on a chromatogram adds a
summary of its parameters to the chromatogram's header.
The Process Description parameter allows you to turn off
just the process information, and leave the remainder of the
header on the chromatogram.
NOTE: The Graph Header parameter overrides the Process Description parameter. That
is, if Graph Header is turned off, Process Description will be turned off as well.
Split Axis
The Split Axis value is enabled when Overlay Graphs is
selected. It allows you to change the aspect ratio of the
chromatogram by dividing the horizontal axis into
segments, then arranging the segments vertically. For
example, if a chromatogram 30 min in duration is on
display, and you set Split Axis to 3, the display will show
three axes, one from 0 to 10 min, one from 10 to 20 min,
and one from 20 to 30 min.
Overlay Step
(%)
The Overlay Step (%) parameter is turned on when
Overlay Graphs is selected. It allows you to offset each
subsequent chromatogram trace by a percentage of the
intensity axis. This can make it easier to examine overlaid
traces.
Grid
Allows you to fit a grid to the chromatogram display. The
pattern of the lines that make up the grid can be chosen as
Dot, Dash or Solid.
3. Click Header to display the Header Editor where you can edit the header
information displayed at the top of the window.
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4. Click OK.
Controlling the Appearance of Peak Labels
Each chromatogram window has its own set of Peak Annotation parameters, which
determine the appearance of peak labels. You can inspect and alter the parameters
for the current window from the Chromatogram Peak Annotation dialog.
Changing the peak annotation parameters
1. Select Peak Annotation from the Chromatogram Display menu to display the
Chromatogram Peak Annotation dialog.
2. Make any changes.
3. Click OK.
Annotation Type Parameters
These parameters control which types of peak annotation will appear on the
chromatogram. The types of peak annotation available are Peak Top Time, Peak
Top Scan, Peak Purity, Scan Base Peak Mass, Peak Response Area, and Peak
Response Height. To display a particular peak annotation select its checkbox.
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Chromatogram
For Scan Base Peak Mass, you can set the number of decimal places to a value
from 0 to 4. For Peak Response Area and Peak Purity you can set the number of
decimal places to a value from 0 to 3. The illustration above shows typical defaults
for GC/MS.
If Display Peak Name is selected, the peak name, if available, will be displayed
above the peak. The Peak Name may be obtained in several ways:
•
While viewing Quantification results, double-click on one of the report lines.
•
In Chromatogram, integrate the chromatogram. Select Integrated Peaks from
the Edit menu. Select the desired peak and enter the name. Click Modify and
then OK.
•
In Chromatogram, display a selected portion of the desired chromatogram (TIC
or selection ion). Select Lib Search Peaks from the Process menu. After the
library searching is complete, return to Chromatogram. Select Integrated Peaks
from the Edit menu and click OK. This will display the top-match library hits
for each of the integrated peaks.
Avoiding Printout of Library Search Results
To avoid printing out extensive library search results, see the following procedure:
1. From the Window Start menu, select Settings > Printers.
2. In the Printers dialog, double-click on the name of the printer.
3. In the Print Queue dialog, select Pause Printing from the Printer menu.
4. After library searching is completed, purge the files from the print queue by
double-clicking on the printer icon in the Windows task bar, then selecting
Purge Print Documents from the Printer menu. Before closing the dialog, be
sure to restart the printer by removing the checkmark from the Pause Printing
command in the Printer menu by selecting the command again.
NOTE: Pausing the printer pauses it for all users, including others who may access it
across a network. If this is a problem, add a new printer in the Printers dialog under
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a custom name and select this printer as your default. Purge the print documents
when done as described above.
Annotation Threshold Parameters
Annotation
Threshold
Allows you to specify a minimum intensity for a peak to be labeled.
% Full Scale
Allows you to set a threshold as a percentage of the base peak
intensity.
Intensity
Allows you to set an absolute intensity threshold
All Peaks
Annotates all peaks, regardless of intensity.
Level
Determines the amount of labels that appear on the chromatogram.
The Level parameter can be set to High, Medium, or Low.
Removing Chromatograms from the Display
You can remove the currently selected chromatogram trace by pressing Delete. A
message will ask you to confirm the deletion. Clicking OK will remove the trace
from the display. This operation does not affect the data stored on disk.
You can also remove traces using the Remove Chromatogram dialog. This is a
quicker method if you want to remove more than one trace.
Removing multiple chromatogram traces from the display
1. Select Remove from the Chromatogram Display menu to display the Remove
Chromatogram dialog.
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2. The traces in the current window are listed in the order in which they appear on
the display. You can select one or more traces in the list. Clicking again on a
selected item will cancel the selection. You can select all the traces by clicking
All, and then clicking OK.
Real-time Display of Chromatograms
If you are acquiring data into a file, and displaying chromatograms from that file,
then you can watch the chromatogram build up by clicking
Real-Time Update from the Chromatogram Display menu.
or by selecting
Each chromatogram window has a separate real-time update switch. You can see the
state of the switch for a particular window by determining if
is selected, or by
making that window current and selecting the Chromatogram Display menu. If realtime update is enabled, Real-Time Update has a check mark by it.
Changing the Order of Displayed Chromatograms
When a window contains multiple traces you can change the order in which they are
displayed. The chromatogram that is first in the list being displayed at the bottom of
the screen, or on top of the others, if graphs are overlaid.
Select Move To First from the Chromatogram Display menu to display the
currently selected chromatogram at the bottom of the screen.
Select Move To Last from the Chromatogram Display menu to display the currently
selected chromatogram at the top of the screen.
Adding Text to the Chromatogram Display
To add text labels to the chromatogram display, click
.
When selected, the Text tool button changes color to show that it is active. Position
the cursor where you want to add text, and left-click to open the Edit Text String
dialog.
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Enter the text in the Text field, select desired options, and click OK. You can change
the position of the user text by dragging it to a new position. Use the handles at the
sides or corners of the text box to size the box. If you want to edit the text, doubleclick it to redisplay the Edit Text String dialog.
The font and color of the user text can be changed in the Colors and Fonts option on
the TurboMass Tools menu. Any changes made to fonts or colors will only apply to
text added after the changes. If you want to change existing text, you must delete
and reinsert it. Other formatting options available for user text are as follows.
Justification
Aligns text to the left, right, or center of the text area.
Border
Draws a box around the user text.
Vertical
Displays text vertically rather than horizontally.
Autosize
Defines the text area to be just large enough to hold the user
text. If not selected, use the handles that appear to size the text
area as required.
Attach to
axis
If selected, user text can be positioned only within a box
defined by the intensity and time/scan axes. If it not selected,
user text can be positioned anywhere on the display.
The current formatting options are saved as the default options each time you exit
from the Edit Text String dialog.
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Chromatogram
Processing Chromatograms
Three processes are available for use on chromatograms: polynomial background
subtraction, smoothing, and integration. Background subtraction and smoothing help
you improve the presentation of the data. Integration locates peaks, positions
baselines, and calculates peak statistics for quantitative work.
Processing Multiple Chromatograms
The background subtract, smooth, and integrate processes can be performed
automatically on all the chromatograms within the current window. To enable this
or select Process All Traces from the Chromatogram Process
operation, click
menu; the menu item will have a check next to it. To turn off multiple processing,
reselect the toolbar button or menu item.
You can choose to add the processed trace to the current window or replace the
current trace with the processed trace. Toggle
to cause each subsequent
chromatogram or chromatogram process to replace the currently selected trace or to
add chromatogram process to be added to the display.
NOTE:
is unavailable when
is selected.
Subtract
Background Subtract fits a smooth curve through the noise in the chromatogram,
and then subtracts this curve from the chromatogram, leaving the peaks on a flat
baseline.
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Polynomial Order
Allows you to specify the degrees of freedom allowed to
the fitted curve. With polynomial order set to 0, a
horizontal straight line is fitted. With polynomial order
set to 1, a sloping straight line is fitted. The further the
background is from a straight line, the higher you must
set the Polynomial Order value. Too high a value will
cause the fitted curve to begin to follow the peak shapes.
Normal operating range for this parameter is 3rd to 20th
order.
Below Curve
Allows you to move the background curve up and down
in the noise. The curve fit is constrained to place the
specified percentage of data points beneath the fitted
background curve. The normal operating range for this
parameter is 5 % - 30 %, depending on the abundance and
width of peaks in the chromatogram. For more or wider
peaks, increase the value.
Tolerance
Affects the precision to which the internal arithmetic is
performed. It should not normally be changed from its
default value of 0.01.
Flatten Edges
If selected, TurboMass verifies that the polynomial
applied is flat or horizontal at the beginning and end of
the trace.
The parameters shown in the figure below produced the background subtracted
chromatogram and total ion chromatogram shown in the printed documentation.
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Chromatogram
You can check the operation of the background subtraction process with a given set
of parameters by selecting the Make graph of fitted polynomial checkbox. This
causes the same calculation to take place, but rather than displaying a chromatogram
with the background curve subtracted, the curve itself is displayed. Selecting
Overlay Graphs and Link Vertical Axes from the Chromatogram Display View
dialog creates a display similar to that shown.
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Subtracting the background from a chromatogram
1. Select Subtract from the Chromatogram Process menu.
2. Set the polynomial order parameter as described above.
3. Set the below curve parameter as described above.
4. Click OK.
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Chromatogram
The Subtract dialog indicates the progress of the subtract algorithm. After every
iteration, TurboMass updates the convergence value in the dialog. The algorithm
terminates when convergence is less than tolerance.
With higher order polynomials, background subtract will sometimes have
difficulty converging on a solution. There is a preset upper limit of
300 iterations. If background subtract does not seem to be making progress,
click Cancel in the Background Subtract dialog and try again with a lower-order
polynomial.
Smoothing Chromatograms and/or Reducing Noise
Smoothing improves presentation and aids interpretation of a chromatogram by
increasing the apparent signal-to-noise ratio.
NOTE: In some instances, if your chromatogram has very small peaks you may want to turn
smoothing off to accurately define the valley of overlapping peaks.
Two types of smoothing are available for chromatograms: Moving Mean and
Savitzky Golay. Both methods slide a window along the chromatogram, averaging
the data points in the window to produce a point in the smoothed chromatogram.
Moving Mean takes the arithmetical mean of the intensities of the data points in the
window. Savitzky Golay takes an average of the intensities weighted by a quadratic
curve. This tends to enhance peak and valley shapes, as well as preserving the height
of the peaks better than the Moving Mean. However, Savitzky Golay does tend to
produce small artifacts on either side of the real peaks.
Noise Reduction is optimized for single GC peaks in the signal-to-noise range of 3:1
to 200:1. A window containing multiple GC peaks may lead to a loss of GC peak
resolution
Smoothing a chromatogram and/or reducing noise
1. Select Smooth from the Chromatogram Process menu to open the Smooth
chromatogram dialog.
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2. Set the Window size parameter.
The number you specify is the half-width of the smoothing window in scans.
This parameter can be set automatically by right-clicking and dragging the
mouse across a chromatogram peak at half height.
3. Select a Smoothing method (Mean or Savitzky-Golay)
4. As required, adjust the number of times the smooth is repeated by changing the
Number of smooths parameter.
Increasing this parameter gives a heavier smooth.
5.
Select Noise Reduction to apply noise reduction to a chromatogram.
NOTE: If you only want to apply Noise Reduction without applying smoothing, select None
and then select Noise Reduction.
6. Click OK.
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Integrating Chromatograms
The integration process locates the peaks in a chromatogram, draws baselines, and
calculates peak heights and areas for quantification.
You can integrate a chromatogram using the current parameters by clicking
.
You can use the Integrate chromatogram dialog to change the parameters. The
integration process operates only on the currently displayed range and not on the
whole chromatogram.
Copy
Allows you to copy the current integration parameters to the
Clipboard. These parameters can then be pasted into another
application such as the Quantify Method Editor.
Paste
Allows you to paste a set of integration parameters from the
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Clipboard.
Noise
Peak-to-peak
amplitude
412
The Integrate chromatogram dialog requires that you enter the
Peak-to-peak Noise amplitude. This value is used by the
integration software to pre-filter the chromatogram. A suitable
value can be measured directly from the chromatogram by
right-clicking and dragging the mouse across a section of noise
in the chromatogram. The sensitivity of the integration
algorithm can be fine-tuned by manually adjusting this value.
Note that the optimum value is likely to differ for each mass
chromatogram.
Enable
smoothing
You can choose to smooth the chromatogram before integrating
by selecting Enable smoothing. The parameters for the smooth
can be examined and altered by clicking Smooth. For more
information, see Smoothing Chromatograms on page 409.
Threshold
Small peaks can optionally be removed by setting one of the
four available threshold parameters. Click Threshold to open
the Response Threshold dialog, where you can examine or
modify these parameters.
Chromatogram
Relative height
Removes peaks whose height is less than the specified
percentage of the highest peak.
Absolute height
Removes peaks whose height is less than the specified
value.
Relative area
Removes peaks whose area is less than the specified
percentage of the largest peak area.
Absolute area
Removes peaks whose area is less than the specified value.
You can examine and modify the parameters that control the positioning of
baselines and separation of partially resolved peaks by verticals (droplines) by
clicking Peak detect in the Integrate chromatogram dialog to display the Peak
Detect dialog.
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The Join valleys parameter affects how baselines for partially resolved peaks are
drawn. The larger the value of this parameter, the more peak baselines will be drawn
up to the valleys between unresolved peaks. The default value for this parameter is
30 %, and the normal operating range is 5 % - 75 %.
Reduce peak tailing and Raise baseline position the baseline end points. In the
example, the pronounced tail on the peak at 5.42 min is reduced by decreasing the
value of the reduce peak tailing parameter from 150 % to 50 %. The default value
for this parameter is 50 %, and the normal operating range is between 25 %
and 300 %.
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Chromatogram
Raise baseline is optionally selected in the Peak Detect dialog, and prevents the
baseline end point from being moved too high up the peak. To prevent the baseline
endpoints from moving up the peaks, reduce the value of this parameter. The default
value is 5 %, and the normal operating range is 5 % - 20 %. This parameter is only
relevant when the reduce peak tailing parameter has a small value (less than 50 %).
In the example below, the reduce peak tailing parameter has been set to 25 %.
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Draw vertical is selected in the Peak Detect dialog, and determines how well
resolved peaks must be before they are separated by a dropline (or baselines are
drawn up into the valleys, depending on the value of the join valleys parameter). If
you want to separate poorly resolved peaks, increase the value of this parameter.
The default value is 90 %, and the normal operating range is 50 % - 100 %.
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Chromatogram
Detect Shoulder peaks is selected in the Peak Detect dialog, and is used optionally
to attempt to detect completely unresolved peaks or shoulders. The algorithm will
detect a shoulder if the slope of the shoulder top is less than the specified percentage
of the steepest slope on the peak. Therefore, to make shoulder detection more
sensitive, increase the value of this parameter. The default value is 30 %, and the
normal operating range is 20 % - 90 %.
Integrating a chromatogram
1. Display the chromatogram range you want to integrate.
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2. Select Integrate from the Chromatogram Process menu.
3. Enter a value for Noise Peak-to-peak amplitude.
To calculate this value, display a section of the chromatogram that contains only
background. Right-click at one end of a section that contains background noise,
and drag the mouse to the other end of the noise section. When the mouse is
released, the integration software will calculate the Noise amplitude and update
the value.
4. Optionally, select Enable smoothing and click Smooth to examine or modify
the smoothing parameters.
5. Optionally, set up one or more thresholds to remove small peaks by clicking
Threshold in the Integrate chromatogram dialog to open the Response
Threshold dialog.
6. Click OK to perform the integration.
The integration software will smooth the chromatogram trace if requested,
locate the peaks, draw baselines, and calculate peak statistics.
Editing Detected Peaks
You can use the Edit Integrated Peaks dialog to change the results of integration by
changing the position of an individual baseline, adding a single peak, or deleting one
or all peaks.
Displaying information about an integrated peak
Left-click on a peak to display the peak top position, peak height and peak area
in the status bar at the bottom of the chromatogram window.
Peak Annotation can be displayed using any combination of peak top time, peak
top scan, peak response height, and peak response area by selecting Peak
Annotation from the Chromatogram Display menu.
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Chromatogram
Editing a peak baseline
1. Select Integrated Peaks from the Chromatogram Edit menu to open the Edit
Integrated Peaks dialog.
2. Do one of the following to select the peak whose baseline you want to edit:
• Right-click and select the peak in the Chromatogram display.
• Select the peak from the Peak Tops list in the Edit Integrated Peaks dialog.
3. Modify a baseline range by doing one of the following:
• Edit the Start or End values.
• Right-click and select a range, and click Modify.
• Left-click on one of the end markers (boxes) and drag it to the required
position.
4. The values in Peak Information will be updated to reflect the edited baseline.
Adding a new peak
1. Select Integrated Peaks from the Chromatogram Edit menu to open the Edit
Integrated Peaks dialog.
2. Enter the Start and End points of the baseline for the new peak, or right-click
and select a range.
3. Click Add to update the values in Peak Information to reflect the new peak.
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Deleting a single peak
1. Select Integrated Peaks from the Chromatogram Edit menu to open the Edit
Integrated Peaks dialog.
2. Do one of the following to select the peak you want to delete:
• Right-click and select the peak in the Chromatogram display.
• Select the peak from the Peak Tops list in the Edit Integrated Peaks dialog.
3. Click Delete.
Deleting all the peaks
1. Select Integrated Peaks from the Chromatogram Edit menu.
2. Click Clear All in the Edit Integrated Peaks dialog.
3. When you are satisfied with your changes, click OK.
Clicking Cancel aborts the edit and discards your changes.
Peak Purity
The Peak Purity process works on TIC chromatograms that have already been
integrated. Note that it is important not to have Enable Smoothing selected in the
Integrate chromatogram dialog; this is because smoothing tends to increase the peak
width, and hence when the Purity process selects scans from the edges of the
smoothed peak, the scans that are chosen are actually in the noise portion of the raw
data. Since it is the raw data that is used for the purity calculation, this will have the
effect of artificially depressing the purity value for each peak.
Select Peak Purity from the Chromatogram Process menu to open the Peak Purity
dialog.
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Chromatogram
There are two separate methods for calculating Peak Purity.
The first, called the Simple method, requires no parameters. It selects five spectra
from across the peak and correlates each spectrum with the other spectra. The mean
correlation value is displayed, scaled to a percentage (0 % - 100 %), with 100 %
representing total purity, and 0 % total impurity. A purity value of 60 % does not
mean that the peak has two components in the ratio 60 : 40.
The second method, called the Bayesian method, requires two parameters. This
method characterizes each mass channel as a set of (up to) its first four moments.
The first moment represents peak position, the second peak width, and the third
asymmetry. The program can be restricted to use less than four moments by
reducing the Max no. of moments parameter. Reducing this value will decrease the
run time of the process. It is also possible to reduce the number of mass peaks used
for comparison. This value is represented by the Max no. of masses parameter.
Decreasing this parameter will also result in reduced run time. The Bayesian method
is based on a rigorous probabilistic analysis. The output value loosely represents the
natural logarithm of the probability that the peak is pure. Therefore, to calculate the
probability that a peak with purity value x is pure, evaluate exp(x). This implies that
the maximum score (100 % probability pure) is 0.
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Unleaded gasoline
GAS2
100
Scan EI+
TIC
3.33e6
- 206
Bayesian Met ho d
- 90
0
- 15
0
- 177
- 758 - 155
%
0
0
0
0
- 49
- 17 - 478
0
- 5188
- 251
0
- 64
0
- 26
0
GAS2
100
Scan EI+
TIC
3.33e6
74%
Sim p le Met ho d
88%
99%
97%
99%
91%
%
41%40%
100%
85%
86% 99%
90%
41%
99%
64% 75%
74%
99%
72%
88%
75%
0
8.40
8.60
8.80
9.00
9.20
9.40
9.60
9.80
Tim e
Calculating the peak purity index for a Total Ion Chromatogram
1. Display the chromatogram range of interest in a chromatogram window.
2. Integrate the chromatogram, remembering to disable smoothing.
3. Select Purity from the Chromatogram Process menu to open the Peak Purity
dialog.
4. Select the purity method, either Simple or Bayesian.
For the Bayesian method, optionally enter the number of moments to use and
the number of mass spectral peaks to consider.
5. Click OK.
Signal to Noise
It is sometimes useful to know the ratio of the peak heights to the level of noise in a
mass chromatogram. TurboMass provides the Signal to Noise calculation to do this.
Signal to Noise can be accessed from Chromatogram by selecting Signal to Noise
from the Process menu.
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Chromatogram
The Signal to Noise (S/N) calculations can be carried out to display peak to peak or
RMS (root mean square) values. If Peak-to-Peak is required, the greatest height of
the signal range above the mean noise value is divided by the variance. If RMS is
required, the greatest height of the signal above the mean noise is divided by the
root mean square deviation from the mean of the noise. The S/N calculated using
RMS noise is usually expected to be about 5 times the S/N value calculated using
Peak-to-Peak noise.
Various authorities have different methods for determining what level of noise is
taken into account for the calculations of noise variance and RMS deviation. A twostep process is carried out. First, the mean should be calculated with or without
zeros as normal. Optional processing then allows three options:
Ignore Worst 5
% of Scans
The 5 % of scans that have the greatest deviation from the
mean are disregarded in the noise signal.
Ignore Scans
Outside 1 SD
Those scans whose deviation from the mean is greater than
one standard deviation are disregarded in the noise signal.
Ignore Scans
Outside 2 SD
Those scans whose deviation from the mean is greater than
two standard deviations are disregarded in the noise signal.
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Options 1 and 3 are expected to give roughly equivalent results. Option 2 should
give an RMS value of about double that of the other two options.
If one of these three processing options is selected, then the mean and RMS
deviation of the noise are recalculated disregarding the appropriate points.
Calculating the signal to noise value for a Mass Chromatogram
1. Display the chromatogram range of interest in a chromatogram window.
2. Select Signal to Noise from the Chromatogram Process menu.
3. Enter Signal and Noise ranges.
Either enter values or, right-click at one end of the Chromatogram region of
interest, and drag the mouse horizontally to the other end. TurboMass indicates
the range you have selected. The dialog will be updated to show this range.
4. Select the Noise Processing and Display methods required.
5. Click OK.
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Chromatogram
Combine Spectra
The Combine process (also called spectral background subtraction) can be accessed
from either Chromatogram or Spectrum by clicking
from the Process menu.
or by selecting Combine
The combine process operates on centroid-mode or continuum data. Its purpose is to
produce a single scan from all the scans across a TIC peak. The combined scan
exhibits enhanced signal-to-noise and improved mass accuracy.
Specify three scan ranges and a background factor. One range contains the scans
across the peak top and the other two ranges contain scans from the background, on
each side of the peak. The scans across the peak top are averaged together and the
average of all the background scans, multiplied by the background factor (X), is
subtracted from the result.
The Peak separation parameter is the spectral peak width in Da (amu). For
centroided data, the peak width can be determined from inspection of the tune peaks
on the Tune page. It is typically 1.0 for GC/MS data. The Combine algorithm
combines peaks within a Peak separation window into a single peak. Clicking Reset
will remove all values that have been entered into the dialog.
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Combining scans in a centroid-mode data file
1. Display the chromatogram peak of interest in a chromatogram window.
2. Click
OR
Select Combine Spectra from the Chromatogram Process menu to open the
Combine Spectrum dialog.
3. Enter the peak top scan range either by entering scan numbers separated by a
colon (for example, 619:626) into the Average field, or by right-clicking and
dragging the mouse across the peak.
4. Optionally, enter one or two background scan ranges:
Enter the scan numbers into the Subtract field. Each range should be in the
form of two numbers separated by a colon, as above; and if there are two ranges,
they should be separated by a comma (for example, 606:612,631:637).
OR
Right-click and drag the mouse across the first background scan range.
Optionally repeat for a second range.
5. Optionally, enter a background factor in the X field.
6. Optionally, enter a Peak separation value.
7. Click OK.
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Chromatogram
Peak Lists
The results of the peak integration can be saved to disk as a named Peak List. Peak
Lists can then be processed using the TurboMass Quantify program.
Creating and Editing a Peak List
Use the following procedures to create a new peak list or edit an existing one.
1. Select Peak List Write from the Chromatogram Edit menu to display the Edit
Peak List dialog.
2. Click File to display the File Open dialog, and select a file.
3. If you want to create a new Peak List file, enter a new name into the File Name
field, and click Open.
4. Click Exit.
Appending a single peak to the current Peak List
1. Select Peak List Write from the Chromatogram Edit menu to display the Edit
Peak List dialog.
2. Select the peak you want to append either from the Peak Tops list, or by rightclicking the peak in a chromatogram trace.
3. Click Append.
The contents of the Peak List list will be updated to include the new peak.
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4. To append all the peaks in the Peak Tops list, click Append All.
Deleting a single peak from the current Peak List
1. Select Peak List Write from the Chromatogram Edit menu to display the Edit
Peak List dialog.
2. Select the peak you want to remove from the Peak List list.
3. Click Delete.
4. To delete all the peaks in the peak list, click Clear All.
Reading a Peak List into a Chromatogram
Use the following procedures to select a peak list file and read a single peak or the
entire peak list into the currently selected chromatogram.
Selecting a Peak List file
1. Select Peak List Read from the Chromatogram Edit menu.
2. Click File to display the File Open dialog.
3. Select a file from the list and click Open.
4. Click OK.
Reading a single peak into the currently selected chromatogram
1. Select Peak List Read from the Chromatogram Edit menu.
2. Select a peak from the Peak List list.
3. Click OK.
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Chromatogram
Reading a whole peak list into the currently selected chromatogram
1. Select Peak List Read from the Chromatogram Edit menu.
2. Click Get All.
3. Click OK.
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Automatic Library Searching
This option automatically searches the specified library for entries that match the
currently integrated chromatogram displayed in the Chromatogram window. This
process uses your current integration and library search parameters.
Note that while automatic library searching can work well for chromatographically
well-resolved peaks, complex chromatograms will probably require manual
background subtraction and library searching.
Performing an automatic library search
1. In the Chromatogram window, set the display range and integration threshold
values to limit the integrated peaks to only those you wish to library search.
See Integrating Chromatograms on page 411 to set up your integration
parameters.
2. Set up your Library search and display parameters.
For more information, see the fully- and semi-automatic library search
procedures in Library on page 495.
to initiate the automatic library search process for the first peak in
3. Click
the integrated chromatogram.
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Chromatogram
As the search process progresses, TurboMass displays a Print dialog where you
can specify whether you want to print out the current window or all windows for
that peak.
TurboMass continues to search the specified library for consecutive peaks in the
integrated chromatogram and prints the results of each search.
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Copying to and from the Windows Clipboard
The Windows Clipboard provides temporary storage for information that is being
transferred between application programs (word processors, spreadsheets,
TurboMass etc.). You can use the Clipboard to move data into or out of the
Chromatogram window, either as a picture or as a text list. For example, you can
paste spectra or chromatograms into reports written with a Windows compatible
word processor.
TurboMass now copies a Chromatogram picture to the Clipboard as a metafile
giving greatly improved resolution. When the metafile is pasted into another
Windows application it can be rescaled if required without distorting the original
image as long as the original aspect ratio is maintained. When you use the
TurboMass Edit Copy Picture command both a metafile and a bitmap are copied to
the Windows Clipboard.
Copying a chromatogram as a picture to the Clipboard
1. Produce the required display in a chromatogram window.
2. Click
OR
Select Copy Picture from the Chromatogram Edit menu to copy the contents
of the window to the Clipboard as both a metafile and a bitmap.
3. To read the image into another application as a metafile, select Paste from the
other application's Edit menu. If you select Paste Special from the other
application's Edit menu, you will be given the option of pasting either the
metafile or the bitmap.
Copying a chromatogram as a text list to the Clipboard
1. Display the required time range in a chromatogram window.
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Chromatogram
2. Click
OR
Select Copy Chromatogram List from the Chromatogram Edit menu. The
section of the chromatogram on display will be transferred to the Clipboard as
(time, intensity) pairs or (scan, intensity) pairs depending on the horizontal axis
setting.
3. To read the information into another application, select Paste from the other
application's Edit menu.
Copying integrated chromatogram peaks as a text list to the Clipboard
1. Display the required time range in a chromatogram window
or select Copy Detected Peaks from the Chromatogram Edit menu.
2. Click
The chromatogram peaks on display will be transferred to the Clipboard. The
information transferred for each peak is the peak top, height, area, start, end,
start height, and end height.
3. To read the information into another application, select Paste from the other
application's Edit menu.
Pasting information into a chromatogram window from the Windows
Clipboard
1. Click
OR
Select Paste from the Chromatogram Edit menu to paste the default Clipboard
object to chromatogram. Select Paste Special to choose which object to paste
into Chromatogram. These objects would typically be metafiles, bitmaps, or
text.
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2. Drag the outline of the image to the required position with the mouse.
You can paste the contents of the Clipboard, whether a bitmap, a metafile, or
text, into a chromatogram window. If the data are in textual or metafile form,
you can re-scale it using the mouse and there will be no distortion of the image.
However, if you paste a bitmap, re-scaling is done by stretching the image,
which will cause some distortion. To avoid this, scale the image to the required
size before you copy it to the Clipboard.
Removing pasted input from the display
1. Select the item you want to remove.
2. Press the DELETE key.
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Spectrum
14
Spectrum
Getting Started
You can open the Spectrum window in several ways.
Displaying the first scan of the current data file
To display the first scan of the current data file, do one of the following:
•
Double-click at the required retention time in the Chromatogram window.
•
Right-click and drag the mouse across the appropriate range of interest in the
Chromatogram window to initiate a Combine Spectrum process.
•
Select Spectrum from the TurboMass View menu.
•
Click
•
Enter CTRL+S.
.
Displaying a particular scan in the current file
To display a particular scan in the current file, do one of the following:
•
Use the mouse to select the required part of a scan in a chromatogram.
•
Click
•
Select Spectrum…At from the Spectrum Display menu and enter the required
scan number.
from the Spectrum toolbar and enter the required scan number.
About the Display
The spectrum application runs in a top level window that has a menu bar at the top.
Under each of the headings on the menu bar is a drop-down menu, and you can
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access every feature of the Spectrum application from this menu structure. The
commands and icons are quite similar to those in Chromatogram.
At the top of the spectrum window is the toolbar. The toolbar provides a quick way
of performing common operations.
The top level window can contain one or more spectrum windows, and each can
contain one or more spectrum traces.
The current spectrum window is identified by a colored title bar. To select another
window to be the current one, either click in any part of the new window, or select
one from the bottom section of the Window menu.
When there is more than one trace in a window, the current one is identified by a
colored square on the left of the trace. To select another trace to be the current one,
left-click any part of the trace, select one from the Graphs option on the Spectrum
Display menu, or use the up and down arrow keys on the keyboard.
The spectra in each spectrum window share a common mass axis. To display spectra
on different mass axes, you must put them in separate windows.
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Spectrum
The Spectrum Toolbar
The toolbar displayed at the top of the spectrum window lets you perform some
common operations with a single click of the appropriate toolbar button. The default
Spectrum toolbar contains the buttons listed below. You can also customize the
Spectrum toolbar and add additional buttons for other Spectrum operations.
Opens a data file.
Prints the current window in portrait format.
Prints the current window in landscape format.
Sends a picture of current window to the Clipboard.
Copies a list of points in the spectrum to the Clipboard.
Pastes the contents of the Clipboard onto the display.
Identifies the current scan using the library search facility.
Toggles between processing all traces in the current window and the current
trace in the current window.
Writes text onto a spectrum. After clicking this button, point to where text is
required, and left-click. The Edit Text String dialog appears for text input. When OK
is clicked, the text is written to the Spectrum display.
Selecting once causes each subsequent spectrum to appear in a new spectrum
window, rather than being added to the current window. Selecting a second time
cancels this mode.
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Selecting once causes each subsequent spectrum or spectrum process to replace
the currently selected trace. Selecting a second time causes each subsequent
spectrum or spectrum process to be added to the traces on display.
NOTE:
is unavailable when
is clicked.
Toggles real time spectrum update on and off.
Increases magnification of current range.
Decreases magnification of current range.
Deletes current magnification range.
Selects a new scan from the current data file.
Decrements the currently displayed scan.
Increments the currently displayed scan.
Click once to restore the previous display range; click again to use the default
display range.
Customizing the Spectrum Toolbar
The Spectrum toolbar can be customized to add other buttons for the operations that
you use most frequently, remove buttons you do not require, and determine the order
in which the toolbar buttons are displayed. In this way you can customize the
TurboMass display to suit the way you work.
To customize the Spectrum toolbar, select Customize toolbar from the Spectrum
Display menu.
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Spectrum
The additional buttons that can be added to the default Spectrum toolbar are:
Save spectrum.
Combine spectra.
Tile windows.
Cascade windows.
Stack windows.
Adding buttons to the toolbar
1. Select the button you want to add to Available Buttons list.
2. In the Toolbar Buttons list, select the toolbar button before which you want to
insert the new button.
3. Click Add to add the new toolbar button.
Repeat Steps 1 - 3 as often as required.
4. Separators can be inserted between toolbar buttons to divide them into logical
groups. To add a separator repeat steps 1 - 3 and then select Separator in
Available Buttons.
5. Click Close to exit and save changes.
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Removing buttons from the toolbar
1. In the Toolbar Buttons list, select the button you want to remove.
2. Click Remove to remove the button.
Steps 1 and 2 can be repeated as often as required.
3. Click Close to exit and save changes.
Changing the order in which toolbar buttons are displayed
1. In the Toolbar Buttons list, select the button you want to move.
2. Click Move Up or Move Down to move the toolbar button.
Steps 1 and 2 can be repeated as often as required.
3. Click Close to exit and save changes.
Resetting the toolbar to default settings
1. Click Reset.
2. Click Close to exit and save changes.
Removing the toolbar from the Spectrum display
Select Toolbar from the Spectrum Display menu to display/hide the toolbar. This
command is a toggle.
A check mark will appear next to this menu item when it has been selected.
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Displaying Spectra
The following procedures describe how to display spectra in the same or separate
windows.
Adding or Replacing Spectra
TurboMass gives you a number of options for displaying any new spectrum traces.
New spectrum traces can be generated by:
•
Opening a new file.
•
Processing spectra (subtract, smooth, center etc.).
•
Selecting spectra by double-clicking on a chromatogram.
Once generated, you can display spectra in the same or in separate windows.
When new traces are displayed in the same window, you can choose whether to add
the new trace to the traces currently displayed or to replace the current trace with the
new trace.
Displaying spectra in a new or in the same window
Toggle
to display each new spectrum trace in a new or in the same window.
Adding or replacing spectra in a window
Toggle
to replace or add each subsequent spectrum or spectrum process in the
current window.
Up to 16 spectrum traces can be displayed in one window.
NOTE:
is unavailable when
is clicked.
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Manipulating the Display
The following procedures describe how to alter the mass and intensity axes.
Changing the range of the mass axis
To change the range of the mass axis, do one of the following:
•
Left-click at one end of the region of interest, and drag the mouse horizontally
to the other end. TurboMass will indicate the range you have selected; do not go
beyond the bounds of the axis. When the mouse is released, the selected range
will be redisplayed to fill the current window.
•
To expand the spectral range of interest, left-click and click
as required to achieve the desired magnification. Click
original range. Repeat this operation as often as required.
•
as many times
to restore the
Change the range of the mass axis from the menu:
1. Select Range From from the Spectrum Display menu.
2. Enter new From and To values for the mass axis.
3. Click OK.
Changing the range of the intensity axis
Left-click at one end of the region of interest, and drag the mouse vertically to the
other end. TurboMass will indicate the range you have selected; do not go beyond
the bounds of the axis. When the mouse is released, the selected range will be
redisplayed to fill the current window.
This operation can be repeated as often as required.
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Spectrum
Setting Magnified Ranges
You can set magnification ranges in several ways.
Creating magnification ranges using mouse and menu commands
•
If you have a three-button mouse, middle-click at one end of the region of
interest and drag the mouse horizontally to the other end. As you drag the
mouse, TurboMass will indicate the range you have selected. When the mouse is
released the selected range will be redisplayed with an initial magnification
factor of 2.
•
Hold down the SHIFT key, and left-click and drag across the region of interest.
•
To expand the spectral range of interest, left-click and drag the mouse, and click
as many times as required to achieve the desired magnification.
Click
•
to restore the original spectral range.
Create single or multiple magnification ranges using the Magnify menu
command:
1.
Select Magnify from the Spectrum Display Range menu, or doubleclick the magnify range indicators of an existing magnified range to
open the Spectrum Magnify dialog.
2.
Enter the range you want to magnify in From and To. Enter the
magnification factor you want to apply in By.
3.
To define more than one magnification range, select a new range in the
Range field and repeat step 2.
4.
You can define up to five different magnified regions of the spectrum.
5.
6.
Click OK to exit.
The spectrum is redisplayed with the data in the selected regions
magnified by the requested factor. The magnified regions are displayed
in a different color and labeled with the magnification factor.
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Magnifying the range of the intensity axis using the toolbar
Use one of the following tool buttons to magnify the intensity axis range.
Increases magnification of the current range. The current magnification factor is
multiplied by 1.5 and rounded up to the nearest even number to give the increased
magnification factor. If the initial magnification factor is 2, this will give subsequent
magnification factors of 4, 6, 10, 16, etc.
Decreases magnification of the current range. The current magnification factor
is divided by 1.5 and rounded down to the nearest even number to give the
decreased magnification factor. If the initial magnification factor is 16, this will give
subsequent magnification factors of 10, 6, 4, etc.
Deletes the current magnification range.
Where multiple magnification regions have been defined, to select the current
magnification range click in the magnification description that appears above the
range. The description will change color to red to indicate the currently selected
range.
Changing the magnification of a particular range
Double click on the magnification description of the magnification range. The
Spectrum Magnify dialog will be displayed. Enter the new magnification factor and
click OK to exit.
Deleting Magnification Ranges
•
To delete a single magnification range, select the range you want to cancel and
click
•
446
.
To delete all magnification ranges, select Magnify from the Spectrum Display
Range menu. Click Default to delete all magnification ranges. Click OK to exit.
Spectrum
Changing the Range of Both Axes
Left-click at one corner of the region of interest, and drag the mouse vertically
to the diagonally opposite corner. As you drag the mouse TurboMass will
indicate the region you have selected; do not go beyond the bounds of the axis.
When the mouse is released, the selected region will be redisplayed to fill the
current window.
This operation can be repeated as often as required.
Restoring the Display
Toggle
to restore the display to its previous state or to the default range.
OR
Toggle the Default command in the Spectrum Display Range menu to restore
the display to its previous state or to the default range.
These operations do not remove magnification ranges.
Setting the Display Range Defaults
The display range default settings specify both the effect of clicking
a new spectrum to the display.
and adding
Changing the default display
1. Select Range, Default from the Spectrum Display menu.
2. Make any changes.
3. Click OK.
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Default range
Only relevant to Centroid mode acquisitions. Specifies whether the
mass axis will range from the first peak in the scan to the last peak
in the scan (Data), or over the range you requested when the
acquisition started (Acquisition).
Default graph
If there is more than one spectrum in the same window, this option
specifies whether the default mass range for that window is made
large enough to include the mass ranges of all the spectra, or the
current spectrum only.
Automatic
range default
If enabled, the display range will return to the specified default (see
Default range and Default graph) when a new spectrum is added
to a spectrum window. If Automatic range default is disabled, the
display range will remain unchanged when a new spectrum is
added.
Displaying a Spectrum as a List
You can replace the display in the current spectrum window with a list of masses
and intensities of the peaks in the currently selected spectrum.
Select List Spectrum from the Spectrum Display menu.
A check mark is placed next to the List Spectrum menu item. You can use most
of the menu commands and the spectrum toolbar.
Restoring the graphical display
Select List Spectrum from the Spectrum Display menu.
The check mark is removed from the List Spectrum menu item.
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Spectrum
Printing a report of the spectrum listing
1. Select Print Report from the Spectrum File menu.
2. Select the data range you want to display.
Select Data to print a listing of the whole data file. Select Display to print a
listing of the current display range.
3. Select the relevant Header Information and Peak Information options you
want to print.
4. Click OK to exit and print the report.
Printing with Chromatogram
This prints the active spectrum and chromatogram on the same page to the default
printer. To Print the Active Spectrum and Chromatogram on the same page:
1. Open the raw file and selected function in the Chromatogram window.
2. Scale the chromatogram as desired.
3. Set up peak annotations as desired.
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4. Select the scan desired or perform a Combine operation (background
subtraction).
5. Set up annotations in the Spectrum window as desired.
6. Choose the Print With Chromatogram command from the File menu in the
Spectrum window.
Controlling the Appearance of the Display
Each spectrum window has its own set of Display Parameters, which determine the
appearance of the spectrum display. You can inspect and alter the parameters for the
current spectrum window from the Spectrum Display dialog.
Changing the display parameters
1. To display the Spectrum Display dialog, select View from the Spectrum Display
menu.
2. Make any changes to the following parameters and click OK.
Normalize Data To
This set of parameters specifies the scale on the intensity axis.
Largest Peak
450
If selected, then 100 % on the intensity axis represents
Spectrum
on Display
the intensity of the most intense peak currently on the
display.
Base Peak in
Spectrum
If selected, then 100 % on the intensity axis represents
the intensity of the most intense peak in the spectrum.
Mass
If selected, then 100 % on the intensity axis represents
the height of the peak at the specified mass.
Intensity
If selected, then 100 % on the intensity axis represents
the specified intensity.
Baseline at
Zero
If selected, the vertical axis is scaled from 0 %
Baseline
If you select Baseline and specify an intensity offset,
the vertical axis is scaled from your specified
intensity. This option can be useful for displaying
spectra that have a raised baseline.
Link Vertical
Axes
When comparing two spectra by overlaying them on
the same mass scale, it may be useful to plot both
spectra on the same intensity scale also. Link Vertical
Axes allows you to do this; if you select this option all
axes in the current window will be given a common
vertical scale.
Data Threshold
When processing centroid type data, it can be useful to specify an
intensity threshold. Peaks whose intensity is less than the threshold will
not be displayed. There are two methods of specifying a threshold:
% Full Scale
Allows you to set a threshold as a percentage of the
intensity of the largest peak in the spectrum.
Intensity
Allows you to set an absolute intensity threshold.
The threshold parameters are not applicable to continuum mode data.
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Spectrum
Style
Overlay
Graphs
If selected, multiple traces in the same window will be
superimposed on the same axis. If deselected, the
traces will be drawn on separate axes, arranged
vertically. When spectra are overlaid only the currently
selected trace is annotated.
Fill Trace
If selected, the area under the spectrum trace will be
colored. This option only applies to continuum-type
(not centroid) data.
Graph Header
Allows you to turn off the header information normally
displayed at the top of the spectrum in order to produce
data for publication. If selected, the header will be
displayed; if deselected, the header will not be
displayed.
Process
Description
Each process performed on a spectrum adds a
summary of its parameters to the spectrum's header.
The Process Description option allows you to turn
off only the process information, and leave the
remainder of the header on the spectrum.
Graph Header over-rides Process Description. That is, if the Graph
Header is turned off, the Process Description will be as well.
Split Axis
Is enabled when Overlay Graphs is selected. Split
Axis allows you to change the aspect ratio of the
spectrum by dividing the mass axis into segments, then
arranging the segments vertically. For example, if a
spectrum from 40 to 340 amu is on display, and you
select 3 from Split Axis, the display will show three
axes, one from 40 to 140 amu, one from 140 to
240 amu, and one from 240 to 340 amu.
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Overlay Step
(%)
The Overlay Step X (%) and Overlay Step Y (%)
parameters are enabled when Overlay Graphs is
selected. Overlay Step (%) allows you to offset each
subsequent spectrum trace by a percentage of the
corresponding axis, which can make it easier to
examine overlaid traces. Entering a value in the X field
will offset each new trace horizontally. Entering a value
in the Y field will offset each new trace vertically.
Entering values in both will offset each new trace
diagonally.
Grid
Allows you to fit a grid to the Spectrum display. The
pattern of the lines that make up the grid can be chosen
as Dot, Dash, or Solid.
Header
Clicking Header displays the Header Editor, which
allows you to edit the header information displayed at
the top of the window.
Controlling the Appearance of Peak Labels
Each spectrum window has its own set of Peak Annotation parameters that
determine the appearance of peak labels. You can inspect and change the parameters
for the current spectrum window from the Spectrum Peak Annotation dialog.
Changing the peak annotation parameters
1. Select Peak Annotation from the Spectrum Display menu.
2. Make any changes.
3. Click OK.
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Annotation Type
Decimal
Places
Affects the precision to which mass labels are displayed. You
can select between zero and four decimal places on masses.
This parameter does not affect intensity labels, which are
always displayed as integers. In general, only one decimal
place is significant for quadrupole GC/MS data, and usually
none are displayed.
There are several types of peak labels. Some are always
available; others are the result of a specific process. All can
be controlled separately by means of a set of checkboxes.
Mass
If selected, peaks in the current spectrum window will be
labeled with their masses to the specified number of decimal
places.
Intensity
If selected, peaks in the current spectrum window will be
labeled with their intensity as an integer value.
Annotation Threshold checkboxes allow you to specify a minimum intensity
for a peak to be labeled.
454
% Full Scale
Allows you to set a threshold as a percentage of the base peak
intensity.
Intensity
Allows you to set an absolute intensity threshold.
Spectrum
Level
Determines the number of labels that appear on the
chromatogram. The level can be set to High, Medium, or
Low.
Annotating a particular peak
•
Hold down the CTRL key and right-click the peak you want to annotate with the
mass label.
•
To remove the mass label from the peak, hold down the CTRL key and rightclick the peak a second time.
Removing Spectra from the Display
You can remove the currently selected spectrum by pressing the DELETE key. A
dialog will ask you to confirm the deletion. Clicking OK will remove the spectrum
from the display. This operation does not affect the data stored on disk.
You can also remove traces using the Remove Spectra dialog. This is a faster
method if you want to remove more than one spectrum.
Removing multiple spectra from the display
1. Select Remove from the Spectrum Display menu.
2. The spectra in the current window are listed in the order in which they appear on
the display. You can select one or more spectrum by clicking in the list.
Clicking again on a selected item will cancel the selection. You can select all the
spectra by clicking All.
3. Click OK to exit.
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TurboMass Software User’s Guide
Real-time Display of Spectra
You can display each new spectrum as a data file is being acquired by clicking
or by selecting Real-Time Update from the Spectrum Display menu.
Each spectrum window has a separate real time update switch. You can see the state
of the switch for a particular window by seeing if
is selected or by making that
window current, then choosing the Spectrum Display menu. If real-time update is
enabled for the current window, Real-Time Update has a check mark next to it.
Changing the Order of Displayed Spectra
When a window contains multiple traces, you can change the order in which spectra
are displayed. The first spectrum in the list is displayed at the bottom of the window.
The first spectrum is displayed on top of the others, if traces are overlaid.
Select Move To First from the Spectrum Display menu to display the currently
selected spectrum at the bottom of the display.
Select Move To Last from the Spectrum Display menu to display the currently
selected spectrum at the top of the display.
Adding Text to the Spectrum Display
To add text labels to the spectrum display, click
. When selected, the Text
toolbar button changes color to show that it is active. Move the mouse to where you
want to position text and left-click to open the Edit Text String dialog.
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Spectrum
Enter the text in the Text field, select desired options and click OK. You can change
the position of the user text by dragging it to a new position. Use the handles at the
sides or corners of the text box to size the text. If you want to edit the text, doubleclick it to redisplay the Edit Text String dialog.
The font and color of the user text can be changed in the Colors and Fonts option
on the TurboMass Tools menu. Any changes made to fonts or colors will only apply
to text added after the changes. If you want to change existing text, you must delete
and reinsert it. Other formatting options available for user text are as follows.
Justification
Text can be aligned to the left, right, or center of the text area.
Border
If selected, draws a box around the user text.
Vertical
If selected, displays text vertically rather than horizontally.
Autosize
If selected, causes the text area to be initially defined just large
enough to hold the user text. If not selected, two boxes will
appear on the display. You must select one of them, and drag
until text area is the required size.
Attach to
Axis
If selected, text can only be positioned within a box defined by
the intensity and time/scan axes. If not selected, text can be
positioned anywhere on the display.
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Processing Spectra
The following procedures describe how to manipulate processed spectra data.
Saving and Recalling Processed Spectra
The spectra resulting from any spectral processing can be saved with the raw data.
Saving a processed spectrum
1. Select the processed spectrum in the Spectrum window, and select Save
Spectrum from the Spectrum File menu.
The Spectrum Save dialog will be displayed giving a brief description of the
process you want to save
2. Click OK to save the process and exit.
Reloading processed data into Spectrum
1. Click Open from the Spectrum File menu.
2. Select the raw data file from which the processed data were obtained, and click
History to open the History Selector dialog.
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Spectrum
3. From the Process History list, select the processed data you want to load.
4. Click OK to exit the History Selector dialog.
5. Click OK to exit the Data Browser and open the processed data.
Refine
The refine process operates on centroid-mode data only. Its purpose is to identify
just those masses that contribute to a specific peak in the TIC.
You identify a particular TIC peak by specifying the peak top scan. You supply two
parameters for the process: window size (based on GC peak width n scans) and
noise threshold.
The refine algorithm proceeds by generating the summed mass chromatogram over a
range of 1 Da centered on each integer mass in turn. It examines these chromatograms
for a number of scans equal to the window size around the peak top scan. If there is a
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TurboMass Software User’s Guide
peak present in this range whose topmost point is within one scan of the peak top scan
and more intense than the noise threshold value, then this mass will appear in the
refined spectrum. Note that it is very important to be on the peak apex when using this
function.
Refine is a good alternative to background subtraction (Combine) when performing
library searches or selecting spectra for a Quantify method.
To refine a scan in a centroid-mode data file
1. Identify the scan at the top of the peak you are interested in. Display this scan in
a spectrum window by double-clicking the chromatogram peak.
Choose Refine from the Spectrum Process menu. Enter values for Window size and
Noise threshold. Window size is the half width in scans at baseline of the TIC peak
of interest. For the first run, set Noise threshold to zero to show all peaks.
2. Choose OK.
If the noise level in the refined spectrum is unacceptable, repeat the refine operation
with a higher Noise threshold setting. Values in the range 0-10 are recommended.
OR
•
Refine the current spectrum using the current refine parameters by choosing
on the Spectrum toolbar.
Combine
The combine process operates on centroid-mode or continuum data. Its purpose is to
produce a single scan from all the scans across a TIC peak. The combined scan
exhibits enhanced signal-to-noise and improved mass accuracy.
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Spectrum
You specify three scan ranges and a background factor. One range contains the
scans across the peak top and the other two ranges contain scans from the
background, on each side of the peak. The scans across the peak top are averaged
together and the average of all the background scans, multiplied by the background
factor (X), is subtracted from the result.
Peak separation is the spectral peak width in Da. For centroided data the peak
width can be determined from inspection of the tune peaks on the Tune page. The
Combine algorithm combines peaks within a Peak separation window into a single
peak. Clicking Reset will remove all values that have been entered into the dialog.
Combining scans in a centroid-mode data file
1. Display the chromatogram peak of interest in a chromatogram window.
2. Select Combine from the Spectrum Process menu.
3. Enter the peak top scan range either by entering scan numbers separated by a
colon (for example, 619:626) into the Average field, or by right-clicking
dragging the mouse across the peak.
4. Optionally, enter one or two background scan ranges. Again, you can do this
either by entering scan numbers into the Subtract field, or by right-clicking and
dragging the mouse. If you enter the values, each range should be in the form of
two numbers separated by a colon, as above; and, if there are two ranges, they
should be separated by a comma (for example, 606:612,631:637). If you use the
mouse, right-click and drag the mouse across the first background scan range;
then optionally repeat for a second range.
5. Optionally, enter a background factor in the X field.
6. Optionally, enter a Peak separation value.
7. Click OK.
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TurboMass Software User’s Guide
Subtract
Background Subtract adjusts the zero level in a continuum spectrum to lessen the
effect of chemical noise caused, for example, by column bleed. A low order
polynomial is fitted to the data to remove a constant, sloping, or curved background
from a spectrum.
The algorithm fits a polynomial of specified order (zero is a flat baseline, one is a
straight, sloping line, two is a quadratic shape, etc.) to a spectrum such that a
specified percentage (usually 30 % - 50 %) of the data points in the spectrum lie
below the polynomial. This operation is performed to an arithmetical tolerance that
you specify.
The Background Subtract process also gives you the option to display a graph of the
baseline, which will be fitted to the data before doing the Background Subtraction.
Subtracting the background from a continuum spectrum
1. Select Subtract from the Spectrum Process menu to open the Background
Subtract dialog.
2. Set the Polynomial order parameter to 0 for a flat baseline, 1 for a sloping
straight baseline, or 5 for a curved baseline.
3. If desired, the Below curve (%) parameter can be changed from its default value
of 40 %. The effect of increasing this parameter is to raise the zero level in the
spectrum. Half the noise lies above the zero line, and half below. Therefore half
of 80 %, or 40 % of the total number of data points, should lie below the
background zero level.
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Spectrum
4. If desired, you can change the Tolerance parameter from its default value of
0.01. Increasing this parameter causes the algorithm to terminate sooner, but the
result may not be as good.
5. If you want to see what the effect of this Background Subtraction would be on
the data before actually performing the run, select Make a graph of fitted
polynomial and click OK.
TurboMass displays a graph of the polynomial function that would be subtracted
from the spectrum above the resulting subtracted spectrum.
If you select Link Vertical Axes and Overlay Graphs from the Spectrum
Display dialog, the new baseline will be superimposed on the existing data.
6. When you are satisfied with the parameters, deselect Make a graph of fitted
polynomial.
7. Click OK.
The Background Subtract dialog indicates the progress of the subtract algorithm.
After every iteration, the convergence value in the dialog is updated. The
algorithm terminates when convergence is less than tolerance.
Select the appropriate parameters in the Spectrum Display dialog to choose
whether to view the zero level and negative data in the spectrum.
When Flatten edges is selected, TurboMass verifies that the polynomial
applied is flat or horizontal at the beginning and end of the trace.
Smooth
Smoothing reduces the high-frequency noise present in a spectrum, thus aiding
interpretation. We strongly recommend that you smooth data before attempting mass
measurement with the Center process; otherwise peaks may result from the noise
spikes.
Three types of smoothing are available in TurboMass: Mean, Median, and Savitzky
Golay. The most generally useful technique is Mean. Using Savitzky Golay
smoothing will allow you to use a heavier smooth without broadening the peak as
much. Median is used for removing noise spikes that are much narrower than actual
real peaks (for example, single ions, electronic spikes).
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TurboMass Software User’s Guide
All three methods slide a window along the data, averaging the data in the window
to produce a point in the smoothed spectrum. The width of the smoothing window in
data points is determined by the data system using the equation:
Halfwidth of smoothing window =
Full peak width at 50% intensity
3δm
Where δm is the spacing between adjacent points on the mass axis, for example,
0.0625 Da for raw continuum/MCA data.
Mean takes the arithmetical mean of the intensities of the data points in the window.
Savitzky Golay takes an average of the intensities weighted by a quadratic curve,
which tends to enhance quadratic-shaped features in the data (peaks!).
Median takes the arithmetical median of the intensities of the data points in the
window. This process is unlike the previous two in that the median smooth iterates
until the spectrum no longer changes. The effect is that the intensity of narrow
spikes is reduced on successive iterations, to background level on convergence.
Smoothing a continuum spectrum
1. Expand a section of the spectrum sufficiently to allow you to estimate the width
of a peak at half height.
2. Select Smooth from the Spectrum Process menu.
3. Set Peak width (Da) according to the value you estimated in step 1.
4. Select a smoothing method.
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Spectrum
If you have selected Mean or Savitzky Golay, you may want to alter the number
of times the smooth is repeated by changing the Number of smooths parameter
from its default value of 2. Increasing this parameter gives a heavier smooth.
NOTE: This parameter has no effect on Median smoothing, which always iterates until the
spectrum is unchanged.
5. Click OK.
The Median smoothing algorithm has the side effect of producing peaks with
flattened tops. For this reason, it is recommended that you follow a Median
smooth with a single iteration of a Mean or Savitzky Golay smooth.
Center
Peak centering uses all the points across a peak in a continuum trace to calculate the
mass of the peak center.
You can use the centering process to either label each peak with the calculated mass,
or to produce a single stick from each peak in a continuum spectrum. The
calculation can be performed in three ways:
•
Select the most intense (top) point on the peak.
•
Calculate the centroid of the peak. This is equivalent to finding the vertical line
passing through the center of gravity of the peak. This will provide a more
accurate mass measurement, unless the peak contains a coeluting compound.
•
Calculate the median of peak area. This is equivalent to drawing the vertical line
such that half the area of the peak lies on either side.
There is little practical difference between the median and centroid methods, though
it may be the case that the median is a more robust statistic on very asymmetric peak
shapes. You should not compare masses from different experiments obtained by
centering with different methods.
The centering algorithm looks for the trace rising then falling to indicate the top of a
peak. You specify how many data points must be visible as a clear peak top before
the algorithm turns the peak into a stick.
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TurboMass Software User’s Guide
For the centroid method, you also have the option of using only a specified fraction
of the resolved part of the peak. This will help to avoid the mass given to the stick
being affected by unresolved neighboring peaks.
Centering a continuum spectrum
1. First background subtract, then smooth the spectrum. Background subtraction
will tell the centering algorithm how much of the spectrum is noise, and
therefore reduce the amount of noise seen in the resultant stick spectrum.
Smoothing will help the centering algorithm make sensible decisions about
whether groups of data points represent peaks, or noise spikes.
2. Select Center from the Spectrum Process menu to open the Spectrum Center
dialog.
3. The Min peak width at half height (channels) parameter determines how
many data points must be visible in the expected shape across the peak top, that
is, minimum width. For continuum/MCA data, setting this parameter to 4 is
safe. As there are 16 data points collected per Dalton, the value 4 is equivalent
to 0.25 Da.
Too low a setting of the peak width parameter will result in the centering
algorithm producing sticks from the high-frequency noise.
Too high a setting of the peak width parameter will result in the centering
algorithm misinterpreting many peaks to produce a single stick.
4. Select a centering method.
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Spectrum
5. If you have selected Centroid top (%), you may want to alter the fraction of the
resolved portion of the peak that is used to calculate the centroid from its default
value of 80 %. Values in the range 60 % - 95 % are reasonable.
6. If you want to generate a stick spectrum, select Create centered spectrum. The
height of the sticks can either represent the intensity of the continuum trace at
the mass of the stick (select Heights), or the sum of the intensities of the points
across the peak in the continuum trace (select Areas). The stick spectrum can be
added to the current spectrum window, replaced with the current spectrum, or be
placed in a new window.
7. Select Add, Replace, or New window, as appropriate.
8. Click OK.
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TurboMass Software User’s Guide
Copying to and from the Windows Clipboard
The Windows Clipboard provides temporary storage for information that is being
transferred between application programs (word processors, spreadsheets,
TurboMass etc.). You can use the Clipboard to move data in or out of the Spectrum
window, either as a picture or as a text list. For example, you can paste spectra or
chromatograms into reports written with a Windows compatible word processor.
TurboMass can copy a Spectrum picture to the Clipboard as a metafile giving
greatly improved resolution. When the metafile is pasted into another windows
application it can be rescaled if required without distorting the original image as
long as the original aspect ratio is maintained. When you use the TurboMass Edit
Copy Picture command both a metafile and a bitmap are copied to the Windows
Clipboard.
Copying a spectrum as a picture to the Clipboard
1. Produce the required display in a Spectrum window.
2. Click
OR
Select Copy Picture from the Spectrum Edit menu to copy the contents of the
window to the Clipboard as both a metafile and a bitmap.
3. To read the image into another application as a metafile, select Paste from the
other application's Edit menu. If you select Paste Special from the other
application's Edit menu, you will be given the option of pasting either the
metafile or the bitmap.
Copying a spectrum as a text list to the Clipboard
1. Display the required mass range in a Spectrum window.
468
Spectrum
2. Click
OR
Select Copy Spectrum List from the Spectrum Edit menu. The section of the
spectrum on display will be transferred to the Clipboard as (mass, intensity)
pairs.
3. To read the information into another application, select Paste from the other
application's Edit menu.
Pasting information into a spectrum window from the Windows
Clipboard
1. Click
OR
Select Paste from the Spectrum Edit menu to paste the default Clipboard
object to Spectrum.
2. Select Paste Special to choose which object to paste into Spectrum. These
objects would typically be metafiles, bitmaps, or text.
3. Use the mouse to move the outline of the image to the required position.
You can paste the contents of the Clipboard, (whether a bitmap, a metafile, or
text,) into a spectrum window. If in textual or metafile form, you can rescale
data using the mouse and there will be no distortion of the image. However if
you paste a bitmap, rescaling is done by stretching the image, which will cause
some distortion. To avoid this, scale the image to the required size before you
copy it to the Clipboard.
Removing pasted input from the display
1. Left-click to select the item you want to remove.
2. Press DELETE.
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TurboMass Software User’s Guide
Manipulating Library Spectra
Displaying a library entry
1. Select Get Spectrum from the Spectrum Edit Library menu.
2. If required, select a new library by clicking File.
3. Enter an entry number in the Entry field.
4. You can add the library spectrum to the current spectrum window, replace the
current spectrum, or be placed the library spectrum in a new window. Click
Add, Replace or New, as appropriate.
5. Click OK.
Once you have displayed a spectrum from a library, you can browse the rest of
the library by clicking
.
Appending the current spectrum to the current library
1. Select Append from the Spectrum Edit Library menu.
2. Click OK.
Adding the current spectrum to a new library
1. Select Append from the Spectrum Edit Library menu.
2. Click File.
3. Enter the name of the user library to be created for File Name.
4. Click Open.
5. Click OK.
NOTE: For this spectrum to be used for library searching it first must be processed by
Index Library in the Library Search Process menu.
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Spectrum
Strip and Combine
Functions
15
471
Strip and Combine Functions
Strip Functions
The Strip application removes unwanted background and noise from a data file.
Processing a data file using Strip creates a new file that is stored in the same format
as a raw data file and can be displayed and processed in the same way as a raw data
file. The original input file is retained unmodified.
Opening the Strip application
Select Strip from the TurboMass top level Tools menu
OR
Click
to open the Strip Datafile dialog.
NOTE: The Strip application cannot be accessed while the Combine Functions
application is opened. Likewise, the Combine Functions application cannot be
accessed while the Strip application is opened.
Strip provides four processing options: Subtract, Enhance, Cluster, and CODA.
Subtract
Can subtract either a single background spectrum or a whole data
file from the input file. Processed spectra can be subtracted,
enabling averaged spectra to be used as background. Both
centroid and continuum type files can be subtracted; different
types cannot be mixed.
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TurboMass Software User’s Guide
Enhance
Removes noise from continuum data files. It examines each data
point, and its close neighbors, to determine if it is noise or part of
a real feature. Data points not considered to be valid are removed
from the output data file. Enhance can significantly reduce data
file size.
Cluster
Detects pairs or triplets of peaks separated by a specified mass
difference. Parameters specified are mass differences and
expected intensity ratios, both with tolerances, together with a
time window and a global threshold. The resulting data file will
contain only these peaks. Again, Cluster will significantly
reduce data file size.
CODA
(COmponent Detection Algorithm) essentially removes mass
chromatograms that represent background from the dataset. Each
raw mass chromatogram is compared to a smoothed,
standardized mass chromatogram, and masses in which the
background is high or in which spikes are present are rejected.
Creating a Subtracted Data File
The following section describes how to create a subtracted data file and provides
examples.
1. Select Subtract in the Strip Datafile dialog.
2. To change Input File or to select a subrange, click Input. Select Input File and
Function by clicking File to open a browser dialog. Set the Mass and
Retention Time ranges if required.
3. To change Background File or Scan number, click Background. Select the
Input File and Function by clicking File. Enter Background scan number or
select Use all background file if the entire file is to be used. If a previously
generated spectrum process is to be used, click File to open the browser, and
click History within the browser.
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Strip and Combine Functions
4. If the default Output file name is not correct, click Output and enter the
required name.
5. Set the Subtract parameters by selecting Subtract Datafile Options from the
Strip Options menu.
6. Click Process to start processing the data file. The status bar at the bottom of
the Strip dialog displays the progress of the current process.
The lower trace shows the TIC chromatogram of the V50 data file. The upper trace
shows the TIC chromatogram of the same data file after a background scan (scan
761 at retention time 32 min) has been subtracted.
50ppm. Volatile Organic Analysis Calibration Standard.
V50A
100 0.99
Scan EITIC
6.53e5
Area
%
7.67
14.10 15.98
10.43 13.35
2.03
0
V50
0.99
100
19.61
26.20 27.58 30.38
21.99 24.87
37.85
34.0536.06
Scan EITIC
6.69e5
Area
%
2.03 3.20
0
5.00
7.67
14.10 15.98
10.43 13.35
10.00
15.00
27.58
19.61
30.38
24.87 26.20
21.99
20.00
25.00
30.00
37.85
34.0536.06
35.00
rt
The illustration shows an example of subtracting a complete data file from another
data file. The lower trace shows a mass chromatogram from the blank sample, the
middle trace shows a mass chromatogram from the analyte sample, and the upper
trace shows the result of subtracting the blank data file from the analyte data file.
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TurboMass Software User’s Guide
LMD25A
100
SIR of 2 Channels
%
0
LMD25
100
706.30
3.77e5
Area
10.61
8.03
14.32
1.58
14.76
SIR of 2 Channels
10.61
706.30
3.77e5
Area
8.03
%
14.32
15.94
0
LMD12
100
1.60
4.17
SIR of 2 Channels
706.30
3.77e5
Area
15.79 17.35 18.96
%
6.78
0
476
17.66
1.71
2 00
11.27
4.19
4 00
6 00
8 00
10 00
12 00
14.06
14 00
16 00
18 00
20 00
rt
22 00
Strip and Combine Functions
Creating an Enhanced Data File
This section describes how to create an enhanced data file and provides examples.
1. Select Enhance in the Strip Datafile dialog.
2. To change Input File or to select a subrange, click Input. Select the input file
and function by selecting File to open a browser dialog. Set the mass and
retention time ranges if required.
3. If the default Output file name is not correct, click Output and enter the required
name.
4. Select Enhance Datafile Options from the Strip Options menu to set the
Enhance parameters.
5. Click Process to start processing the data file. The status bar at the bottom of
the Strip dialog displays the progress of the current process.
The following illustration shows two chromatogram traces. The lower trace is the
raw data file. The upper trace shows the same data file after it has been processed
using Enhance. As you can see the background noise level has been greatly reduced
in the enhanced data. The original data file size of 19 MB has been reduced to
0.5 MB in the enhanced data file.
TH01R
100
31.56
29.01
%
25.87
20.17
12.18 16.5217.37
21.11
8.87
1.64
0
TH01
100
%
0
TIC
1.41e9
Area
35.73 39.47
44.91
31.14
1.64
TIC
1.89e9
Area
29.01
20.09
16.5217.37
21.11 25.87
12.18
15.92
11.59
8.95
5 00
10 00
15 00
20 00
25 00
35.73 39.47
30 00
35 00
40 00
44.91
45 00
50 00
rt
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TurboMass Software User’s Guide
The following illustration shows part of a single scan from the raw and enhanced
data files. The background noise in the enhanced spectrum has been greatly reduced.
TH01R 384 (32.667)
100
%
0
TH01 384 (32.667)
100
%
0
Da/e
In the following illustration the lower trace is the raw data file, the upper trace
shows the same data file after it has been processed using Enhance to reduce
background noise. The original data file size of 41.2 MB has been reduced to 1.4
MB in the enhanced data file.
FET01C
Scan ES+
TIC
1.23e8
Area
32.43
100
20.55
42.55
7.59
%
9.34
6.10
13.26
26.22
30.54
35.80
51.33
18.39
58.35
24.33
3.54
54.84
47.55
39.18
0
FET01
32.43
100
20.55
7.59
%
3.54
6.10
9.34
26.22
13.26
18.39
TIC
2.00e8
Area
42.55
30.54
35.80
42.15
24.33
51.33
54.84 58.35
43.77 47.41
60.37 61.32
0
25
50
75
100
125
150
175
200
225
250
275
300
325
350
375
400
425
450
Scan
Creating a Clustered Data File
The following describes how to create a clustered data file and provides examples.
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Strip and Combine Functions
1. Select Cluster in the Strip Datafile dialog.
2. To change Input File or to select a subrange, click Input. Select input file and
function using by choosing File to open a browser dialog. Set the mass and
retention time ranges if required.
3. If the default Output file name is not correct, click Output and enter the
required name.
4. Select Cluster Datafile Options from the Strip Options menu to set the Cluster
options.
5. Click Process to start processing the data file. The status bar at the bottom of
the Strip dialog displays the progress of the current process.
The illustration shows the spectrum of a mixture of chlorinated and non-chlorinated
compounds. The lower trace is the raw data file, the upper trace shows the same data
file after it has been processed using the Cluster option to show pairs of peaks
differing in mass by 2 Da. The illustration shows the spectrum of a mixture of
chlorinated and non-chlorinated compounds.
V50B
Scan EI+
TIC
8.36e4
7.67
100
%
11.89 13.35
14.14
18.23 19.61
26.00
27.58
15.52
0
V50
100
Scan EI+
TIC
6.69e5
0.99
%
27.58
24.87 26.20
19.61
7.67
2.03
3.20
10.43 13.35
14.10 15.98 17.98
21.99
30.38
34.05
36.06
0
5.00
10.00
15.00
20.00
25.00
30.00
35.00
37.85
Time
Creating a CODA Data File
The following describes how to create a CODA data file and provides examples.
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1. Select CODA in the Strip Datafile dialog.
2. To change Input File, click Input to open a browser dialog. Note that input mass
range cannot be changed and all functions are processed irrespective of function
selected.
3. If the default Output File name is not correct, click Output and enter the
required name.
4. Select CODA Options from the Strip Options menu to set the CODA options.
5. Click Process to start processing the data file. The status bar at the bottom of
the Strip dialog displays the progress of the current process.
UCSF20C
TIC
6.48e8
100
30.40
%
38.06
44.04
44.42
45.10
52.38 53.44 56.54
60.86
64.57 67.53 69.12
0
UCSF20
48.82
30.48
67.61
52.45
44.04
100
45.56
53.51
53.67
49.12
56.62
63.43 66.62
38.13
69.65
49.58
%
37.15
21.61
0.17
8.35
11.54
16.00
19.42
24.64
29.57
38.89
41.47
33.82
14.42
0
50
100
150
TIC
6.48e8
200
250
300
350
400
450
500
550
600
650
700
750
800
850
900
Scan
Selecting a Data File to Process
The Input section of the Strip Datafile dialog identifies the data file and function
number that will be processed.
Changing the current input file
Select Input from the Strip File menu to open a Datafile Browser dialog from
which a new file, function, and directory can be selected.
By default, TurboMass will process the entire selected function.
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Selecting a new input file automatically defaults the name of the output file.
Selecting a Data File and Subrange to Process
NOTE: CODA does not allow subrange selection. This is because all functions in the
dataset are processed.
Processing a mass or retention time subrange of the input file has the advantages of
reducing both processing time and the size of the resulting output file.
Selecting a different file and function
1. Select File to open the Strip Data Browser dialog.
2. Selecting a new file automatically defaults mass and retention time to full range.
3. Enter values for the Mass Range and Retention Time range that you wish to
process.
These ranges can be set from Spectrum and Chromatogram respectively, by
right-clicking and selecting the desired range.
4. To set the Mass Range parameters, right-click at one end of the Spectrum
region of interest, and drag the mouse horizontally to the other end. TurboMass
indicates the range you have selected. The Input Datafile dialog will be updated
to show the new mass range.
5. To set the Retention Time parameters, right-click at one end of the
Chromatogram region of interest, and drag the mouse horizontally to the other
end. TurboMass indicates the range you have selected. The Input Datafile dialog
will be updated to show the new retention time range.
6. Click Default to set both mass and retention time to the full range of the current
file.
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Selecting a Background Data File
The Background section of the Strip Datafile dialog identifies the data file,
function, and scan number to be used as background when performing the Subtract
process. Previously processed spectra can be used as background. The background
file is not used for Enhance processing.
Subtracting a background file
1. Click Background in the Strip Datafile dialog to open the Subtract Background
File dialog.
2. To select a different file and function, click File to open the Strip Data Browser.
3. A previously processed spectrum can be selected by clicking Browser History.
Selecting a new file automatically defaults to the first scan in the data file.
4. If a single background scan is to be subtracted, enter the scan number in the
Background scan field. The scan number can also be set from Spectrum and
Chromatogram by right-clicking and selecting the desired scan.
If Background scan is deselected, deselect Use all background file.
5. To subtract the entire background file, select Use all background file. In this
case, the background scan with the closest retention time to each input scan will
be subtracted.
Selecting an Output Data File
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The Output section of the Strip Datafile dialog identifies the data file that will be
created by Strip when processing.
When an Input File is selected, the Output File defaults to the same directory and a
name based upon the Input name with an extra letter appended. For example, if the
input file was \turbomass\data\v50.raw the default output file might be
\turbomass\data\v50a.raw. When defaulting the output name, TurboMass attempts to
choose a name that does not already exist.
Changing the default output file and directory
1. Click Output in the Strip Datafile dialog to display the Output File dialog.
2. Enter a name for the output file.
To change the directory of the file, enter the full path name of the file.
Setting Subtract Datafile options
1. Select Subtract Datafile Options from the Strip Options menu to display the
Subtract Datafile Options dialog, and enter the appropriate values.
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Peak Width
This parameter is the spectral peak width in amu. It is only
used when subtracting centroid data. The peak width can be
determined from inspection of the tune peaks on the Tune
page. The peak width is used to determine if peaks present in
the input and background data represent the same peak.
Background
multiplication
factor
This is applied to the intensities of the peaks in the
background spectra before they are subtracted from peaks in
the input spectra. This provides a method of adjusting the
height of the subtracted background.
2. To set parameters to their default values, click Default.
Setting Enhance Datafile Options
Enhance operates on continuum data only. It works by examining each spectrum
data sample to determine if it is a noise spike or part of an actual peak. This is
achieved by looking at neighboring samples on the mass scale and at the same area
in the preceding and following scans.
For example, using the values in the Enhance Datafile Options dialog, two samples
either side of the current sample will be examined, including the current sample.
This makes five in all. One scan either side of the current scan will be used, so
including the current scan three scans will be used. Multiplying the number of scans
by the number of samples in each scan shows 15 samples are examined in all.
Consequently for a sample to be accepted 60 % of these samples (nine samples)
must have an intensity greater than the specified Intensity Threshold.
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Setting the Enhance processing parameters
1. Select Enhance Datafile Options from the Strip Options menu.
2. Set the following parameters as required.
Mass (data
points ±)
Determines how many samples to look backwards and
forwards along the mass scale. The Mass parameter should
not exceed half the number of samples that make up a peak.
Scans (±)
Determines how many scans to look backwards and
forwards, respectively. It should not exceed half the number
of scans a chromatogram peak is present.
Intensity
Threshold
Defines an absolute intensity that a data point must exceed
to be regarded as being significant. For spectra with a high
baseline, this parameter will need adjusting so that its value
is approximately equal to the intensity at the top of the noise.
The larger this value the more likely that information will be
discarded as being noise.
Minimum
Abundance
(%)
Determines the minimum percentage of neighboring samples
examined whose intensity must be above the specified
threshold for the current sample not to be rejected as noise.
The larger this value the more likely that a sample will be
discarded.
3. To set the parameters to their default values, click Default.
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Setting Cluster Datafile Options
Cluster operates on both centroid and continuum data. For continuum data, a special
fast centroid process is used. See Setting Cluster Centroid Options on page 488. The
centroid process works by examining each pair (or triple) of peaks in each spectrum
to determine if they are separated by the correct mass difference(s) and if their
intensity ratios lie in the correct range(s). If Time Window is set to a value other
than zero, then neighboring scans within that time window (+/-) are examined.
For example, using the values in the Cluster Analysis Options dialog; mass
difference 1 22.0 Da, mass difference 2 33.0 Da, both intensity ratios 1.0, mass
tolerance 0.5 Da, ratio tolerance 30 %, time window 0.00 min, threshold 0.01 %.
Triplets will be detected, with the mass difference between the first two peaks being
21.5-22.5 Da, and between the first and third peaks 31.5 - 32.5 Da. The intensity
ratios of the peaks must lie in the range 0.7 to 1.3 (low mass peak / high mass peak),
and the peaks must lie in the same scan. The peaks must be more intense than 0.01
% times the most intense peak in the function.
Setting Cluster processing parameters
1. Select Cluster Datafile Options from the Strip Options menu to open the
Cluster Analysis Options dialog.
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2. Set the following parameters as required
First Mass Diff
and
First Ratio
Second Mass Diff
and
Second Ratio
Determines the requested separation and intensity
ratio of the first pair of peaks. The intensity ratio is
calculated as (intensity of low mass peak) / (intensity
of high mass peak). The requested intensity ratio may
be less than 1. Intensity ratio comparison may be
deselected using Use Intensity Ratios; if not
selected, then no ratio comparison is attempted, and
peaks are selected purely on the basis of mass
difference.
Determines the mass difference between, and
intensity ratio of, the first and third peaks in the
triplet; note, not the first and second. The second
mass difference can be calculated by selecting Use
Second Mass Diff; if not selected, then examination
is restricted to pairs of peaks only, not triples.
Mass Tolerance
Specifies a window (+/-) for each of the (maximum
of two) specified mass differences. Pairs or triples of
peaks are detected if the corresponding peak(s) lay at
the specified mass difference +/- the specified mass
tolerance.
Ratio Tolerance
Specifies the maximum mismatch between specified
and calculated intensity ratios. It is specified as a
percentage of the intensity ratio(s).
Time Window
Determines how far apart scans may lie in which
peaks forming part of the pair/triple are located. For
instance, if time window is +/- 0.5 min, with mass
difference 5.0 amu, then a peak at mass 25.0 Da in a
scan at time 2.2 min will match with a peak at mass
30.0 Da in a scan at time 2.7 min.
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Threshold
Defines an absolute intensity that a data point must
exceed to be regarded as being significant. For
spectra with a high baseline this parameter will need
adjusting so that its value is approximately equal to
the intensity at the top of the noise. The larger this
value the more likely that information will be
discarded as being noise.
3. Click Default to set the parameters to their default values.
Setting Cluster Centroid Options
The Fast Centroid process is unique to the cluster algorithm. It was developed to
reduce the time taken to centroid each scan of a run. Consequently, it will not deal
as accurately with multiplets as the standard centroid algorithm, but should be
perfectly adequate for most applications.
Setting the Cluster Centroid processing parameters
1. From the Cluster Analysis Options dialog, click Centroid to open the Fast
Centroid dialog.
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2. Set the following parameters, and click OK.
Peak width
at base
(amu)
Specifies the expected width of the continuum peaks at
baseline. It has two purposes; first, it determines the
amount of smoothing that is applied to the continuum
spectrum prior to centroiding proper, and second it
determines how close together two sticks must lie in order
to be grouped into a single stick, that is, it controls the
multiplet resolution. For smoothing, the width at half
height of the peak is estimated as half the specified width at
baseline, and it is this estimated value that is used in the
smooth. For multiplet resolution, peaks closer than the
specified Peak width at base distance together will be
regarded as a singlet.
Baseline
threshold
Specifies the minimum signal level in the spectrum above
which a peak will be considered significant.
Top,
Centroid,
Median
These parameters allow a selection of peak Top, peak
Centroid, and peak Median methods to be made. This
functions as for the standard centroid software (see Center
on page 465). Similarly, selection of peak areas or heights
is the same as in Spectrum.
Setting CODA Options
CODA operates on both centroid and continuum data. It works by standardizing and
smoothing each mass chromatogram in the dataset, and then comparing the
smoothed, standardized mass chromatogram with the raw chromatogram. If they are
sufficiently similar, as determined by the MCQ Index parameter, then the mass
chromatogram is preserved; otherwise, it is removed. Essentially, mass
chromatograms that contain spikes or are noisy will be dissimilar after smoothing
and standardization to the raw mass chromatogram and are hence rejected.
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Setting the CODA processing parameters
1. Select CODA Options from the Strip Options menu to open the CODA dialog.
2. Set the following parameters, and click OK.
MCQ Index
Specifies how similar the smoothed, standardized mass
chromatogram must be to the raw mass chromatogram before
it is preserved. The parameter is in the range 0 - 1 inclusive;
a value of 0 will preserve all mass chromatograms and result
in the raw file being copied to the output. A value of 1 will
result in all mass chromatograms being rejected, and an
empty file. Values around the default value of 0.75 are most
useful, with the range 0.65 - 0.85 recommended.
Smoothing
window
Specifies the amount of smoothing given to raw mass
chromatograms. The default value of 5 is usually adequate.
This window is (+/-) a number of data points around the
central point.
Stopping a Process
When you stop a process before completion, the output data file will contain all the
information written up to the point at which the process was stopped.
Click Stop in the Strip Datafile dialog.
Confirmation of the action will be requested.
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Combine Functions
The Combine Functions application provides a way of combining all functions in a
data file to produce a new data file containing a single function, which is the sum of
the multiple functions. The Combine Functions option is particularly useful for
combining functions acquired with CI+ and CI- in the same chromatogram.
To use the Combine Functions option, all the functions in the data file must have
been acquired using the same scan range and scan rate, or must contain the same
SIR ions.
NOTE: The Combine Functions application cannot be accessed while the Strip application
is opened. Likewise, the Strip application cannot be accessed while the Combine
Functions application is opened.
Creating a Combined Datafile
1. Select Combine Functions from the TurboMass top level Tools menu
OR
Click
to open the Combine Datafile Functions dialog.
2. To change the Input File or to select a subrange, click Input. Select the input
file by clicking File to open a browser dialog. Set the Mass and Retention Time
ranges, if required.
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3. If the default Output file name is not correct, click Output and enter the
required name.
4. Click Process to start processing the data file.
The status bar at the bottom of the Combine Datafile Functions dialog displays
the progress of the current process.
Selecting a Data File and Subrange to Process
The Input section of the Combine Datafile Functions dialog identifies the data file
that will be processed.
Changing the current input file
1. Click Input from the Combine Datafile Functions dialog. This opens the Input
Datafile dialog from which a new file and directory can be selected.
2. Set the parameters and click OK.
3. Clicking Default sets both Mass Range and Retention Time to the full range of
the current file.
By default, the entire selected file will be processed and all functions will be
combined into a single function. To specify subranges, see below. Selecting a
new input file automatically defaults the name of the output file.
Processing a mass or retention time subrange of the input file has the advantages
of reducing both processing time and the size of the resulting output file.
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Selecting a different file and function
1. Click File to open the Combine Functions Data Browser.
Selecting a new file automatically defaults Mass Range and Retention Time to
full range.
2. Enter values for the Mass Range and Retention Time range that you wish to
process.
These ranges can be set from Spectrum and Chromatogram respectively, by
right-clicking and selecting the desired range.
3. To set the Mass Range parameters, right-click at one end of the Spectrum
region of interest and drag the mouse horizontally to the other end. TurboMass
indicates the range you have selected.
The Combine Datafile Functions, Input Datafile dialog will be updated to show
the new mass range.
4. To set the Retention Time parameters, right-click at one end of the
Chromatogram region of interest, and drag the mouse horizontally to the other
end. TurboMass indicates the range you have selected.
The Combine Datafile Functions, Input Datafile dialog will be updated to show
the new retention time range.
Selecting an Output Data File
The Output section of the Combine Datafile Functions dialog identifies the data file
that will be created by Combine Functions when processing.
When an Input file is selected, the Output file defaults to the same directory and a
name based upon the Input name with an extra letter appended. For example, if the
input file was \mldata1\davlc7.raw, the default output file might be
\mldata1\davlc7a.raw. When defaulting the output name, TurboMass attempts to
choose a name that does not already exist.
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Changing the default output file and directory
1. Click Output in the Combine Datafile Functions dialog to open the Output File
dialog.
2. Enter a name for the output file.
To change the directory of the file, enter the full path name of the file.
Stopping a Process
When you stop a process before completion, the output data file will contain all the
information written up to the point at which the process was stopped.
Click Stop in the Combine Datafile Functions dialog.
Confirmation of the action will be requested.
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Library
16
Library
The Library application is used to identify unknown spectra by comparing the
unknown spectrum to a library of known spectra. The result of a library search is a
list of library compounds or "hits." The spectra in these compounds give the best
match with the unknown spectrum.
This chapter describes how to search the libraries supplied, create your own mass
spectral libraries, and how to use the Library Locator.
NOTE: The terms “scan” and “spectrum” are used interchangeably in this chapter and in
the TurboMass software.
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TurboMass Library Windows
The Library window presents the search results in several formats.
Hit List — Gives a text listing of the best hits. You can format the Hit List window
to display a variety of information about each hit including compound name, fit
values, formula, and molecular weight.
Hits Window — Shows the unknown spectrum followed by the spectra of the best
hits.
Structure Window — Shows the chemical structure of the currently selected hit.
Delta Window — Shows the difference between the unknown spectrum and the
spectrum of a particular hit.
Library also allows you to create your own user libraries that contain spectra from
data files in the Spectrum window.
Library Editor — Used to edit libraries.
Library Locator — Used to examine a library and search for library entries that
meet various criteria.
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Searching a Library
The Library Search process has two parts: the Presearch and the Mainsearch. The
Presearch is a faster search designed to select a number of likely candidates from the
library. These candidates are then passed through to the Mainsearch, where they
undergo a more rigorous and lengthy comparison. TurboMass displays the
Mainsearch results in the Hit List, Hits, Structure, and Delta windows.
The Presearch
The unknown spectrum is first reduced to its eight most intense mass-weighted
peaks. This reduced spectrum is then compared to the current library Presearch file.
The library Presearch file contains a spectrum for each library entry that has been
reduced to its eight most intense mass-weighted peaks. The Presearch process
results in a list of the most likely candidates to be passed to the Mainsearch process.
The most likely candidates are those compounds that have the greatest number of
matching peaks with the unknown compound. You can control how many
candidates are passed to the Mainsearch by changing the Match By parameter in the
Library Search Parameters dialog.
The Mainsearch
For the Mainsearch the unknown spectrum is again reduced, this time to a number of
peaks, determined by the Sig. Peaks parameter in the Library Search dialog.
The Search spectrum is compared to each of the possible candidates from the
library, and the results of this comparison are displayed in the Hits, Hit List, Delta
and Structure windows. The hits are ranked in order of best fit to the search
spectrum.
You can apply various filters to the Mainsearch process to make it more specific.
These filters contain requirements that must be met in order for the library entry to
be included in the Hits list. These filters can contain information about the
compound elemental formula and molecular weight.
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TurboMass computes two types of fit values for each hit: Forward and Reverse Fit.
The maximum obtainable fit value is 1,000, which represents a perfect match
between the search spectrum and the library entry.
The Forward Fit value shows how likely it is that the search spectrum is a pure
sample of the library entry. Any peaks that are present in the search spectrum, but
not present in the library spectrum, decrease the Forward Fit value. Likewise, any
peaks that are present in the library spectrum, but not present in the search spectrum,
decrease the Forward Fit value.
The Reverse Fit value shows how likely it is that the search spectrum contains the
library entry. In this case, the search spectrum may be a mixture of compounds. Any
peaks present in the library spectrum, but not present in the search spectrum,
decrease the Reverse Fit value. However peaks that are present in the search
spectrum, but not present in the Library spectrum, have no effect on the Reverse Fit
value.
An Overview of Library Searching
This section lists the steps in a library search. Each step is described later in this
chapter.
1. Select the library or libraries that you want to search by selecting Search List
from the Library File menu.
2. Select the search spectrum (scan) from the Spectrum or Library windows:
or
• To select a scan from a new data file from within Library, click
select Open from the Library File menu to open the Library Data Browser.
OR
• To select a new scan from the current data file, click
Spectrum from the Library Display menu.
or select
3. Edit the Library search parameters by selecting Parameters from the Library
Edit menu.
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Library
4. Apply any search filters by selecting Filters from the Library Edit menu.
5. Initiate the Library search from Library or Spectrum by clicking
OR
Selecting Search from the Library Process menu.
6. Adjust the Library display by selecting View from the Library Display menu.
7. Format the Hit List window by selecting Format List from the Library Edit
menu.
8. Print the results of the Library search by clicking
or
OR
Select Print from the Library File menu.
NOTE: All the above settings are retained for future searches and need to be edited only if
you want to change them. You do not need to edit them each time you do a search.
Library Toolbar
At the top of the Library window is a set of buttons called the library toolbar. The
toolbar allows you to perform some of the most commonly used actions with the
click of a button.
Selects a data file.
Prints the current window in portrait format.
Prints the current window in landscape format.
Copies the bitmap of current window to the clipboard.
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Copies the current hit list to the clipboard.
Refines the current search spectrum.
Searches the current search spectrum against the current library.
Arranges the windows in a tiled view.
Arranges the windows in a cascaded view.
Arranges the windows in a stacked view.
Selects a new scan number as the search spectrum.
Toggles to restore the previous display range or to display the default axis
range.
Selecting Which Libraries to Search
The Library application searches one or more Libraries specified in the Library
Search List. These can be standard Libraries such as the NIST or Wiley libraries, or
user libraries.
Building a search list
1. Select Search List from the Library File menu to open the Library Search List
dialog.
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2. To add a library to the search list, click Add.
The Add Library dialog is displayed.
3. Select the library you want to add from the Add Library dialog, and click Open.
TurboMass adds the new library to the Library Search List.
4. To remove a library from the search list, select file you want to remove from the
Library Search List, and click Remove.
5. Click the Close button to return to the Library Hits window.
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Selecting a New Search Spectrum
The spectrum currently displayed in the Library window is the current search
spectrum. From the Library (Hits) window, you can select a new search spectrum
(scan) from one of the following:
•
The data file for the currently displayed spectrum (the current data file)
•
A different data file
•
The Spectrum window
Selecting a new search spectrum from the current data file
1. Click
from the Library toolbar
OR
Select Spectrum from the Library Display menu.
2. Enter the desired scan number or retention time.
to
To obtain the scan number or retention time of a particular peak, click
display the total ion chromatogram, and select Scan or Time as the horizontal
axis unit from the Chromatogram Display menu.
3. To display the new spectrum in the Library Hits window, click Update.
4. Click OK.
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Library
Selecting a new search spectrum from a different data file
1. Click
OR
Select Open from the Library File menu to open the Library Data Browser
dialog.
2. Select the new data file from the File Name list.
3. To select a processed spectrum that is the result of Combine or Refine
processes, click History.
4. Click OK.
The Hits window is updated to show Scan 1 of the new data file, which becomes
the current search spectrum.
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Selecting a new search spectrum from the Spectrum window
, or Display
Select a new spectrum by using the Data Browser, by clicking
Spectrum.
If you initiate the Library search from the Spectrum window, the spectrum
currently displayed in the Spectrum window is used as the search spectrum. For
more information, see Spectrum on page 435.
Setting Library Search Parameters
The Library Search parameters control how many library entries are passed from the
Presearch to the Mainsearch, exactly which entries are used, and how the results are
reported.
Editing the Library Search parameters
1. Select Library from the TurboMass Process menu to open the Library Hits
window.
2. Select Parameters from the Library Edit menu to open the Library Search
Parameters dialog.
3. Edit your library search parameters, and click OK.
Match By
These parameters determine how many candidates or entries are passed from the
Presearch to the Mainsearch.
Level
506
Sets the number of matching peaks that the library entry must have
to be passed to the Mainsearch. You can enter a value from eight to
zero matching peaks. The higher the value, the fewer entries are
passed to the Mainsearch.
Library
Viables
Sets the number of matching peaks to the minimum number of
entries to be passed from the Presearch to the Mainsearch. For
example, if you enter a value of 8, Library first takes all entries that
have eight matching peaks. If the number of entries is less than the
Viables value, Library takes all entries that have seven matching
peaks, adds these to the previous entries, and compares the new
total to the Viables value. This process is repeated until the number
of entries passed to the Mainsearch is greater than or equal to the
Viables value. In practice, the number of entries passed to the
Mainsearch is often much larger than the Viables value.
Sig.
Peaks
Determines how many spectral peaks are compared during the
Mainsearch.
Exclude Masses
Masses
1-4
Allow you to exclude up to four specific masses in the search
spectrum from the Mainsearch. These excluded peaks are not
compared to library entries. This can be useful, for example, to
exclude a contaminating ion that cannot be removed from the
spectrum by any physical or chemical means.
All below
Allows you to exclude all masses below a certain value.
Ranking
These parameters determine whether hits are listed in order of Forward or
Reverse Fit.
Forward
Indicates how likely it is that the search spectrum is a pure sample
of the library entry. Any peaks present in the search spectrum, but
not present in the Library spectrum, decrease the Forward Fit
value. Likewise, any peaks present in the library spectrum, but not
present in the search spectrum, decrease the Forward Fit value.
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Reverse
Indicates how likely it is that the search spectrum contains the
library entry; in this case, the search spectrum may be a mixture of
compounds. Any peaks present in the library spectrum, but not
present in the search spectrum, decrease the Reverse Fit value.
However peaks that are present in the search spectrum, but not
present in the library spectrum, have no effect on the Reverse Fit
value.
Setting Library Search Filters
Library search filters are used to specify certain criteria that a library entry must
meet in order to appear in the Hit List. If you have the molecular weight and
elemental formula of a compound, you can use these filters to refine the search. For
example, if you know that the search compound contains at least one chlorine atom,
you can specify this information in the search filters. If you know that its molecular
weight falls within a certain range, you can specify this information in the search
filters.
Specifying library search filters
1. Select Filters from the Library Edit menu to display the Filters dialog.
2. Change the library search filters as required by setting the following parameters.
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Fit
Specifies a Minimum Forward and/or a Minimum Reverse
Fit value that a library entry must have in order to appear in
the Hit List. To make the filter active select the checkbox next
to it and enter a value between 0 and 1000 into the relevant
field.
Mol Wt
These parameters specify a range within which the molecular
weight of the library entry must fall in order to be included in
the Hit List.
Active
To make the filter active, select Active and enter the minimum
and maximum molecular weights in the Min and Max fields.
Min and
Max
Specifies the minimum or maximum molecular weight that an
element must have for its entry to appear in the Hit List.
To specify a particular molecular weight, enter equal Min and
Max values.
Elements
These parameters specify the number of particular elements
that must be present in the library entry molecular formula in
order for the entry to appear in the Hit List.
Min
Specifies the minimum number of elements that must be
present in an entry in order for it to appear in the Hit List.
Max
Specifies the maximum number of elements that must be
present in an entry in order for it to appear in the Hit List.
Active
To activate the filter specified in the Max/Min fields, select the
Active checkbox.
Enter elemental formulas in the “standard” format as an
element symbol, followed immediately by its count, if greater
than unity, and then immediately by another symbol, as
relevant.
For example, suppose you want to set the Elements parameter
to C6H20NClBr2. Enter symbols in the standard upper and
lower case format. Note that "Cl" does not need a "1" after it
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and that there are no spaces. The specific order of elements is
irrelevant.
If you have a specific formula to match, enter this formula in
both the Min and Max fields, and do not select Include Other
Elements.
If an element appears only in the Min field, there is no upper
limit on the number of atoms of this element that may appear
in the library entry. If an element appears only in the Max
field, there is no lower limit on the number of atoms of this
element that may appear in the library entry.
510
Include
Other
Elements
If selected, other elements may be present in the library entry.
If not selected, the library entry must contain only the
elements specified in the Min and Max fields.
Flags
Specifies a range of values within which a library entry Flags
parameter must lie in order for the entry to appear in the Hits
List. The Flags parameter is only relevant to user libraries.
User
flags
These are strings of one or more characters that have been
entered in the user library. Enter the required text in the User
flags field.
The search for the User flags text is always case sensitive. If
Apply exact is not selected, the library entry must contain the
characters specified in the User flags field. These characters
can appear in any order in the matching library entry.
Apply
Exact
If selected, the library entry needs to contain the characters
specified in the User flags field in the exact order in which
they are entered.
For example, if the Flags parameter is set to Bv, BpKv, vKpB
and KBvp will pass a nonexact search; only KBvp will pass an
exact search.
User
Values
These parameters specify a range within which a library entry
User Value must fall in order for the entry to appear in the Hits
List. The User Values parameter is only relevant to user
libraries.
Library
No. 1 and
No. 2
These are numeric values that have been entered in the user
library. Select the No. 1 and No. 2 values as required.
Min and
Max
Enter a maximum and minimum value for each User Value in
the Min and Max fields. To specify a particular User Value,
make the Min and Max values equal.
3. Click OK.
Starting a Library Search
You can initiate a library search from either Library or Spectrum.
Click
from the Library toolbar
OR
Select Search from the Library Process menu.
OR
from the Spectrum toolbar, or select Library Search from the
Click
Spectrum Tools menu.
Library Search Results
The result of a library search is a list of library compounds, or hits, whose spectra
give the best match with the unknown spectrum.
The results are displayed in four windows:
Hit List — Gives a text listing of the best hits. The Hit List can be formatted to
display a variety of information about each hit including compound name, fit values,
formula, and molecular weight.
Hits — Shows the unknown spectrum followed by the spectra of the best hits.
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Structure — Shows the chemical structure of the currently selected hit.
Delta — Shows the difference between the unknown spectrum and the spectrum of
the current hit.
The mass spectral library is stored in the Idendb sub-directory in the TurboMass
installation directory. The mass spectral structures library is stored in the Structdb
sub-directory in the TurboMass installation directory.
Automatic Library Search
The library search application used for identifying spectra by matching them with a
standard library (for example, NIST) works on a single spectrum when started from
the Spectrum display. Chromatogram has an automated library search facility to
automatically search a number of spectra in a chromatogram.
Note that while automatic library searching can work well for chromatographically
well-resolved peaks, complex chromatograms will probably require manual
background subtraction and library searching.
Using automatic library search in fully-automated mode
1. In the Chromatogram window, set the display range and integration threshold
values to limit the integrated peaks to only those you wish to library search.
2. In the Chromatogram window, click
Process menu.
or select Lib Search Peaks from the
3. The Library search process performs a search for the first peak in the list and
displays the Print dialog.
4. To print results for all currently displayed Library windows, select All
Windows.
5. To print results for the currently selected window, select Current Window, and
click OK.
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Library
6. All other spectra matches will also be printed out in this format.
Using automatic library search in semi-automated mode
1. In the Chromatogram window, set the display range and integration threshold
values to limit the integrated peaks to only those you wish to library search.
2. Integrate the chromatogram of interest.
3. To append specific peaks, select Peak List Write from the Chromatogram Edit
menu, select the desired peaks, and click Append. Repeat for each peak
required.
OR
To append all peaks, click Append All.
4. To automatically remove calculated background spectra, select Auto Refine
from the Library Hits Process menu.
5. Select Search Peak List from the Library Hits Process menu.
The Library search process performs a search for the first peak in the list and
displays the Print dialog.
6. To print results for all currently displayed Library windows, select All
Windows.
OR
To print results for the currently selected window, select Current Window and
click OK.
All other spectra matches will also be printed out in this format.
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Manipulating the Library Display
The appearance of the display can be changed from the Library Display menu.
1. Select View from the Library Display menu to open the Library Display View
dialog.
2. To display a window, select Visible for that window.
3. Edit the Library Display View dialog parameters for each of the Library
windows, and click OK.
Hits Window
Specify how many hits (1 to 4) to display with the search
spectrum in the No. Hits drop-down list.
Header
Displays a header at the top of each window. Clicking
Header opens the Header Editor, where you can edit the
header information. For more information about using the
Header Editor, see The Header Editor on page 54.
Peak Label Threshold
These parameters change peak labeling in the Hits Window and Delta
Window.
Decimal
Places
514
Select 0 to 4 from the Decimal Places drop-down list to
specify the number of decimal places to which peaks are
labeled. You can set a threshold for labeling peaks with
mass.
Library
None
If selected, TurboMass does not display mass labels for
any peaks.
%Full Scale
If selected, this parameter sets a relative intensity
threshold for peak labels.
Intensity
If selected, this parameter sets an absolute intensity
threshold for peak labels. Select Intensity and enter an
intensity value.
4. Use the Window menu commands to arrange the different Library windows.
Hit List Window
The Hit List window gives a text listing of the best 20 hits resulting from the library
search. These hits are listed in order of either reverse or forward fit, depending on
which order was selected as the Ranking parameter in the Library Search
Parameters dialog. You can format the Hit List window to include the following
about each hit:
•
Hit number.
•
Compound name.
•
Forward fit value.
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TurboMass Software User’s Guide
•
Reverse fit value.
•
Chemical formula.
•
Molecular weight.
•
Library entry number.
•
Library.
•
CAS number.
The current hit is that selected in the Hit List window. It is the first hit that is
displayed in the Hits, Delta, and Structure windows. You can make any other hit the
current hit by selecting it in the Hit List window.
Modifying the fields displayed in the Hit List window
1. Select Format List from the Library Edit menu to open the Format DB List
dialog.
The Format list contains the fields currently displayed in the Hit List window.
The Fields list contains additional fields available for display. To change which
fields are displayed, edit these two lists.
2. To add a field, select the field you want to add from the Fields list, and click
Append.
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Library
3. To remove a displayed field from the Hit List window, select the field you want
to remove from the Format list, and click Remove.
4. To insert a new field between two currently displayed fields, select the field you
want to insert from the Fields list, then in the Format list select the field before
which you want to insert the new field, and click Insert.
5. To modify the justification for any fields, select the field for which you want to
change the justification from either the Fields or Format lists, click
Justification to open the List Field Justification dialog, select Left, Right or
Center justification, modify the Field Size Width, Significant Figures (SF), and
Decimal Places (DP) as required, repeat as required, and click OK to return to
the Format DB List dialog.
6. Repeat steps 2 - 5 as required for each change you want to make to the Hit List
window fields.
7. To view the results of your changes without exiting the dialog, click Update.
8. Click OK.
Hits Window
The Hits window displays the search spectrum with up to four of the hits spectra.
The header above each hit spectrum shows the hit number, fit value, the library
name, library entry number, and the compound name.
The mass axis can be zoomed to expand a region of particular interest; these
changes are also reflected in the Delta window.
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You can manipulate the display in a number of different ways:
•
Determine which hits are displayed.
•
Change the range of the mass axis.
•
Restore the display.
Determining which hits are displayed:
1. The first hit displayed is always the current hit, which is the hit selected in the
Hit List window.
2. To change the number of hits displayed, select View from the Library Display
menu, and change the No. Hits value.
The Hits window displays up to four of the next best hits.
Changing the range of the mass axis (zoom):
Left-click at one end of the region of interest and move the mouse horizontally
to the other end.
TurboMass indicates the range you have selected. Do not go beyond the bounds
of the axis. When you release the mouse button, TurboMass redisplays the
selected range to fill the current window.
OR
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Library
1. Select Range From from the Library Display menu.
2. Enter new mass axis From and To values, and click OK.
Restoring the displayed mass axis range:
Toggle the
tool button to restore the display to its previous mass range or to
the default mass range.
OR
Select Range Default from the Library Display menu to display the default
mass range.
Delta Window
The Delta window shows the difference between the search spectrum and the
currently selected hit. Positive peaks are those that are more intense in the search
spectrum than in the hit spectrum. Negative peaks are those that are more intense in
the hit spectrum than in the search spectrum.
The 100 % annotation point of the intensity axis refers to the base peak intensity of
the spectra, before subtraction. The mass axis of the Delta window is always the
same as that of the Hits window and cannot be changed independently.
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Structure Window
The Structure window shows a graphical representation of the chemical structure of
the currently selected hit.
The structural pictures are derived from structure data supplied by the United States
National Institute for Standards and Technology (NIST) and are their copyright. Not
all NIST Library entries have associated structures. If the currently selected hit has
no associated structure, the message "No structure found" appears in the Structure
window.
If the Structure window is blank, it may be because it is too small to contain the
structure. As a quick check, try maximizing the window.
Structures are associated with library entries by their CAS number. If you create a
user library and enter the correct CAS numbers, you can view the structures for the
entries.
The mass spectral structures library is stored in the Structdb sub-directory in the
TurboMass installation directory.
Printing the Results of a Library Search
You can print the library search results displayed in currently selected Library
window.
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Library
Printing the library search results
Click
or
to print in portrait or landscape format, respectively.
OR
Select Print from the Library File menu.
You can choose whether to print all windows or only the current window.
Copying To and From the Windows Clipboard
The Windows clipboard can temporarily store information that is being transferred
from one application to another. You can use the Clipboard to move data out of a
window as a picture and in some cases as a text list.
Copying a picture to the Clipboard
1. Set up the picture you want to copy in its window, and select the window.
2. Click
OR
Select Copy Bitmap from the Edit menu.
The displayed picture is transferred as a bitmap to the Windows clipboard.
Copying the current hit list to the Clipboard
Click
to copy the current hit list to the Clipboard.
Retrieving data from the Clipboard
Many Windows applications have an Edit Paste or similar command to read data in
from the Clipboard. Consult the documentation for more information.
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You can use the Edit Paste command to copy bitmaps into the Spectrum and
Chromatogram applications.
Refining the Search Spectrum
The Refine process is used to identify only those masses that contribute to a specific
peak in the TIC. In this way, Refine Search removes small peaks that are the result
of background noise, and can therefore improve library search results. You supply
two parameters for the Refine process: Window Size and Noise Threshold.
The refine algorithm generates the summed mass chromatogram over a range of 1
Da centered on each integer mass, in turn. It examines these chromatograms for a
number of scans equal to the window size around the peak top scan. If a peak is
present in this range for which the topmost point is within one scan of the peak top
scan, and more intense than the noise threshold value, then this mass appears in the
refined spectrum.
To refine the search spectrum
1. Specify new Refine parameters by choosing Refine from the Library Process
menu to open the Refine Spectrum dialog.
Enter values for Window Size and Noise Threshold. Window Size is the half-width
in number of scans at the baseline of the TIC peak of interest. For the first run, set
Noise Threshold to zero to show all peaks, and choose OK.
If the noise level in the refined spectrum is unacceptable, repeat the Refine operation
with a higher Noise threshold setting. Values in the 0-10 range are recommended.
OR
•
Refine the current spectrum using the current Refine parameters by
choosing
522
from the Library toolbar.
Library
Auto Refine
To automatically use the refine parameters in all searches, select Auto
Refine from the library Process menu. A check mark appears next to the
item if it is selected. To turn this option off select it from the menu again. It
is especially useful with automatic library searching from Chromatogram.
Using the Library Compare Process
The Compare process allows you to compare the search spectrum to a particular
library entry. This can be useful if you have an idea of what the compound is or
what type of compound it is, particularly if the compound in question does not
appear in the top 20 hit list.
Comparing the search spectrum to a library entry
1. Select Compare from the Library Process menu.
2. Enter the number of the entry to which you want to compare the search
spectrum. You can access a different library by clicking File, and click OK.
TurboMass updates the Library display to show the results of the comparison in
the Hit List, Hits, Delta, and Structure windows, if these windows are currently
displayed. The format of the display is the same as for a normal search except,
of course, there is only one hit.
Using the Library Subtract Process
The Subtract process allows you to subtract the spectrum of a particular hit from the
search spectrum. The resulting subtracted spectrum becomes the new search
spectrum, and the library search can be repeated.
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The Library Subtract process can be useful if you suspect that the search spectrum is
a mixture of more than one compound. A mixture is indicated by a high Reverse Fit
and low Forward Fit value. If you subtract the spectrum of one of the hits from the
search spectrum and repeat the library search, the other component of the mixture
now appears high on the Hit List. For mixtures that contain more than two
compounds, this process can be used to identify compounds one at a time.
Subtracting a hit from the search spectrum
Select Subtract Hit from the Library Process menu, enter the number of the hit
you want to subtract, and click OK.
The subtracted spectrum becomes the new search spectrum.
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Library
Creating User Libraries
In addition to the libraries available from PerkinElmer, you can create your own
"user" libraries that contain your own spectra. These spectra can come from raw data
files or from existing libraries.
Creating a User Library
The steps involved in setting up a user library are as follows:
•
Run the Spectrum application, and select the first spectrum that you want to add
(append) to your library.
•
Select Library Append from the Spectrum Edit menu.
•
Click File and enter the name for the new library. Click OK. When prompted,
click Yes to create the new library. Click OK to add the first spectrum.
•
Using the TurboMass Spectrum application, select spectra one at a time to put
into your library.
•
For each selected spectrum, use the Library Append command from the
Spectrum Edit menu to add to your library.
•
In the Library application, select Edit Library, and set up the text data for each
entry.
•
Use the Index Library command from the Library Process menu to create the
Presearch file for the new user library.
Once you have created a user library, you can add new spectra to it at any time by
repeating these steps.
Creating a new user library
1. Open the Spectrum application.
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2. Display the first spectrum you want to append to the library by doing one of the
following:
To add spectra to an existing user library, display the spectrum you want to
append to the library.
OR
To add spectra from a different library to an existing user library, display the
library entry that you want to append to the new user library by selecting
Library Get Spectrum from the Spectrum Edit menu, enter the number of the
library entry you want to display, and click OK.
3. Select Library Append from the Spectrum Edit menu.
The Append Spectrum dialog is displayed.
4. If the current library is the one you want, click OK. If not, click File to display
the Append File Select dialog, enter or select the desired library file, and click
OK to add the first spectrum into the new user library.
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Library
5. Enter a new file name for the user library, and click Open.
6. Click OK to add the first spectrum into the new user library.
Adding Text Data to the Library Entries
Once you have appended a spectrum to a user library, you need to edit it to add text
data such as Compound Name, Text, CAS Number, Formula, and Molecular
Weight.
You can also add two numerical User Values and User Flags for the entry. These
can be used to hold information about the compound. These fields can then be used
as library search filters.
Entering text data for a user library entry
1. Select Library from the Library Edit menu to display the Edit dialog.
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2. Select the entry that contains the data you want to enter or modify, and then
enter the data.
Name
The compound name for the entry up to a maximum of 128
characters.
CAS
The Chemical Abstracts Sequence (CAS) number for the
compound. The CAS number is used to link library entries to their
chemical structures in the Structures Library for display in the
Structures window. The CAS number has the format "x-yy-z",
where:
x is a string of numbers; for example, 12398 or 6;
yy is a two-digit number string; for example, 23 or 07;
z is a one-digit number string; for example, 7 or 0.
Formula
The elemental formula for the compound.
Elemental formulas are entered in “standard” format as an
element symbol, followed immediately by its count if greater than
one, and then immediately by another symbol, as relevant.
For example, consider Formula set to "C6H20NClBr2". Enter in
the standard upper and lower case format. Note that, "Cl" does not
need a "1" after it and that there are no spaces. The specific order
of elements is irrelevant. Formula and Mol Wt are compared
within an entry and you are warned if there is a discrepancy.
528
Library
Mol Wt
The molecular weight of the compound that is entered as an
integer, based on nominal masses for elements. For example, H is
1 and Cl is 35. Formula and Mol Wt are compared within an
entry, and you are warned if there is a discrepancy.
Text
Any text to a maximum of 30 characters.
Value
Any positive or negative, integer (no decimal point) or decimal
point value. These values can be used when setting filters for
library searches or in the Process Locate dialog.
Flags
A string of one or more characters representing user-specific
information. You can enter any characters you like, including
spaces to a maximum of eight characters. The order and case of
the characters are significant.
These values can be used when setting Filters for library searches,
in the Process Locate dialog or when selecting the Flagged
Entries parameter in the Edit Library dialog.
3. Repeat step 2 as necessary.
Each time you select a new entry you are prompted to save the changes you
have made.
4. Click Close, and click Yes to save changes.
Indexing a User Library
Before you can use a new or newly appended user library for searching, you must
index the library to create a Presearch file for it. The Presearch file contains each
library spectrum reduced to its eight most intense mass-weighted peaks.
Indexing a library requires a lot of processing and may take considerable time,
depending on the size of the library. The Library Reindex dialog displays an
estimate of the time required to index the library. Each time you add new entries to
the library, you need to re-index it before you use it for searching.
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Indexing a user library
1. Select Index Library from the Library Process menu.
The Library Reindex dialog is displayed.
2. Click Start to begin the indexing process.
A display keeps you updated on the indexing progress and gives you an
indication of the remaining time required. When indexing starts, the Start button
changes to the Stop button. You can cancel indexing at any time by clicking
Stop.
3. When the indexing is complete, click Close.
Deleting Library Entries
You can only edit the text associated with a library entry; you cannot edit the
spectrum itself. If you want to change the spectrum associated with a library entry,
you must delete the entry and then create a new entry by appending the correct
spectrum to the library.
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Library
Deleting a user library entry
1. Select Library from the Library Edit menu to open the Edit dialog.
2. Select the entry to be deleted.
3. Click Delete Entry and confirm the deletion.
4. To view deleted entries, select View to open the View dialog .
You see the text DELETED above the top left of the spectrum, and all input
fields are unavailable. Restore Entry has replaced Delete Entry and can be
used to restore this entry. At this point, the entry has been Flagged as deleted
but has not yet been physically removed from the library file.
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Using the Library Locator
The Library Locator can be used to look through a library. Filters can be set up and
searches performed to select certain classes of compounds.
Locating one or more library entries
1. Select Locate from the Library Process menu.
The Locator dialog is displayed.
The Library Locator dialog contains the following information about a library
entry: Library Name, Entry No., Compound Name, CAS Number, Formula,
Molecular Weight (Mol Wt), Spectrum and Structure. User Libraries may also
contain Values 1 and 2, and User Flags.
The Locator dialog can be used in two different ways: to select a particular entry
for examination, or to set filter parameters that control the entries displayed by
the Locate process.
2. Search the library:
Manually: Use the scroll arrows to page through the library entries one at a
time, or click Select, enter the desired Entry No. and click Update.
OR
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Library
Using filters: Click Filters from the Locate dialog to set the match (locate)
criteria, and click OK to confirm the criteria.
A message notifies you which filters are to be used for the Locate process.
TurboMass searches the library and displays the first entry that satisfies the
locate criteria.
3. Click Fwd>> or <<Rev to find the next entry matching the locate criteria. Both
operations start at the current entry and search in ascending (Fwd) or descending
(Rev) entry-number order.
4. A message appears indicating the progress of the location. When the next
suitable entry is found, TurboMass updates the display.
5. Repeat step 2 as required.
6. To stop the Locate process before it is finished, click Cancel.
7. When you have finished your search, click Close to return to the Library Hits
window.
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534
Map
17
Map
Overview
The Map application provides a three-dimensional representation of an entire data
file.
Figure 11 Map display of gasoline data file
The vertical axis displays mass/charge units (m/z) and the horizontal axis displays
retention time in minutes. The third dimension is the intensity of a particular mass at
a particular retention time, which is represented by a user selected color scheme.
The current cursor position is given by a pair of cross hairs. The mass chromatogram
for the currently selected mass is displayed at the top of the Map window. The
spectrum at the currently selected retention time is shown at the bottom of the Map
window.
The Map program provides the ability to overview a complete data file very quickly.
This is particularly useful for complicated GC/MS data files. The data file can be
rapidly searched for particular masses, with the simultaneous display of mass
chromatograms and spectra.
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How to create a data file map
1. Select Map from the TurboMass top level Process menu
OR
.
Click
The first time the Map program is loaded the Map window will initially be
blank.
2. Click
OR
Select Open from the Map File menu, or select Create Map from the Map
Process menu.
The Create Datafile Map dialog is displayed.
3. If you wish to change the data file select File to open the Map Data Browser
dialog.
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Map
4. Select the new data file from the File Name list.
You can access a data file on a different drive or directory.
5. Click OK to exit the Map Data Browser dialog.
6. Alter values as required in the Create Datafile Map dialog and click OK.
A status bar at the bottom of the map window will keep you informed of the
progress of the Map process.
Stopping the Map process before it has been completed
Click
OR
Select Stop Process from the Map Process menu.
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About the Map Display
The Map display has three parts. The top trace shows a mass chromatogram of the
currently selected mass. The lower trace shows the spectrum for the currently
selected retention time.
The middle trace shows the map display of mass against retention time for the data
file. Each block of color represents the intensity of a particular mass at a particular
retention time. You can select a mapping mode and color scheme for the map
display using the Display Scale options.
The currently selected mass and retention time can be changed by moving the crosshairs cursor over the display. Moving the cursor in the vertical direction changes the
current mass. Moving the cursor in the horizontal direction changes the current
retention time. The current cursor position is shown on the right side of the status
bar at the bottom of the display.
Double-clicking on the mass chromatogram will open the Chromatogram window
with that mass chromatogram displayed. Double-clicking on the spectrum will open
the Spectrum window showing that spectrum.
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Map
The Map Toolbar
The Map toolbar at the top of the Map window allows you to perform some
commonly used actions by clicking a button.
Selects a data file.
Prints current window in portrait format.
Prints current window in landscape format.
Sends bitmap of current window to the Clipboard.
Stops the current map process.
Edits intensity scaling for map display.
Toggles to restore the previous display range or to display the default display
range.
You can toggle the toolbar display on/off by selecting Toolbar from the Map
Display menu. When the toolbar display is selected, a check mark will appear next
to it in the Display menu.
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Selecting a Range to Map from the Data File
By default the Map program will create a map for the whole file, covering the full
range of retention time and mass.
Reducing the mass and retention time ranges will require less memory and the map
process will take less time. You may find this useful for large data files.
It is also possible to reduce the resolution used for the mass and retention time axes.
Reducing the resolution will reduce memory requirements and may also enhance
features in the data.
The Map program will sum all masses in a window equal to the mass resolution to
create the map display. For example, if the mass range is set to 50 amu to 350 amu,
and the mass resolution is set to 1 amu, a point will be plotted at 100 amu that is a
sum of all masses between 99.5 and 100.5 amu.
The Map program will sum all scans in a window equal to the scan resolution to
create the map display. Summing scans in the data file can also improve the signal
to noise ratio, this will help to make peaks more visible and reduce the displayed
noise.
Mapping part of the data file of interest
1. Select Create Map from the Map Process menu.
The Create Datafile Map dialog is displayed.
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Map
2. Enter values for the Mass Range and Retention Time range that you wish to
map.
3. Click OK.
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Manipulating the Display
You can alter the display, retention time, and mass axis ranges using the mouse or
by using a menu command. The Map Display menu contains commands for
changing the range of the mass axis and restoring the default display.
Altering the display range with the mouse
Mass and retention time axes may both be expanded by clicking with the mouse
on the spectrum. The previous state of the display can be restored by clicking
.
Altering the range of the retention time axis
Left-click at one end of the region of interest and drag the mouse horizontally to
the other end. As you drag the mouse, TurboMass will indicate the range you
have selected. Do not go beyond the bounds of the axis. When the mouse is
released, the selected range will be redisplayed.
This operation can be repeated as often as required.
Altering the range of the mass axis
Left-click at one end of the region of interest and drag the mouse vertically to
the other end. As you drag the mouse, TurboMass will indicate the range you
have selected. Do not go beyond the bounds of the axis. When the mouse is
released, the selected range will be redisplayed.
This operation can be repeated as often as required.
Altering the range of both axes
Left-click at one end of the region of interest and drag the mouse diagonally to
the opposite. As you drag the mouse, TurboMass will indicate the range you
have selected. Do not go beyond the bounds of the axis. When the mouse is
released, the selected range will be redisplayed.
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Map
This operation can be repeated as often as required.
Restoring the display
toggles from restoring the display to its previous state to displaying
Clicking
the default range.
Altering the range of the mass axis from the Map menu
1.
Select Range from the Map Display menu.
2. Enter new Start and End values for the mass and time axes as required.
3. Click OK.
Restoring the display to the default range
Select Default from the Map Display menu.
Changing the Map Intensity Scaling
To enhance features within the data file it may be necessary to experiment with the
map intensity scaling.
Each mass intensity is compared to the most intense mass in the data file range that
is being mapped. Each mass is then mapped according to its comparative intensity to
the corresponding color.
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The value of Start (%) corresponds to the % intensity at which the color mapping
starts, and the value of End (%) corresponds to the % intensity at which the color
mapping ends. In the example, all masses with intensities less than 20 % on a
logarithmic scale of the most intense mass would be shown in the first user color.
All masses with intensities greater than 80 % on a logarithmic scale of the most
intense mass would be shown in the last user color. All masses with intermediate
intensities would be mapped to the other user colors.
Changing the map intensity scaling
1.
Click
OR
Select Scale from the Map Display menu.
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2.
Set the Intensity Mapping Mode.
The options available are Linear, Square Root and Log. The log and square
root intensity modes will give more weighting to lower intensity masses.
3.
Set the Color Palette.
The options available are White On Black, Black On White, Gray Scale, User or
one of the Map color schemes. The Map color schemes available are Ocean
Deep, Embers, Emerald Forest, Hot Metal, Cool Metal, Morning Frost, Polar
Dawn and Tropical Lagoon.
Map
4. Define the User colors.
The User colors are defined by selecting Fonts and Colors from the
TurboMass top level Customize menu, and selecting the colors for Data 6 to 10.
5. Set the Map Intensity Range values, and click OK to create the map.
Changing user color scheme for Map display
1.
Select Fonts and Colors from the Customize menu to open the Color and
Font Editor dialog.
2.
Select Data 6 to 10 in Type and change the colors as required.
3.
Click OK to update the Map display with the new colors.
Controlling the Appearance of the Display
The appearance of the Map display is controlled from the Map View dialog.
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Changing the appearance of the Map display
548
1.
Select View from the Map Display menu to open the Map View dialog.
2.
Select the appropriate Map View parameters.
TIC chromatogram
If selected, the TIC chromatogram of the current
data file is displayed at the top of the Map window.
Deselect this checkbox to remove the TIC
chromatogram.
BPI Chromatogram
If selected, the BPI chromatogram of the current
data file is displayed at the top of the Map window.
Deselect this checkbox to remove the BPI
chromatogram.
Current mass
chromatogram
If selected, the mass chromatogram of the currently
selected mass is displayed at the top of the Map
window. Deselect this checkbox to remove the
mass chromatogram. All chromatograms displayed
are overlaid on the same axes.
Current Spectrum
If selected, the spectrum at the currently selected
retention time is displayed at the bottom of the Map
window. Deselect to remove the spectrum.
Map
3.
Cross-hairs
This drop-down list controls the color used to
display the cross-hairs cursor: Inverse, Black,
White or Axis color. The cross-hairs cursor can be
moved to change the currently selected mass and
retention time.
Map, Spectrum, and
Chromatogram Grid
Apply a grid to each part of the display. The grid
pattern can be set to Off, Dot, Dash or Solid for
each part of the display.
Automatic Link to
Spectrum
If selected, the Spectrum window will be updated to
show the current spectrum as the cross-hairs cursor
is moved across the map display. Deselect to
remove the link between Map and Spectrum.
Automatic Link to
Chromatogram
If selected, the Chromatogram window will be
updated to show the mass chromatogram of the
currently selected mass as the cross-hairs cursor is
moved across the map display. Deselect to remove
the link between Map and Chromatogram.
Click OK.
Displaying the Chromatogram and Spectrum windows
•
Double-click the mass chromatogram to display that mass chromatogram in the
Chromatogram window.
•
Double-click the spectrum to display that spectrum in the Spectrum window.
Displaying the Status Bar and Toolbar
The status bar at the bottom of the Map window displays:
•
The current cursor position in terms of mass and retention time.
•
The status of an ongoing process such as the Create Map process.
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•
The function of the currently selected menu item or toolbar button.
Displaying the status bar and toolbar
Toggle the status bar or toolbar display on/off by selecting Status Bar or Toolbar
from the Map Display menu, respectively.
Selecting the Current Cursor Position
You can select the cursor position using the mouse or from the menu.
Changing the current cursor position
Double-click the required position on the Map display.
This position will become the current cursor position. The Spectrum and
Chromatogram displays will be updated accordingly.
If the cross-hairs cursor is displayed, you can change the current cursor position
by left-clicking anywhere on the cross-hairs and dragging them to the new
position.
OR
Choose Select Mass or Select Time from the Map Display menu, enter the
new value, and click OK.
Editing the Header Information
The Map Window has a customizable header. Various pieces of information such as
raw data file name can be displayed here, as well as any user text. For more detailed
information about the Header Editor, see The Header Editor on page 54.
Changing the displayed header
Select Header from the Map Display menu, make the required changes, and
click OK.
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Map
Printing from Map
To print the Map window:
1.
Select Print from the Map File menu.
2.
Make any changes required to the print parameters.
3.
Click OK.
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Copying to the Windows Clipboard
The Windows Clipboard provides temporary storage for information that is being
transferred between application programs (for example, word processors,
spreadsheets, TurboMass). You can copy a bitmap of the Map window to the
Clipboard and then, for example, paste the bitmap into a report written with a
Windows compatible word processor.
Copying the Map display to the Clipboard
1.
Produce the required display in the Map window.
2.
Click
OR
Select Copy Bitmap from the Map Edit menu to copy the contents of the
window to the Clipboard.
3.
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To read the image into another application, select Paste from the other
application's Edit menu.
Molecular Mass
Calculator
18
Molecular Mass Calculator
Calculating the Molecular Mass
The mass calculator can calculate two different molecular masses for a given
chemical formula.
•
Monoisotopic mass: Calculates the mass using the atomic weight of the
most abundant isotope of each element.
•
Average mass: Calculates the mass using the average atomic weight of
each element taking into account the relative abundance of its isotopes.
Calculating the molecular mass for a given chemical formula
1. Select MW Calculator from the TurboMass Tools menu or click
the Molecular Mass Calculator dialog.
, to open
2. Enter the chemical formula using standard International Union of Pure and
Applied Chemistry (IUPAC) notation.
3. To specify user defined elements or isotopes, follow the procedure Defining
User Elements on page 556.
4. Select either Monoisotopic or Average Mass.
NOTE: Monoisotopic mass is the usual choice for GC/MS.
5.
To display the calculated mass in the Mass field, click Calculate.
6.
To edit the current formula and recalculate the mass, click Calculate.
7.
To clear the current formula, click Reset.
8.
To copy selected formulas or calculated masses to the Windows clipboard,
click Copy.
The Copy function is convenient for pasting ion masses into the SIR scan
function.
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Defining User Elements
You can define a user element by specifying its name, symbol, average, and
monoisotopic masses.
1. In the Molecular Mass Calculator dialog, click User elements to display the
User-definable elements dialog.
2.
556
Enter the parameters and click Add to add the group to the list.
You can add up to 10 elements, isotopes, or molecules to the list.
3.
To edit a particular element or group, click Update.
4.
To remove a selected group, click Delete.
5.
Click OK to save the list and return to the Molecular Mass Calculator dialog.
6.
Click Close to exit the Molecular Mass Calculator.
Report Method
Editor
19
Report Method Editor
About the Report Method Editor
The Report Method Editor is an extension to the TurboMass software. It enables
you to specify a collection of report definitions (Communiqué report templates and
related parameters) that are printed sequentially. The Report Method is a dataset that
you can specify in each row of the Sample List. It defines the reports to be
generated following the analysis data or at the end of the Sample List. The Report
Method will consist of a list of report templates and associated parameters, namely:
1. When the report will be generated (for all runs, for runs of a specific type,
for only the last run in the sample list)
2. The output destination(s) of the report (print, save to database, save to file,
send via email)
3. The printer (if printed) and/or the file name (if saved)
4. The email address(es) and message text (if emailed).
5. Sections of the report template to be printed or suppressed
NOTE: Only a single report method can be loaded in the Editor at a time and only a single
instance of the Report Method Editor can be run. If you edit a Report Method while
the Editor is already open (e.g. by choosing the Open command from the context
menu when the Report Method cell is selected in the sample table) then the new
report method will replace the existing one, provided it is not in a modified state. If
the current method is in a modified state the ‘Do you want to save the changes to
“<report method name>”?’ warning dialog will be displayed.
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You open the Report Method Editor in one of two ways:
1. By choosing Open from the context menu when the Report Method cell is
selected in the Sample List. If no method name is specified in the cell, or if
there is currently no report method of that name in the Project directory,
then the Report Method Editor will open in the ‘New Method’ state. If the
cell contains the name of an existing report method then Report Method
Editor will open in the ‘Edit Method’ state.
2. By choosing the Report Method Editor command from the TurboMass
Tools menu. The default method will be the method most recently used. If
there is currently no report method of that name in the project directory (that
is the METHDB subdirectory in the project hierarchy), then the Report
Method Editor will open in the ‘New Method’ state.
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Report Method Editor
Report Method Editor Toolbar
The toolbar displayed at the top of the window lets you perform some common
operations with a single click of the appropriate toolbar button. The default toolbar
contains the buttons listed below. You can also customize the toolbar and add
additional buttons for other operations.
File New
File Open
File Save
File Save As
File Print
File Exit
Help Contents
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Selecting an Existing Template
1. Select Report Method Editor from the Tools menu.
The Report Method Editor screen appears:
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Report Method Editor
2. Click the Browse button to the right of the Template field. The Report
Template Browser appears:
3. Select a Template name and click OK (for example, click Qualitative Report).
This now appears in the Report Method Editor dialog:
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4. Select the Frequency of reporting. The options available are:
•
Generate report for every run
•
Generate report for every run of specified type
Selecting this option enables a second drop-down list. Here you select the
type of run from the available options.
•
Generate report only for final row in the sample list
5. Select a desired Output type.
6. Click the Append button to add this template to the current method.
This template appears in the Report (#/Template) field This is a display of the
reports defined for the current method.
When the list is empty (New Method, after Clear List or after all reports have
been Deleted) the controls on the right will be set to default values. In this way
the Append button is always enabled and valid.
Using the Move Up and Move Down command buttons reorders the Reports in
the list. Reports will be processed by report number (i.e. in the order in the
list).
7. Select Save As from the Report Method Editor File menu.
The Save Report Method As dialog appears:
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Report Method Editor
8. Type a File name for your Report Method (for example, Qualitative Report)
then click Save.
This Report Method is now available for the Report Method column of the
Sample List.
9. Double-click in the Report Method field and select Qualitative Method from the
drop-down list.
10. Close the Report Method Editor by clicking the Close box (in the upper-right
hand corner of the screen).
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Report Template Browser
In the Report Method Editor dialog click the Browse button to the right of the
Template field. The Report Template Browser appears:
To locate a template in a large list:
Browse through the tree view on the left of the window to find your project
folder.
or
1. Click the Define Template Filter button on the toolbar.
2. Set up the desired filter conditions in the Filter Templates dialog.
3. Apply the defined filter settings.
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Filtering the Template List
The list of templates may become very large, thereby a filtering mechanism
helps you locate the template of interest. The filter may be defined by accessing
the report template filter dialog, using the toolbar button.
The setting of the apply template filter button determines whether or not the
filter is active. This button can be in the ‘up’ or ‘down’ position. When the
button is down the filter will be active and the list view will display only the
templates matching the filter conditions.
Report Template Filter Toolbar
The toolbar displayed at the top of the Report Template Filter window contains
the tool buttons listed below. The tool button functions are duplicated in the
Report Template Filter menus.
Displays the Template Filter dialog box.
Toggles the defined filter for the template list on and off.
The filter will be active when the button is in the ‘down’
position.
Displays the Help window.
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Communiqué
Reporting
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Communiqué Reporting
About the Report Method Editor
In this section we will show you how to use the Report Method Editor and
Communiqué to modify an existing report template and create a new report
template.
A vital aspect to the flexible reporting capabilities of the TurboMass software will
be the data model. This defines the data that will be made available to Communiqué
for design of the template and generation of the report. Most TurboMass data is
available through the data model. This includes:
1. All existing quantitative data generated by the TurboMass Quantification
process (including Area% and Norm% values).
2. The chromatograms and spectra defined by the Qualitative method and its
processing.
3. Values associated with the multiple ion ratio identification process (ratios,
pass/fail, etc.)
4. Peak plots associated with multiple ion ratio processing (for target
compounds and internal standards).
5. Calibration curve plots associated with target compounds.
6. Library search spectral plot data and text results.
7. Quantification and Qualitative method parameters.
TurboMass creates a collection of Data Objects that appear in the Communiqué
Report Creator.
In the Communiqué Report Creator, note that collections (in the Communiqué
sense of the word) are indicated by parentheses ‘()’ following the collection name
for example Samples().
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Opening a Report Template
To open an existing report template, follow this procedure:
1. Select Report Method Editor from the Tools menu.
2. The Report Method Editor screen appears:
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3. Click the Browse button to the right of the Template field. The Report
Template Browser appears:
4. Select a template name and click OK (For example, click Qualitative Report).
This now appears in the Report Method Editor dialog:
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5. Click the Edit button.
This launches the Communiqué Report Creator.
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Communiqué Reporting
Modifying the Template
To modify the template, follow this procedure:
1. Add a graphic by clicking Graphic in the Layout Tools toolbox.
A dialog similar to the following appears:
2. Browse to the directory where the graphic is stored and select it by clicking on
it.
3. Move your cursor to the design page and click. The cursor changes to the
following cursor:
4. Move your cursor to a desired spot on the page. Click the left mouse button,
drag the mouse to scale the graphic to a desired size, then release the mouse
button.
The graphic appears on the page.
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Adding a Data Object to the Template
To add a data object to the template, follow this procedure:
1. Click on Data Objects to display the available data objects.
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Communiqué Reporting
2. Move the table (see above) and then the Chromatogram Plot down the page to
make room at the top of the Chromatogram Plot.
•
To move the table and Chromatogram Plot, move your cursor over the table.
•
It turns into
Now hold the left mouse button down and move
.
your mouse to move the table.
•
Next move the Chromatogram Plot the same way.
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3. Click on Project Name, move your cursor to the designer page, the click where
you want the Project Name to appear and drag it to the desired size.
4. Click on Layout Tools to display the Layout Tool selections, click on Text
Block, move your cursor to a position on the designer page, click and drag to
put the text block on the page. Position the cursor on an edge of the Text Block
and hold the left mouse button down and drag the edge to the proper size.
5. Click in the Text Block and type (for example, Project Name).
6. Highlight the text and right click to display the text formatting options.
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7. Click Save As from the File menu, name and save your file.
8. Exit the Report Designer.
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Creating a New Report Template
To create a new report template:
1. Select Report Method Editor from the Tools menu.
2. The Report Method Editor screen appears:
3. Click the New button to the right of the Template field. The Communiqué
Report Creator appears:
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Communiqué Reporting
Add a Header and Footer
1. Click on Header in the Layout toolbox on the left of your screen.
The Header appears.
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If you click on New Template the template description page will be displayed.
Here you can allow for A4/Letter resizing of your template. To properly use
the non-A4 templates as the only set, the Allow A4/Letter page resizing
option in each template's description page should be selected and in all cases
the Paper drop-down list on the template description page should always be set
to Letter so that the page size appears properly in the template editor.
2. Drag a Text Block into the Header. Label it “Qualitative Report Test1.” Then
format the text as follows:
a. Highlight text and right-click to select Format.
b. Select Font tab.
c. Set to Blue, 20 pt. Ariel, Bold.
d. Set Paragraph tab, alignment Horizontal / Center.
e. Click OK.
f.
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Communiqué Reporting
3. Click on Footer in the Layout toolbox on the left of your screen. The footer
appears.
4. From the Data Objects toolbox, left click DateTimeReport.
5. Click in the footer, then size Date Time Report into the Footer to full width.
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6. Click on Page Type 1 in the Layout toolbox on the left of the screen. This will
display the main body of the template.
Add Data Objects
NOTE: The Communiqué user interface supports click and drop rather than drag and drop.
Simply left click on the object in the Data Objects tree and release the mouse button.
Next, position the mouse pointer in the template, click and drag the pointer, then
release. Use this same functionality for placing any object onto a template.
NOTE: To ensure that a CSV file puts data items on the same line, enclose all items that are
required to appear on one line of the CSV file in a Communiqué Section object. All
items enclosed in the Section should have the 'Down from Top' property set to zero
(0). Also, all items should have the same 'Height' value set as the Section
itself.
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1. Click on Chromatogram (Active X) in the Project > Samples() directory of the
Data Objects toolbox (Graphic Data Objects have a small red “x” as their icon.
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2. Left-click on Chromatogram (ActiveX), move the cursor to the center of the
design page, then left click and hold the mouse as you drag the mouse to expand
the box. The box displays as CHROMATOGRAM PLOT GRAPH HEADER.
3. From Layout Tools, left click on Table then move your cursor to the page and
left click. A four column by two row table appears.
4. Select the table. Right-click Format.
The Format Table dialog appears:
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5. Change the Number of columns from 4 to 5 then click OK. If necessary, click
on the Columns tab and change the Column width to 0.5.
6. Add text blocks to the top row of the table. Label each cell as follows; #, RT,
Name, Match Factor, and Area%.
NOTE: Remember to first put a Text Block (from the Layout Tools) in the table so that you
can enter a label.
7. Under “#” put Peak Number, from the Project / Samples() / Qualitative Peaks ()
path in the Data Objects toolbox.
If you move your cursor over Peak Number (DATA) the following appears:
This information Project.Samples(Current).QualPeaks(Current).PeakNumber is
the source string of the data. In this example, it will report the peak number of
the current QualPeak in the current Sample.
About Samples; Current versus Last: The template is used to pull
information from the data source during report creation. From the point of view
of the data source, the most recent data (e.g., the current line on the Sample
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List) is the last data entered into the data source. Therefore, to view data from
the current line of the Sample List, use Samples(Last).
To report the most recent line in the Sample List we need to change the
Indexing of the Peak Number. Right click on Peak Number (DATA) and select
Indexing from the menu.
The Data Object Indexing dialog appears:
Double click on Current in the Samples Index cell.
The following Index dropdown menu appears:
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Communiqué Reporting
Select Last then click OK.
8. Under “RT” put Retention Time, from the Project / Samples() / Qualitative
Peaks () path in the Data Objects toolbox. Set to Samples (Last).
9. Under “Name” put Name, from the Project / Samples() / Qualitative Peaks ()
path in the Data Objects toolbox. Set to Samples (Last).
10. Under “Match Factor” put Match Factor, from the Project / Samples() /
Qualitative Peaks () / Text Hits / path in the Data Objects toolbox. Set to
Samples (Last).
11. Under “Area%” put Area%, from the Project / Samples() / Qualitative Peaks () /
path in the Data Objects toolbox. Set to Samples (Last).
12. Check your Date/Time Data Object Properties for the correct Time Format.
The default Communiqué setting for Date/Time Data Objects is "Local time."
In order to ensure that the correct time is reported on your computer, right-click
the Date/Time Object in your template, select Object Properties from the popup menu and in the following dialog select "Original time" to set the Time
Format, then click OK.
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NOTE: When setting the Numeric Data Object Properties in your Communiqué template,
increase the number of significant figures from the default of 4 to 6 in order to see
the reported number with no rounding applied. Otherwise Communiqué does not
report 6 figures but instead applies rounding.
13. Select Save from the Communiqué Report Creator File menu and name the file
(for example, Mod Qualitative Report).
14. Close Communiqué Report Creator by clicking Exit from the File menu.
Select the Template in the Report Method Editor
After closing the Communiqué Report Creator the Report Method Editor
appears:
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1. Click the Browse button.
The following dialog appears:
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2. Select your template (for example, Qualitative Report) and click OK.
Qualitative Report appears as shown below:
3. Click the Append button.
This template appears in the Report (#/Template) field. This is a display of
the reports defined for the current method.
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When the list is empty (New Method, after Clear List or after all reports have
been Deleted) the controls on the right will be set to default values. In this way
the Append button is always enabled and valid.
Using the Move Up and Move Down command buttons reorders the Reports in
the list. Reports will be processed by report number (i.e. in the order in the
list).
4. Set the other options on this screen. For example, set the Frequency to one of
the following:
5. Generate report for every run.
6. Generate report for every run of specified type. (Analyte, Blank, QC, or
Standard)
7. Generate report only for final row in the sample list.
8. Set the Output options and specify a Report name prefix if it is required by the
Output type selected. (For example, if you select Save to file, select a Report
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name prefix of <Sample Name>, and click the Setup button. This drop–down
list contains the report output file types supported by Communiqué:
NOTE: To ensure that a CSV file puts data items on the same line, enclose all items that are
required to appear on one line of the CSV file in a Communiqué Section object. All
items enclosed in the Section should have the 'Down from Top' property set to zero
(0). Also, all items should have the same 'Height' value set as the Section itself.
•
•
•
•
•
•
Rich Text Format (.RTF)
HTML (.HTM)
ASCII Text (.TXT)
Comma separated (.CSV)
Portable Data Format (.PDF)
Web Archive, Single File (.MHT)
NOTE: The Web Archive, Single File type embeds the graphics into the same .htm as the
text portion of the report resulting in a single file with both text and graphics.
The following dialog appears:
9. Click OK.
10. Select Save As from the Report Method Editor File menu.
11. The Save Report Method As dialog appears:
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12. Type a File name for your Report Method (for example, Qualitative Report)
then click Save.
This Report Method is now available for the Report Method column of the
Sample List.
Add the Report Method to the Sample List
1. Double-click in the Report Method field and select Qualitative Method from
the drop-down list.
2. Close the Report Method Editor by clicking the Close box (in the upper-right
hand corner of the screen).
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Environmental
Reporting
21
Environmental Reporting
About Environmental Reporting
TurboMass Environmental Reporting software generates reports based on lists of
PerkinElmer TurboMass and Clarus GC/MS samples (Sample List). These reports,
while based on U.S. Environmental Protection Agency (US EPA) requirements, are
designed to be flexible and customizable to support worldwide environmental and
QA/QC reporting requirements governed by NELAC and ISO 17025.
You can add samples to the list or create new lists using either the Sample List or
Sample List Wizard. While the Sample List is typically created prior to data
acquisition, it can be created and edited any time prior to environmental report
generation.
In the Report Generation window you can select the Forms you want printed and the
data set to be used as input. Also, the selection of Tentatively Identified Compounds
(TIC) from the initial library search qualitative processing is made within this
environment.
IMPORTANT: If you change the quantitative results at the report generation time (for
example, you select a different method) you must reprocess, otherwise the
qualifier flag assignments may be invalid.
Report generation is a daily operation within the environmental laboratory and
TurboMass Environmental Reporting is designed to streamline the process.
TurboMass Environmental Reporting supports:
•
Efficient environmental report generation based upon environmental
QA/QC sample batches
•
A powerful interactive data review environment
•
Custom per-client and per-project compound lists
• Automatically report only client-requested compounds
• Does not need a new Quantify method and Calibration curve
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• Do not need to manually delete target compounds for TIC searching
and reporting
600
•
Intelligent errors and warnings report of missing information during file
selection
•
Intelligent default selection of files for QA/QC reports
•
Optional reporting of “J” flagged-compounds
•
Easy review and selection of TIC compound name results
•
Easy to customize reports without programming
Environmental Reporting
Select Forms Dialog
The Select Forms dialog provides you with the interface to select reports to be
printed. These reports are based upon templates, or “Forms” defined by the US
EPA.
The exact format of the report you generate depends upon several selections you
make within the Sample List or Sample List Wizard environments. These include
the following:
Sample Type
Volatiles (VOA), Semivolatiles (SV), or QA/QC
Matrix
Water or Soil
Concentration (SV only)
PerkinElmer provides two sets of reports, one based on the US EPA OLM04.2
specification (“CLP-Like), and the other (the default) a format enhanced with
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additional laboratory information and with a more attractive and convenient format
(PKI format).
The reports may optionally be defined by a configuration table set up by the
TurboMass administrator. This table maps the specified report to a Communiqué
reporting template. The table applies to the current TurboMass Project and the
configuration file is copied to a new Project as part of the New Project Wizard
functionality.
In TurboMass terms, the Forms are a combination of single run reports and
summary reports. Additional information is in the section Report Method Usage on
page 650. The Environmental Reporting environment automatically generates one or
more temporary Sample Lists based upon the needs of each report, and adds them to
the Communiqué report generation queue.
The normal Communiqué report generation procedures can be used to produce most
of the non-summary Forms automatically after data acquisition. Non-environmental
Communiqué reports (e.g. chromatogram plots, library search results, quantitation
plots) can also be produced in the same manner.
The selections in the Select Forms dialog are described below:
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Parameter
Description
Sample list
The name of the sample list to be processed. You type it
in or select it from the current project (only) using the
Browse button.
Browse...
A button, when clicked, displays a standard File Open
dialog (with the Title ‘Select Sample List’), allowing you
to select a stored sample list (*.SPL file).
Form 1 - Organics
Analysis Data Sheet
Selecting this check box indicates that Form 1 report is to
be generated for each applicable sample in the sample
list. Form 1 reports the concentrations of target
compounds in the sample.
Environmental Reporting
Form 1 - Tentatively
Identified
Compounds
Selecting this check box indicates that Form 1
Tentatively Identified Compound (TIC) report is to be
generated for each applicable sample in the sample list.
Form 1 TIC shows library search results for the largest
(typically 10 to 30) non-target peaks in the. Each is
assigned an estimated concentration based upon its
response compared to the Total Ion Current of the nearest
internal standard compound.
TurboMass qualitative processing prior to entering the
Select Reports window will initially generate a list of
several potential hits from the NIST library search. You
must choose one of these hits for each unidentified peak,
enter an alternative text (e.g., long-chain hydrocarbon),
or delete the TIC peak from the report. Until you have
performed this task the qualitative results will be marked
(in the qualitative data file) as Pending. The data file be
marked Complete only after you have reviewed the data
for each peak and accepted the default compound
identification, or selected a different one.
Form 2 SMC/Surrogate
Compound Recovery
Form 2 reports the recoveries of the specific analytes
defined as System Monitoring Compounds (SMC, also
called “surrogates”.) It flags any compound whose
recovery is outside of Quantify Method specified limits.
The sample to be used as the source of the header
information for the report is indicated by the data source
item ‘Header Sample Index’. This defaults to the first
checked (i.e., selected for processing) Analyte or Analyte
Dup row in the sample list but you may reassigned this.
Form 3 - Matrix
Spike/Matrix Spike
Duplicate Recovery
Form 3 reports the recoveries of specific analytes defined
as spike compounds in the sample; the matrix spike
(MS), and the matrix spike duplicate (MSD). It flags any
compound whose recovery or relative percent deviation
(RSD %) is outside of the Quantify Method defined
limits.
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Form 4 - Method
Blank Summary
Form 4 designates which samples were acquired
reporting to a particular method blank.
Form 5 - Instrument
Performance Check
Form 5 reports the compliance of the BFB or DFTPP
tune evaluation sample (instrument performance check),
and lists all data files acquired while this tune file was
valid.
Form 6 - Initial
Calibration Data
Form 6 reports the initial calibration of the instrument
based on a multi-level calibration. The average relative
response factor (RRF) and its relative standard deviation
(RSD) are reported for all RRF-calibrated target
compounds. It flags any compound whose response
factors or relative standard deviations are outside of the
Quantify Method defined limits. The r-squared
correlation coefficient is calculated for linearly calibrated
compounds, and the Form flags values outside of
Quantify Method defined limits.
You will identify a specific row in the sample list to be
used as the source of the Form 6 header data. This will
default to the first checked (i.e., selected for processing)
Analyte or Analyte Dup row identified as referencing the
calibration file to be used as the source of the Form 6
data.
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Form 7 - Continuing
Calibration Check
Form 7 compares the daily calibration check (continuing
calibration) data against the initial calibration data of the
instrument. Compounds whose relative response factors
or % differences exceed Quantify Method defined limits
are flagged. Linearly or quadratically calibrated
compounds are flagged if their % drifts exceed Method
limits.
Form 8 - Internal
Standard Area and
RT Summary
Form 8 reports the retention time and area reproducibility
for the internal standards for all data selected.
Environmental Reporting
Continue
This button opens the main environmental reports
generation window.
Cancel
This button closes the Generate Forms dialog.
NOTE: Whenever you select a new sample list and click Continue, the main environmental
reports generation window will open with the Sample List tab selected. If the sample
list is the same one you had previously been working with in the current session and
the Select Forms dialog was only used to change Forms selected then Continue will
return to the previously selected Form tab (unless this is no longer present, in which
case the Sample List tab will be selected).
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Report Generation Window
In this window you can select the Forms you want printed and the Sample List(s) to
be used as input. The selection of Tentatively Identified Compounds from the initial
qualitative processing will also be made within this window. This window displays a
comprehensive view for generating reports using the EPA Forms 1 through 8 that
apply to GC/MS analyses.
The process of generating the Forms will involve the reprocessing a Sample List by
the TurboMass software (as with other Communiqué reports) but there are several
unique aspects in this case:
1. The Sample List is queued for reprocessing from this window rather than
from the Sample List window.
2. The Start Sample List Run dialog does not appear. The reprocessing always
uses the following options:
Auto Quantify Samples = On (Quantify Samples only)
Generate Communiqué Reports = On
Quantify, Qualify, and Generate Reports = After Each Run (or summary
reports at the end of the sample list)
3. Which sample rows are processed will be indicated by the user on the
Sample List tab. Individual rows can be turned on or off for processing.
4. The Report Method supplied to the Report Manager (and hence the
template(s) provided to Communiqué will not be that in the Report Method
column of the Sample List but will instead depend on the Forms selected by
the user and the Submitter and Task associated with the sample. The Report
Method in the Sample List can be executed in the usual manner (Run/Start
from the Sample List).
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NOTE: During the sample list processing associated with report generation, processing
from within the Quantify window (View Results) will be inaccessible to a user. This
is to prevent possible data file conflicts.
Context Menu (Sample List Tab) - The following pop-up menu appears when you
right–click on the Sample List tab (i.e., the label area you click on to select the tab).
It allows you to quickly select and deselect Forms for printing.
Form tab - Remove This Form - Removes the tab associated with the clicked–on
label from the Report Generation Window. The associated Form will not be printed.
Report Generation Window Menu
The following reporting controls are available from the Report Generation Window.
Menu Item Command
Description
Sample List Append Sample List…
Opens a data browser, allowing the
selection of a sample list file from the
current Project only. The selected sample
list will be appended to the list already
displayed in the window. This command is
only enabled when the Sample List tab is
selected.
Save As…
Opens a Save As dialog, allowing you to
enter a file name within the current
Project.
Exit
Exits the Report Generation window.
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Menu Item Command
Forms
Print
Description
Queues the selected sample list rows for
reprocessing.
Opens the Tentatively Identified
Assign Tentatively
Identified Compounds... Compounds dialog. Enabled when the
Form 1 TIC tab is selected and no Form 1
TIC errors exist.
Assign Header Sample
Assigns the selected row as the source of
report header information for Form 2.
Displays Header in the Status column for
that row.
Assign Analyte
Assigns the selected row as the Analyte to
be treated as the sample which gets spiked
to produce the MS and MSD samples for
Form 3. Displays Analyte in the Status
column for that row and displays the row
in the Analyte color.
Assign Matrix Spike
Sample
Assign Matrix Spike
Duplicate
Enabled when the Form 3 tab is selected.
Assigns the selected row as the Matrix
Spike sample for Form 3. Displays Spike
in the Status column for that row and
displays the row in the Spike color.
Enabled when the Form 3 tab is selected.
Assigns the selected row as the Matrix
Spike Duplicate sample for Form 3.
Displays Spike Dup in the Status column
for that row and displays the row in the
Spike Dup color.
Enabled when the Form 3 tab is selected.
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Menu Item Command
Assign Method Blank
Description
Assigns the selected row as the Method
Blank sample for Form 4. Displays Meth
Blank in the Status column for that row
and displays the row in the primary data
color.
Enabled when the Form 4 tab is selected.
Assign Tune Evaluation Assigns the selected row as the Tune
Sample
Evaluation sample for Form 5. Displays
Tune Eval in the Status column for that
row and displays the row in the primary
data color.
Enabled when the Form 5 tab is selected.
NOTE: It is valid for the same row to be
identified as a Tune Eval for Form 5 and a
Cont Calib for Form 7.
Assign Continuing
Calibration
Assigns the selected row as the Continuing
Calibration sample for Form 7. Displays
Cont Calib in the Status column for that
row and displays the row in the primary
data color.
Enabled when the Form 7 tab is selected.
NOTE: It is valid for the same row to be
identified as a Tune Eval for Form 5 and a
Cont Calib for Form 7 [and Form 8].
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Menu Item Command
Assign Mid-Level
Standard
Description
Assigns the selected row as the Continuing
Calibration (Mid–Level Calibration)
sample for Form 8. Displays Cont Calib
in the Status column for that row and
displays the row in the primary data color.
Enabled when the Form 8 tab is selected.
NOTE: It is valid for the same row to be
identified as a Tune Eval for Form 5 and a
Cont Calib for Form 8 [and Form 7].
Select Forms…
Displays the Select Forms dialog. If you
select a new sample list within the Select
Forms dialog the existing sample list will
be replaced and any reassignments will be
lost.
Options
Customize Display...
Opens the Customize Field Display dialog
to enable you to select the columns to
appear in the sample list view (Both on
Sample List tab and Form–specific tabs).
When the dialog is closed the display is
updated. It is disabled when the Form 6 tab
is displayed (since there are no selectable
columns on the tab).
Help
Help Topics
Opens this TurboMass Report Generation
Help window.
Sample List Context Menu
The following pop-up menu appears when you right–click on the Sample List tab
itself (i.e., the area you click on to select the tab).
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NOTE: The symbol in front of an item indicates that this is an on/off toggle command.
The check mark appears in front of the Form when the function is active or selected.
This applies to all menus described in this document.
Menu Item
Form X
Where X is a Form number
1 through 8
Description
Toggles display of the Form X tab. If the change is from Off to
On, the error/warning checks for Form X will be performed. If
the change is from On to Off any errors/warnings for Form X
will be eliminated.
The following pop-up menu appears when you right–click on the Sample List view
pane.
Menu Item
Description
Select Forms…
Displays the Select Forms dialog, enabling you to change the
set of Forms to be generated.
De-select All Samples
Removes the checks from all boxes leaving no samples
selected.
Select All Samples
Add check marks to all boxes thereby selecting all samples.
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How to Generate a Report
To generate a set of environmental reports, follow this procedure:
IMPORTANT: If you change the quantitative results at the report generation time (for
example, you select a different method) you must reprocess, otherwise the
qualifier flag assignments may be invalid.
1. Choose the Environmental Reports… command from the Tools menu of the
Sample List window or press the icon on the Sample List icon bar.
2. Use the default sample list (the one displayed in the Sample List window) or
select a different one.
3. Select the set of Forms to be generated.
4. Review the displayed sample list and any global errors or form–specific errors
identified by the TurboMass software.
•
Correct any global errors (if possible) by changing the rows selected for
processing in the sample list.
•
Correct any form–specific errors (if possible) by adjusting sample
assignments associated with Form.
5. Open the Tentatively Identified Compounds dialog (if a Form 1 TIC has been
selected – or else skip to step 8) and review the default compound assignments
for each reported peak.
6.
As appropriate, compare the spectra of the alternate search hits with the peak
spectrum and change the TIC assignment if necessary.
7. Close the Tentatively Identified Compounds dialog when all peaks have been
reviewed.
8. Choose the Print command from the Report menu. The TurboMass software
then queues the selected rows of the sample list for processing for all selected
reports.
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Customized Field Display
You are able to define which data columns are displayed using the Options menu
item Customize Field Display dialog to appear in the sample list view (both on
Sample List tab and Form–specific tabs, where applicable). The display is updated
when the dialog is closed.
This dialog is disabled when the Form 6 tab is displayed (since there are no
selectable columns on this tab) but enabled at all other times.
Sample List Tab
The Report Generation window is displayed when the Continue button is clicked in
the Select Forms dialog. The Sample List tab is selected initially. An additional tab
will display for each of the Forms selected in the Select Forms dialog. The
following screen shows all forms selected.
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Row Colors
The color in which rows are displayed indicates how they will be used in the
generation of the current form.
Disregard – Gray: Gray indicates that the row is not involved in the generation of
the Form.
Primary – Blue: Blue indicates that the row is the primary data set for a Form. For
example, multiple blue rows in the Form 1 tab indicate that a separate Form 1 will
be generated for each row. Most other Forms have just one blue row indicating that
just one Form of that type will be generated for the sample list.
Summary – Black: Black indicates that the row will form part of a summary table
on the form. For example see Form 2 or Form 5.
Other Colors: Form 3 is a unique case, in that it involves three (or possibly just
two) files that are interrelated. Each of these three rows uses a unique color to
indicate its role.
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Environmental Reporting
About this Window
1. You can size this window and the relative sizes of the sample list and message
panes may be adjusted using the splitter bar.
2. The first column in the list view (check box and row number) always appears
but the other columns are configurable by the user in the same way as for the
main TurboMass Sample List window.
3. Any rows in the sample list that do not contain a (raw data) file name will be
ignored and not added to the view. (This would remove the comments added to
the Tutorial Reports sample list included with the example data.)
4. The row number associated with each row in the sample list remains unchanged
on all tabs. That is, if rows are unchecked on the Sample List tab then there will
be gaps in the numbering on the Form tabs (which only display data files that
have been selected for reporting).
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Form 1 Tab – Organics Analysis Data Sheet
When you select Form 1 - Organics Analysis Data Sheet from the Select Forms
dialog the Report Generation Window – Form 1 Tab appears.
Qualifiers (Q Flags)
In addition to the concentration of a compound the Form 1 also contains a column
labeled "Q" for qualifier. A qualifier provides additional information about the
compound.
IMPORTANT: If you change the quantitative results at the report generation time (for
example, you select a different method) you must reprocess, otherwise the qualifier
flag assignments may be invalid.
The EPA-defined qualifiers are:
U This flag indicates the compound was analyzed for but not detected or below the
MDL.
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NOTE: For the purpose of environmental reports the term MDL is used to indicate the
threshold value for the "U" qualifier flag. Values below this threshold value will flag
the compound with a "U" in the Form 1 report and no concentration values will be
printed.
J
This flag indicates an estimated value. This flag is used in the following
circumstances:
•
When estimating a concentration for Tentatively Identified
Compounds where a 1:1 response to the total ion current of the nearest
internal standard is assumed (Form 1 TIC)
•
When the mass spectral and retention time data indicate the presence
of a compound that meets the volatile and semivolatile GC/MS
identification criteria, and the result is between the compound’s MDL
and Reporting Limit. (Form 1).
IMPORTANT: The Reporting Threshold value will be used as the Reporting Limit for the
purpose of Setting flags on Form 1 and determining what Compounds to show on
the general environmental Quantitative Report (PKIEnvQuant template) if no
Custom Compound List (which includes Reporting Limits) is defined.
N This flag indicates presumptive evidence of a compound. This flag is only used
for Tentatively Identified Compounds, where the identification is based on a
mass spectral library search. It is applied to all Tentatively Identified
Compounds results. For generic characterization of a Tentatively Identified
Compound, such as “chlorinated hydrocarbon”, the N flag is not used.
B This flag is used when the analyte is found in the associated method blank as
well as in the sample. It indicates probable blank contamination and warns the
data user to take appropriate action. This flag is used for a tentatively identified
compound as well as for a positively identified target compound. Blank
contaminants are flagged B only when they are detected in the sample.
E
This flag identifies compounds whose concentrations exceed the upper level of
the calibration range of the instrument for that specific analysis. If one or more
compounds have a response greater than the upper level of the calibration range,
the sample or extract shall be diluted and reanalyzed.
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D If a sample or extract is reanalyzed at a higher dilution factor, for example when
the concentration of an Analyte exceeds the upper calibration range, all reported
concentrations on that Form I are flagged with the D flag. This flag alerts data
users that any discrepancies between the reported concentrations may be due to
dilution of the sample or extract.
A This manually-applied flag indicates that a tentatively identified compound is a
suspected aldol-condensation product.
X Other specific flags may be required to properly define the results. If used, the
flags should be fully described.
Section of the Window
Description
Sample List view
The spreadsheet displays selected information from the
Sample List.
Column widths can be changed in the standard way, by
dragging the header divider. The selected columns can
be changed using the Options/Customize Display.
Deactivate Q flags
reporting for Form 1
This Form includes one unique feature; it contains
check boxes enabling you to deactivate specific Q flag
reporting.
Any Q Flags selected will not be printed in the Q
column of Form 1 for any compound.
The All flags selection will prevent any Q flags from
being reported.
Message pane
Shows general warnings and all form–specific
errors/warnings.
NOTE: The row numbers appearing for each sample on this tab (and all Form tabs) will be
the same as those from the Sample List tab.
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Environmental Reporting
Form 1 TIC Tab – Tentatively Identified Compounds
The Status column of the Form 1 TIC (Tentatively Identified Compounds) indicates
whether or not the qualitative results have been reviewed and a Tentatively Identified
Compound selected for each peak (even if this was just an implicit acceptance of the
default top hit). Pending indicates that the file has not yet been fully reviewed,
Complete indicates that TIC selection has been completed for the file.
NOTE: When using TurboMass to run Environmental Reports, in the Qualitative Method
Editor, 'Exclude target compounds' must be checked so that Form 1 TIC reports the
proper results.
Section of the Window
Description
Sample List view
The spreadsheet displays selected information from the
Sample List.
Column widths can be changed in the standard way, by
dragging the header divider. The selected columns can be
changed using the Options/Customize Display.
Message pane
This is a read–only display window displaying messages.
Shows general warnings and all form–specific
errors/warnings.
As for Form 1, the Form 1 TIC display shows all rows other than Tune Eval and
calibration rows in the primary data color (see Row Colors), which indicates that a
separate report will be generated for each row.
Context Menu
A pop-up menu appears when you right–click on the Form 1 TIC row with the
following item:
Assign Tentatively Identified Compounds... - This opens the Tentatively
Identified Compounds dialog which allows you to match peaks with compound
names.
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About Tentatively Identified Compounds
This dialog displays when you choose the Assign Tentatively Identified
Compounds... command from the Forms menu (or the context menu on the Form 1
TIC tab). In this dialog you review the hits for the set of unidentified peaks from
each sample run (excluding tune evaluation and calibration samples) and assign a
compound name to each peak. In addition to the specific compound names supplied
from the NIST library search you have access to a set of generic terms (such as
unknown alkane, unknown aromatic) created previously by an administrator.
A typical session of assigning TICs might involve selecting names to be applied to
each of 10 to 20 peaks from 20 or more samples. This list of TICs must be
previously generated in the Sample List window using a qualitative method.
If the NIST library search has done a good job it may be possible to simply accept
all the default compounds names offered (i.e., the highest rated hit). For this reason
the software provides for a simultaneous display of the current tentatively identified
compound setting for each peak in a selected sample. This display also allows
reviewing the final set of selections to ensure consistency, e.g., the same compound
name has not been used twice).
The following screen is a general layout of the Tentatively Identified Compounds
dialog prior to your interaction (other than selecting a file).
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Parameter
Description
File list
This list displays the files for which TICs must be identified.
It also displays the TIC status as Pending or Complete.
Sample ID - The Sample ID field from the selected sample
list row (this can be left empty)
File name - The raw file name for the selected sample row
(this cannot be left empty)
Status - Indicates whether or not the TIC names have been
reviewed for each sample row
When an unreviewed file is selected (directly or using the
Next Sample button) the peak list associated with that file will
be displayed in the center list, with the first peak selected.
A single row in the list can be selected, which causes the peaks
from the associated qualitative file to be displayed in the peak
list, along with the current TIC name associated with each.
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Peak list
This list view displays the peaks from the selected file that
require a TIC assignment.
Del - Contains an “X” if the peak will be deleted from the
report
RT - The peak retention time
Assigned Name - The currently assigned TIC name for the
peak (best spectral match originally)
Est. Conc. - The estimated concentration of the compound
based on the ratio of its total ion current area to that of the
nearest internal standard.
Qualifiers - EPA qualifier codes assigned to the peak (‘J’
and ‘N’ originally)
When a peak is selected (directly or using the ‘Next Peak’
button) the library search hits associated with that peak will be
displayed in the right–hand list.
The Assigned Name field will display the current compound
name associated with the selected peak. The first time the
peak is selected that will be the top hit from the right–hand
list. Subsequently the Assigned Name will be that selected by
the user (which may also be the top hit).
A single row in the list can be selected, which causes the
library search results from the associated qualitative file to be
displayed, along with predefined ‘generic’ compound names
list.
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Compound list
This list view displays the top hits from the library search with
a predefined generic compound list at the bottom.
Compound Name - The names from the plot hits list, plus
the generic names.
CAS # - The Chemical Abstracts Service number for the
compound (for NIST hits only)
Match - The Match factor for this compound, as returned by
the NIST library search
A single row in the list can be selected, which causes that
compound name to be assigned to the currently selected peak
and displayed in the ‘Assigned Name’ column for that peak.
If the selected item is one of the predefined ‘generic’ names
and the current Qualifier string contains the ‘N’ flag, the ‘N’
will be eliminated from the string.
Qualifiers
A text box indicating the EPA qualifier codes applied to the
selected peak. This field is enabled when a peak is selected in
the peak list and you have permission to edit qualifier codes.
Next Sample
(below file list)
Click this button to mark the currently selected file as
Complete and select the next file in the list.
Next Peak
(below peak list)
Click this button to select the next peak in the currently
selected file.
If the current peak is the last in the file, then current file will
be marked Complete and the next file will be selected in the
file list and the first peak from that file will be selected in the
peak list.
Next Name
Click this button to select the next compound name from the
compound list. If this is one of the NIST plot hits then its
spectrum will be displayed in the bottom spectrum control.
New Name
Click this button to display the Generic TIC Names dialog.
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Accept
A command button that assigns the currently selected name in
the right–hand list to the selected peak. That name will then
appear in the center list in the ‘Assigned Name’ column.
PEAK plot
A plot of the currently selected chromatographic peak.
Plot properties can be changed for this and all other plots by
selecting Properties from the right-click context menu.
Behavior is similar to the TurboMass Chromatogram
window.
SPECTRUM
The apex spectrum from the currently selected peak
(top)
Plot properties can be changed by selecting Properties from
the right-click context menu. Behavior is similar to the
TurboMass Chromatogram window.
SPECTRUM
(middle)
The background subtracted spectrum from the currently
selected peak. Background subtraction is performed
automatically using the Chromatogram Combine function.
The three peak apex spectra are averaged, and the spectrum of
the scan just before the beginning of the peak is subtracted.
LIBRARY SPECTRUM
(bottom)
The library reference spectrum for the currently selected plot
hit from the compound list. This plot is empty when one of the
‘generic’ compound names is selected.
OK
Click this button to close the dialog and save the set of
selected compound names with each file marked Complete. If
the last file in the list is selected (peaks displayed in the peak
list) but not yet marked ‘Complete’, it will be changed to
‘Complete’.
Cancel
Click this button and a message box with the message “Save
changes?” plus Yes/No/Cancel buttons appears. If you click
the Yes button, the set of selected compound names for each
peak will be saved and the dialog closed.
Clicking the No button causes no data to be saved and the
dialog closes.
If you click the Cancel button the dialog will remain open (but
no data saved)
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To assign the tentatively identified compounds for the selected files:
1. Review the displayed peak plot and spectra associated with the first peak in
the selected file (and the spectrum for the top hit).
2. Click Next Name (or click on another name in the right–hand list) to
display the spectrum associated with another plot hit compound.
3. When you have decided which compound name should be assigned to the
selected peak, select that name and click Accept.
or
Having decided that none of the compound names from the plot hits list can
be definitely assigned to the peak, select one of the generic names supplied
or
Having decided that none of the generic names is applicable either, click the
New Name button and enter a new generic name for selection.
or
Right-clink on the current peak’s retention time and select Hide/Show. This
will place an “X” under the Del(eted) column and the peak will not be
reported.
4. Edit the qualifier codes applied to the peak, if required. (The TurboMass
software will automatically change the codes if a generic name is selected –
see the Behavior table.)
5. Click Next Peak, or select another peak, or click Next Sample to review
peaks from the next file.
6. Click OK after reviewing the files and changing the TIC assignments as
required, to save all assignments and close the dialog. Or you can click
Cancel to abandon the procedure without saving changes to the data.
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Form 2 Tab - SMC/Surrogate Compound Recovery
When you select Form 2 - SMC/Surrogate Compound Recovery from the Select
Forms dialog the Report Generation Window – Form 2 Tab appears with the files
displayed in the summary data color.
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Section of the Window
Description
Sample List view
This is a read–only display. The view cannot be sorted and
no data item in any cell can be directly edited. Column
widths can be changed in the standard way, by dragging the
header divider. The selected columns can be changed using
the Options/Customize Display.
Message pane
This is a read–only display window. Shows general warnings
and all form–specific errors/warnings
Environmental Reporting
Context Menu
A pop-up menu appears when you right–click on a row (any cell) of the table
containing the following item.
Assign Header Sample -
If the row is an active one, it assigns the selected row as
the source of report header information for Form 2. It
displays Header in the Status column for that row (and
eliminates Header from any other row). Inactive rows
(displayed in gray) cannot be selected.
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Form 3 Tab - Matrix Spike/Matrix Duplicate Recovery
When you select Form 3 - Matrix Spike/Matrix Duplicate Recovery from the
Select Forms dialog the Report Generation Window – Form 3 Tab appears.
Section of the Window
Description
Sample List view
This is essentially a read–only display. No data item in
any cell can be directly edited.
Column widths can be changed in the standard way, by
dragging the header divider. The view cannot be sorted.
628
Comment
You may enter up to 120 characters which will be printed
on the report.
Message pane
This is a read–only display window. Shows general
warnings and all form–specific errors/warnings
Environmental Reporting
Row Colors
Form 3 shows primary data file in blue, which represents the unspiked sample
analysis. It also uses two unique colors (dark green and dark red) to indicate the
Matrix Spike sample and the Matrix Spike Duplicate samples. All the remaining
rows are unused for the report and shown in the grey Disregard color.
Status Column
The Status column indicates which rows are currently flagged as the Analyte, Spike
and Spike Dup samples to be used in generating Form 3. This apparent duplication
with the Sample Type column is because it will be possible for you to over–ride the
Sample List’s file Type and assign a different row as one of the three key data files.
Context Menu
A pop-up menu appears when you right–click on a row in the Form 3 sample list
view pane. These selections allow you to reassign the Matrix, Matrix Spike, and
Matrix Spike Duplicate samples without returning to the Sample List. (Note that
any reassignments made here are lost after the reports are printed.
Assign Analyte -
Assigns the selected row as the Analyte to be treated
as the sample from which the MS/MSD sample are
prepared for Form 3. Displays Analyte in the Status
column for that row and displays the row in the
Analyte color.
Assign Matrix Spike Sample -
Assigns the selected row as the Matrix Spike sample
for Form 3. Displays Spike in the Status column for
that row and displays the row in the Spike color.
Assign Matrix Spike
Duplicate -
Assigns the selected row as the Matrix Spike
Duplicate sample for Form 3. Displays Spike Dup in
the Status column for that row and displays the row
in the Spike Dup col.
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Form 4 Tab - Method Blank Summary
When you select Form 4 - Method Blank Summary from the Select Forms dialog
the Report Generation Window – Form 4 Tab appears:
Section of the Window
Sample List view
Description
This is a read–only display. The view cannot be sorted and
no data item in any cell can be directly edited.
Column widths can be changed in the standard way, by
dragging the header divider.
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Comment
You may enter up to 120 characters which will be printed on
the report.
Message pane
This is a read–only display window. Shows general warnings
and all form–specific errors/warnings
Environmental Reporting
Row Colors
Form 4 uses the primary data file data color (see Row Colors), for the method blank
(Meth Blank) sample. Any Tune Eval, Cont Calib, Init Calib or additional Meth
Blank rows will be shown in the disregard color since they are not included in Form
4. All remaining rows will be shown in the summary color, indicating they will be
included in the summary section of the printed report.
Status Column
The Status column indicates which row is currently flagged as the method blank.
This may be used to distinguish between several Meth Blank rows in the sample list
(only one can be treated as the primary data set for Form 4) or to flag a row of
another Sample Type as being the method blank.
Reassign Sample Type
The software allows the Method Blank assignments to be altered without going back
to the Sample List. The basic procedure is the same for all forms (where appropriate):
1. Select the tab associated with the Form for which a primary data set will be
changed
2. Select the sample list row which is to become the new primary data set
3. Right-click on that row and select the required assignment
Context Menu
This pop-up menu appears when you right–click on a row in the Form 4 sample list
view pane.
Assign Method Blank
Assigns the selected row as the Method Blank
sample for Form 4. Displays Meth Blank in the
Status column for that row and displays the row in
the primary data color.
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Form 5 Tab - Instrument Performance Check
When you select Form 5 Instrument Performance Check from the Select Forms
dialog the Report Generation Window – Form 5 Tab appears.
Section of the Window
Description
Sample List view
This is a read–only display. The view cannot be sorted
and no data item in any cell can be directly edited.
Column widths can be changed in the standard way, by
dragging the header divider.
Message pane
632
This is a read–only display window that shows general
warnings and all form–specific errors/warnings.
Environmental Reporting
Row Colors
Form 5 uses the primary data color (see Row Colors), represent the tune evaluation
(Tune Eval) sample (BFB/DFTPP). Any additional Tune Eval rows will be shown in
the disregard color. All other sample type rows will be shown in the summary color
and printed on the report.
Status Column
The Status column indicates which row is currently flagged as the tune evaluation
sample. This may be used to distinguish between several Tune Eval rows in the
sample list (only one can be treated as the primary data set for Form 5) or to flag a
row of another Sample Type (e.g. the Continuing Calibration) as being the tune
evaluation sample
Reassign Sample Type
The software allows the Tune Eval assignments to be altered.
Context Menu
This pop-up menu appears when you right–click on a row in the Form 5 sample list
view pane.
Assign Tune Evaluation Sample
Assigns the selected row as the Tune
Evaluation sample for Form 5. Displays
Tune Eval in the Status column for that
row and displays the row in the primary
data color.
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Form 6 Tab – Initial Calibration Data
The Form 6 tab - Initial Calibration Data has a unique layout among the Forms. It
consists of three adjustable–size panes; the calibration sample table, the compound
data table and the message window.
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Section of the Window
Description
Calibration Sample Table The table lists all the initial calibration data files identified
in the calibration file. The table includes columns for:
•
Row number
•
Sample ID
•
File Name (the raw file name)
•
Time and date of injection of the standard sample
The data for this table is taken from the first Calibration file
referenced by the selected lines of the Sample List.
When a row is selected the arrow keys can be used to
change the selected row and cause the list to scroll. Column
widths can be changed in the standard way, by dragging the
header divider
Compound Data Table
The data for this table are also taken from the Calibration
file. The table lists all compounds identified in the
calibration file and displays the RRF value calculated for
each concentration level, plus the average RRF and the
percentage relative standard deviation for the RRF values.
For compounds using a linear or higher-order curve fit
calibration in place of Average RRF, the goodness of fit
value (r² correlation coefficient for first order, coefficient
of determination (CofD) for higher orders).
RRF values flagged as below the minimum required value
for that compound (as defined in the Quantify method) will
be displayed in red. Similarly if the average RRF value is
below the minimum required value or the %RSD value for
a compound is greater than the specified maximum value
for that compound, they will be displayed in red..
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Section of the Window
Description
Form 6 Header sample
This drop–down list enables you to indicate the source of
the information that will appear in the Form 6 header. Note
that this information is not related to the calibration
standard samples but rather the samples analyzed utilizing
the calibration. This means that in general the source of the
header information will be one of the Analyte samples from
the Sample List tab.
The drop–down list contains the file names of all the
checked samples from the Sample List tab.
The initial selection will be the first checked Analyte (or
Analyte Dup) row from the Sample List tab.
Message pane
636
This displays errors and warnings associated with Form 6,
in a similar manner to that for all other Forms.
Environmental Reporting
Form 7 Tab – Continuing Calibration Check
When you select Form 7 - Continuing Calibration Check from the Select Forms
dialog the Report Generation Window – Form 7 Tab appears.
Section of the Window
Description
Sample List view
This is a read–only display. The view cannot be sorted and
no data item in any cell can be directly edited.
Column widths can be changed in the standard way, by
dragging the header divider.
Message pane
This is a read–only display window. Shows general
warnings and all form–specific errors/warnings
NOTE: If you change the Min RRF value in the Quantify method you must reprocess
(recalibrate) the sample list for this new value to display in the report.
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Row Colors
Form 7 uses a single data file in the primary data color (see Row Colors), for the
continuing calibration (Cont Calib) sample. All other rows will be shown in the
disregard color and are not used for the report.
Status Column
The Status column indicates which row is currently flagged as the continuing
calibration sample. This may be used to distinguish between several Cont Calib
rows in the sample list (only one can be used for Form 7) or to flag a row of another
Sample Type as being the continuing calibration sample.
Reassign Sample Type
The software allows the continuing calibration file assignments to be altered.
Context Menu
This pop-up menu appears when you right–click on a row in the Form 7 sample list
view pane.
Assign Continuing Calibration - Assigns the selected row as the
Continuing Calibration (Cont Calib) sample for Form 7.
Displays Cont Calib in the Status column for that row and
displays the row in the primary data color.
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Form 8 Tab – Internal Standard Area and RT Summary
When you select Form 8 - Internal Standard Area and RT Summary from the Select
Forms dialog the Report Generation Window – Form 8 Tab appears.
Section of the Window
Description
Sample List view
This is essentially a read–only display. The
view cannot be sorted and no data item in any
cell can be directly edited.
Column widths can be changed in the standard
way, by dragging the header divider.
Message pane
This is a read–only display window. Shows
general warnings and all form–specific
errors/warnings.
Row Colors
Form uses the primary data color (see Row Colors), for the continuing calibration
(Cont Calib) sample. Any Tune Eval, Init Calib or additional Cont Calib rows
will be shown in the disregard color since they are not included in Form 8.
Status Column
The Status column indicates which row is currently flagged as the continuing
calibration sample. This may be used to distinguish between several Cont Calib
rows in the sample list (only one can be treated as the primary data set for Form 8)
or to flag a row of another Sample Type as being the continuing calibration sample.
Reassign Sample Type
The software allows the Method Blank assignments to be altered without going back
to the Sample List.
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Context Menu
A pop-up menu appears when you right–click on a row in the Form 8 sample list
view pane.
Assign Mid–Level Standard
640
Assigns the selected row as the Mid–Level
Standard (labeled as type Cont Calib)
sample for Form 8. Displays Cont Calib
in the Status column for that row and
displays the row in the primary data color.
Environmental Reporting
Error Messages and Warnings
The list of samples in Environmental Reports is checked when it is opened and
whenever the rows are added or the state of any row is changed. All selected rows of
the sample list are examined to identify errors or warnings. If any errors are
identified then the Sample List title of the tab is displayed in red and all Form tabs
are disabled. General errors and warnings are displayed in the message pane located
on the bottom of the window.
Error Messages
An error is defined as a condition that will prevent the generation of a coherent data
set for reporting. The Print command remains disabled while such errors exist. The
following checks are made:
1. All sample rows must reference the same Analysis type (VOA, SV or QA/QC).
If more than one Analysis type is present (empty Analysis fields will be ignored
for this test) an error message will be displayed:
General
Error
Sample list contains mixed Analysis types Rows, a, b, x-z
2. All sample list rows selected for processing, other than Tune Eval types, must
reference the same Calibration file. If more than one Calibration file is referenced
an error message will be displayed:
General Error Sample list contains more than one Calibration file Rows a, b, xz
3. If no Calibration file is included in the sample list rows selected for processing,
then an error message will be displayed:
General Error
No Calibration file is defined
Rows az
4. All sample list rows selected for processing, other than Tune Eval types, must reference
the same Quantify Method. If more than one Quantify Method is referenced an error
message will be displayed:
General Error Sample list contains more than one Quantify Method file Rows a, b, xz
5. If no selected rows reference environmental sample types (e.g. all set to
Standard) an error message will be displayed:
General Error Sample list contains no environmental sample types
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6. All sample list rows selected for processing that specify a matrix type must
specify the same type, or an error message will be displayed:
General
Error Sample list contains mixed matrix types Rows a, b, xz
7. All sample list rows selected for processing that specify a concentration level
(low/med) must specify the same level, or an error message will be displayed:
General Error Sample list contains mixed matrix concentration levels Rows a, b, xz
8. A sample list row selected for processing cannot be reassigned as different
sample types on different Form tabs, with the exception of Tune Eval (Form 5)
and Cont Calib (Form 7) [or Form 8], which is valid. For example assigning the
same row as Meth Blank for Form 4 and as Tune Eval for Form 5 would cause
an error message to be displayed:
General Error Sample list contains invalid multiple sample type assignments
Rows a, b, xz
9. If the calibration file identified in the sample list does not exist in the Project
CurveDB directory then an error message will be displayed:
General Error Calibration file cannot be found
Rows az
10. Selected rows, other than Tune Eval or Calib types, must contain values for
Analysis and Matrix.
General Error Sample list contains sample rows with blank Analysis or Matrix
column Rows az
11. If Matrix is Soil, then the Conc Level column cannot be blank.
General Error Sample list contains Soil sample with blank Conc Level column
Rows az
NOTE: For items 1 to 5, the display of row numbers exhibiting the error is determined in
one of the two following ways:
1. The first Calibration file, Quantify Method, etc located (ignoring any referenced
by the Tune Eval sample) will be taken as the correct one and any row that
references a different one will be flagged as in error.
2. The Calibration file, Quantify Method, etc that is referenced most frequently in
the selected rows will be taken as the correct one and any row that references a
different one will be flagged as in error.
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Contiguous groups of rows will be displayed in the form xz, while isolated rows will
displayed separated by commas.
General errors must be cleared before the report generation process can proceed.
Although general errors can be cleared by unchecking rows this may leave a sample
list that cannot be used to generate the required forms (i.e., Form specific errors may
be generated in the process). In this event you may have to leave this environment
and edit the sample list or create a new one before generating reports.
Warnings
A warning is defined as a condition that does not meet the strict rules of CLP
reporting but may be valid in the context of “CLP–like” reporting. Warnings do not
prevent access to the Form tabs nor do they prevent reports being generated,
although there is no guarantee the results will be complete or entirely valid. The
following checks are made:
1. If sample list rows selected for processing specify a sample type other than one
of those listed (plus Analyte), a warning message will be displayed:
General
Warning
Sample list contains nonenvironmental sample
types
Rows a, b, xz
NOTE: The display of row numbers exhibiting the warning should be determined as
described in the previous section.
2. A sample list row selected for processing should not be reassigned as different
sample types on different Form tabs, with the exception of Tune Eval (Form 5)
and Cont Calib (Form 7) [or Form 8], which is valid. For example assigning the
same row as Meth Blank for Form 4 and as Tune Eval for Form 5 would cause a
warning message to be displayed: General
Warning
Sample list
contains invalid multiple sample type assignments
Rows a, b, xz
3. If the injection time of any rows selected for processing is more than 12 hours
after the injection time of the tune evaluation sample.
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Form Specific Checks
The sample list is checked when it is opened and whenever the state of any row is
changed. All selected rows of the sample list will be examined to identify errors or
warnings. If any errors related to a specific Form are identified then the title of that
Form tab will be displayed in red. The error will be displayed in the message pane
on the Form tab as well as on the Sample List tab. Form-specific warnings will also
be displayed in both places.
Form–specific errors/warnings follow General errors/warning in the message pane
on the Sample List. A Form–specific error is defined as a condition that will prevent
the generation of that Form. The Print command will remain disabled while such
errors exist.
A Form–specific warning is defined as a condition that does not meet the strict rules
of CLP reporting but may be valid in the context of “CLP–like” reporting. Warnings
do not prevent reports being generated, although there is no guarantee the results
will be complete or entirely valid.
Form 1
The sample list is checked for the existence of sample types reported on
Form 1.
Errors: If no rows selected for processing are of sample type other than
Tune Eval, Init Calib or Cont Calib then an error message will be displayed:
Form 1 Error Sample list contains no sample types reported on Form 1
Form 1 TIC
The sample list is checked for the existence of sample types reported on
Form 1 TIC.
Errors:
If any rows selected for processing (of sample type other than Tune Eval, Init Calib
or Cont Calib) have no associated qualitative results saved, then an error message
will be displayed: Form 1 TIC Error No qualitative data found for some selected
samples Rows a, b, x–z
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If no rows selected for processing are of sample type other than Tune Eval, Init
Calib or Cont Calib then an error message will be displayed: Form 1 TIC Error
Sample list contains no sample types reported on Form 1 TIC
Either of these errors will prevent the TIC assignment process being performed.
Warnings: If any rows selected for processing (other than Tune Eval, Init
Calib or Cont Calib rows) still have the Pending status then an error
message will be displayed: Form 1 TIC Warning Samples with incomplete TIC
selection will not be reported Rows a, b, x–z
Form 2
The sample list is checked for the existence of sample types reported on Form. The
first Analyte (or Analyte Dup) row found in the selected rows will be marked as the
source of the header information for Form 2. You can change this assignment if
necessary.
Errors: If no rows selected for processing are of sample type other than Tune Eval,
Initi Calib or Cont Calib then an error message will be displayed: Form 2 Error
Sample list contains no sample types reported on Form 2
Warnings: No warnings specific to Form 2 have been identified.
Form 3
Generation of Form 3 requires three (and only three) files: An Analyte sample, a
Matrix Spike sample (prepared by spiking the analyte) and a Matrix Spike (a second
spiked sample). The default rows are identified as follows:
Matrix Spike Duplicate:
•
Look for the last Spike Dup sample in the list. If no Spike Dup can be
located a warning condition exists (see below).
Matrix Spike:
•
If a Spike Dup was located and its Sample ID ends with MSD, look for the
Spike sample with the same root Sample ID but ending with MS. If this is
not located, look for the first Spike sample preceding the Spike Dup. If one
is not found look for the first Spike sample following the Spike Dup. If no
Spike can be located an error condition exists (see below).
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•
If a Spike Dup was located and its Sample ID did not end with MSD look
for the first Spike sample preceding the Spike Dup. If one is not found look
for the first Spike sample following the Spike Dup. If no Spike can be
located an error condition exists (see below).
•
If no Spike Dup was located, look for the last Spike sample in the sample
list. If no Spike can be located an error condition exists (see below).
Analyte:
•
If a Spike Dup was located and its Sample ID ends with MSD, look for the
Analyte sample with the Sample ID formed by removing the MSD (i.e.
same root, no suffix). If this is not located, look for the first Analyte (or
Analyte Dup) sample preceding the Spike Dup. If one is not found look for
the first Analyte (or Analyte Dup)sample following the Spike Dup. If no
Analyte (or Analyte Dup) can be located an error condition exists (see
below).
•
If a Spike Dup was located and its Sample ID did not end with MSD look
for the first Analyte (or Analyte Dup) sample preceding the Spike Dup. If
one is not found look for the first Analyte sample following the Spike Dup.
If no Analyte (or Analyte Dup) can be located an error condition exists (see
below).
•
If no Spike Dup was located, look for the first Analyte (or Analyte Dup)
sample preceding the Spike in the sample list. If one is not found, look for
the first Analyte (or Analyte Dup) following the Spike. If no Analyte (or
Analyte Dup) can be located an error condition exists (see below).
Errors
646
•
If no Spike sample was located in the rows selected for processing
(according to the rules given above), then an error message will be
displayed: Form 3 Error No matrix spike sample identified
•
If no Analyte (or Analyte Dup) sample was located in the rows selected for
processing (according to the rules given above), then an error message will
be displayed: Form 3 Error No Unspiked sample identified
Environmental Reporting
Warnings: If no Spike Dup sample was located in the rows selected for
processing (according to the rules given above), then a warning message will be
displayed: Form 3 Warning No matrix spike duplicate sample identified –
form will be incomplete. This is a valid condition, since Spike Dup samples are
not always run.
Form 4
Primary data for Form 4 will be taken from a Meth Blank sample with summary
information from samples types other than Tune Eval, Init Calib or Cont Calib. The
default Meth Blank to be used as the primary data set will be the last Meth Blank
sample row selected in the sample list.
Errors: If no Meth Blank sample was located in the rows selected for processing
(according to the rules given above), then an error message will be displayed: Form
4 Error No method blank sample identified
Warnings: If no rows selected for processing (excluding the Meth Blank
row) are of sample type other than Tune Eval, Init Calib or Cont Calib
then a warning message will be displayed: Form 4 Warning Sample list
contains no sample types reported in Form 4 summary
Form 5
Primary data for Form 5 will be taken from a Tune Eval sample with summary
information from other samples types (other than Tune Eval). The default Tune Eval
to be used as the primary data set will be the last Tune Eval sample row selected in
the sample list.
Errors: If no Tune Eval sample was located in the rows selected for processing
(according to the rules given above), then an error message will be displayed: Form
5 Error No tune evaluation sample identified
Warnings:
If no rows selected for processing are of sample type other than Tune Eval then a
warning message will be displayed: Form 5 Warning Sample list contains no
sample types reported in Form 5 summary
If the Analysis type is Volatiles and the specified Tune Eval file references DFTPP
(or Analysis is Semivolatiles and Tune Eval references BFB) then a warning
message will be displayed: Form 5 Warning Tune evaluation sample references
the wrong compound for the Analysis type
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Form 6
The data for Form 6 will be taken from the Calibration file referenced by most of the
rows in the sample list. The general checks will have ensured that only one
Calibration file is referenced. This Calibration file can be taken from any sample
row other than the Tune Eval (which is ignored).
The first Analyte (or Analyte Dup) row found in the selected rows of the
sample list will be marked as the source of the header information for Form
6. The file name of this sample will be displayed on the Form 6 tab. The user
can change this assignment if necessary.
Errors: No errors specific to Form 6.
Warnings: No warnings specific to Form 6.
Form 7
Primary data for Form 7 will be taken from a Cont Calib sample. The default Cont
Calib will be the last Cont Calib sample row selected in the sample list.
Errors: If no Cont Calib sample was located in the rows selected for
processing (according to the rules given above), then an error message will
be displayed: Form 7 Error No continuing calibration sample identified
Warnings: No warnings specific to Form 7.
Form 8
Primary data for Form 8 will be taken from a Cont Calib sample (which may be the
Mid-Level of an Initial Calibration with summary information from other samples
types (other than Tune Eval, Cont Calib or Init Calib types). The default Cont Calib
to be used as the primary data set will be determined as follows:
648
•
If the selected sample rows contain Cont Calib rows then the primary
data set will be last Cont Calib sample row selected in the sample list.
•
If the selected sample rows do not contain a Cont Calib row but
contain one or Init Calib rows then the middle row of this set will be
Environmental Reporting
marked (in the Status column) as the Cont Calib. If an even number
of Init Calib rows are selected then the closest row past the mid–point
will be flagged as the Cont Calib. If only one Init Calib row exists
then that will be chosen.
Errors: If no Cont Calib sample was located in the rows selected for processing
(according to the rules given above), then an error message will be displayed: Form
8 Error No continuing calibration sample identified
Warnings: If no rows selected for processing are of sample type other than Tune
Eval, Cont Calib or Init Calib then a warning message will be displayed: Form 8
Warning Sample list contains no sample types reported in Form 8 summary
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Report Method Usage
The following report methods specify templates designed for use from the
TurboMass environmental report generation window only. To use these report
methods they must be specified in the Submitter/Task Data window’s Report
Method tab. Examples of these reports in .PDF file format are found in the
directories:
C:\TurboMass\Tutorial_VOA.pro
C:\TurboMass\Tutorial_SVOA.pro
IMPORTANT: Using these report methods in a sample list Report Method column for
acquisition or processing could lead to invalid or misleading results.
Form1TIC_SV
Form1TIC_VOA
Form2_SV_soil
Form2_SV_Water
Form2_VOA_Soil
Form2_VOA_Water
Form3_SV_Soil
Form3_SV_Water
Form3_VOA_Soil
Form3_VOA_Water
Form4_SV
Form4_VOA
Form5_SV
Form5_VOA
PKI1TIC_SV
PKI1TIC_VOA
PKI2_SV_soil.
PKI2_SV_water
PKI2_VOA_soil
PKI2_VOA_water
PKI3_SV_Soil
PKI3_SV_Water
PKI3_VOA_Soil
PKI3_VOA_Water
PKI4_SV
PKI4_VOA
PKI5_SV
PKI5_VOA
The following report methods can be included in a sample list Report Method
column to generate reports during acquisition or reprocessing. Where the report
method is specific to a particular sample type, the required sample type is indicated
in parentheses. Other specific limitations are also indicated in parentheses.
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Form1_SV
Form1_VOA
Form6_SV
Form6_VOA
Form7_SV
Form7_VOA
Form8_SV
Form8_VOA
ICV_SV
ICV_VOA
LCS_SV
LCS_VOA
PKI1_LCS_SV
PKI1_LCS_VOA
PKI6_SV
PKI6_VOA
PKI7_SV
PKI7_VOA
PKI8_SV
PKI8_VOA
PKIEnvQuant
(a valid calibration file must be specified on the sample list row)
(a valid calibration file must be specified on the sample list row)
(Cont Calib samples only)
(Cont Calib samples only)
(report method must appear only on the last row and the first
row must be a Cont Calib)
(report method must appear only on the last row and the first
row must be a Cont Calib)
(Cont Calib samples only)
(Cont Calib samples only)
(Lab Control samples only)
(Lab Control samples only)
Lab Control samples only)
Lab Control samples only)
a valid calibration file must be specified on the sample list row)
a valid calibration file must be specified on the sample list row)
Cont Calib samples only)
Cont Calib samples only)
report method must appear only on the last row and the first row
must be a Cont Calib
report method must appear only on the last row and the first row
must be a Cont Calib
intended for Analyte samples; will give incomplete results for
calibration samples)
In addition to the above Report Methods and associated templates, there are three
other included templates of use if .CSV (comma separated variable) reports are
required. All must be produced within the environmental report generation
window. Examples are in the same directories as the .PDF files.
Form1_CSV
Form5_CSV
Form6_CSV
(reports both Form 1 and Form 1 TIC)
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Submitter/Task Data Window
The Submitter/Task Data Window combines several related functions:
•
Maintenance of Submitter/Task hierarchy
•
Maintenance of Custom Compound Lists
•
Mapping of Forms to Report Methods
These functions are combined in one Submitter/Task Data window since both
Custom Compound Lists and mapping of Forms to Report Methods are specific to a
Task.
The basic requirements for Custom Compound Lists are that an environmental
laboratory should be able to define subsets of the compounds in a quantify method
to be reported for a particular project (Task in TurboMass terms) of a particular
client (Submitter in TurboMass terms), and also to set the (concentration) reporting
level of each of these compounds uniquely for each client’s (Submitter’s) projects.
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The mapping of Forms to Report Methods allows Form customization by providing
a translation between the EPA Forms and Communiqué templates (referenced in
TurboMass report methods). This translation enables the environmental report
generation process, which is driven from the selection by the user of the Forms to be
printed, to assemble the appropriate set of report methods/templates automatically.
The Status Bar
When a Custom Compound List is displayed the status bar (located on the bottom of
the window) displays the exact origin of the Custom Compound List: the Project
name is displayed in the left–hand segment and the Quantify Method name, along
with the time and date the compound list was imported, is displayed in the right–
hand segment. At all other times the status bar will be left empty.
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Submitter/Task List
This window is displayed when the Submitter/Task Data… command is chosen
from the Environmental Configuration submenu under the Tools menu in the main
TurboMass Sample List window. The following Submitter/Task pane on the left
side shows a Submitter and Task selected.
This pane is a hierarchical tree view showing clients (Submitters) and their projects
(Tasks) displayed in alphabetical order. The tree view can be expanded and
collapsed by clicking on the “+” or “-“ nodes next to the Submitter names.
Nodes can be renamed by using the right-click context menu.
You can also associate a Custom Compound List with a particular Task, but not
directly with a Submitter.
Context Menu for the Submitter/Task List
Right–clicking on a node of the Submitter/Task tree view displays the Context
menu. Note that it will not appear if you click on empty space within the list.
Command
Description
New Submitter
Displays the New Submitter dialog to create a new Submitter name.
New Task
Displays the New Task dialog to create a new task for the Submitter.
Collapse All
Closes all expanded nodes so that only the top level nodes are
displayed.
Expand All
Displays all nodes.
Rename…
Enables you to change the name of the selected node
Delete
Deletes the Task node and its associated data (compound list and/or
report methods)
Info
Displays a Task Info dialog showing the comments entered by the user
when the Task was created.
The Submitter/Task Data window has the following Menu item commands.
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Menu
Command
Description
File
Save
Saves the Submitter/Task data.
Export…
Displays the to export Submitter/Task data from
TurboMass to archive or another computer.
Import…
Displays a File Open dialog, allowing you to select a
previously exported Submitter/Task Data file. When a
file has been chosen the Import dialog will be displayed.
Exit
Closes the Submitter/Task Data window. If unsaved
changes exist then a dialog will be displayed with the
message “Save changes?” and Yes and No buttons.
Clicking Yes saves the data.
Clicking No closes the dialog and any changes to the
data will be lost.
Edit
New Submitter…
Displays the New Submitter dialog to enter a new
Submitter.
After entering a new submitter Name the OK button will
be enabled. Each submitter name must be unique
(independent of case). If the entered name is valid, the
dialog will close and a new submitter node will added to
the tree.
If the entered name already exists, an error message is
displayed.
New Task…
Displays the New Task dialog to enter a new task for a
submitter.
Load Compound
List…
Displays the Load Compound List dialog. When you
have selected a method the compound list is read from
the Quantify method and assigned to the selected Task.
Initially all compounds are selected for use.
Select All
Puts a checkmark next to all compounds in the current
compound list.
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Unselect All
Removes checkmarks from all compounds in the current
compound list.
Rename…
Allows you to change the name of the selected node.
Delete
If a Task node is selected, it deletes the task node and its
associated data (compound list and/or report methods).
If a Submitter node is selected, all Tasks, associated
report methods and custom compound lists for this
submitter are also deleted.
You can recover deleted data by closing the window
without saving the data.
Help
Help Topics
Displays the Help topics for this window
New Task Dialog
This dialog displays when New Task… is chosen from the Edit menu in the
Submitter/Task Data window.
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Parameter
Description
Name
An edit box in which you can enter a name of up to 50
characters for the new task. Each task name must be unique
for that submitter (independent of case).
Load compound list from
Quantify Method
A drop–down list from which you can select the Quantify
Method to be used as the source of the compound list.
Environmental Reporting
Browse
Click this button to open a file selector dialog from which
you can select a Quantify method from any project.
OK
Each task name must be unique for that submitter
(independent of case). If the entered name is valid, the
dialog closes and a new task node is added to the tree under
the current submitter. If the entered name already exists, an
error message will be displayed.
Cancel
Closes the dialog without creating a new task or compound
list.
Export Submitter/Task Data Dialog
This Export dialog displays when you select Export… from the File menu in the
Submitter/Task Data window. Here you select the Submitters and Tasks with their
corresponding Custom Compound List and Report Methods that you want to Export
(as a *.CCL file). The default directory is the MethDB directory of your current
project.
Parameter
Description
Select Submitter/Task data
to be exported
Displays the Submitter/Task hierarchy as shown in the
Submitter/Task Data window. This includes all of the
Submitters and Tasks available with none selected. Click in
the box to the left of the item you want to select.
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Select All
Clicking this button that will applies check marks to all
Submitters and Tasks.
Unselect All
Clicking this button removes any check marks from all
Submitters and Tasks.
OK
Clicking this button displays a File Save As dialog allowing
you to enter a file name for the exported data and to select
the directory where the file will be stored.
Cancel
Clicking this button closes the dialog without exporting any
data.
Import Submitter/Task Dialog
The Import dialog displays when you select a previously exported Submitter/Task
data file following use of the Import… command from the File menu in the
Submitter/Task window.
The form of the Import dialog is similar to that of the Export dialog, except for the
title and the caption above the tree list are modified appropriately.
Control
Description
Submitter/Task list
Applying a check mark to a Submitter will cause all Tasks
belonging to that Submitter to be checked. Unchecking a
Submitter will cause all Tasks belonging to that Submitter
to be unchecked.
Unchecking one or more (but not all) Tasks under a
Submitter will cause the Submitter check box to 'gray'
indicating there are some Tasks selected and some
unselected.
Select All
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Clicking this button applies check marks to all Submitters
and Tasks.
Environmental Reporting
Unselect All
Clicking this button removes any check marks from all
Submitters and Tasks.
OK
Clicking OK imports the selected Submitter/Task data.
If a name conflict occurs (i.e., the same Task name already
exists for that same Submitter) a dialog displays with the
message:
Data already exist for Task : <taskname>.
Enter new task name.
The dialog will include a New name edit box and OK,
Cancel and Cancel All buttons. The OK button will be
disabled until you enter a new name for the Task. Upon
clicking OK the new Task will be created and the data
imported.
Cancel
Clicking this button closes the dialog without exporting
any data.
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Report Method Tab
An independent mapping of Forms to Communiqué Report Methods can be defined
for each Submitter and Task. This mapping is global across all Projects.
NOTE: It is up to you to ensure the appropriate report methods are in the Project (this
occurs automatically when a new project is created via the Project Wizard).
If specific report methods have not been selected for a given Submitter/Task, then
the Default or the most recently selected set will be assigned to that Submitter/Task
(see below).
The Report Methods dialog uses the Form descriptions that appear on the EPA
Forms. The separate VOA/SV and Matrix columns of the dialog describe when the
specific Report Method is used.
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In the Report Method form, the only column that contains information that you can
change is the Report Method column. The columns can be sized in the standard way
by dragging the header divider.
Form
The EPA Form number and subcategory letter (from
OLM04.2)
Description
The full description of the Form.
VOA/SV
The analysis type the Form is used for — volatiles or
semivolatiles.
Matrix
The matrix type the Form is used for — water samples,
soil samples or both.
Report Method
The Communiqué Report Method used to generate this
Form. Positioning your cursor in the Report Method
column displays a button. Clicking this button displays
a file selector for the MethDB directory of the current
Project.
To define the report methods
To define the report methods (and hence Communiqué templates) to be used in
generating the EPA Forms for an existing Submitter/Task:
1. Choose Submitter/Task Data… from the Environmental Configuration
submenu under the Tools menu in the Sample List window.
2. Select the appropriate Task for the Submitter.
3. Select the Report Methods tab.
4. Review the table displaying Forms 1 to 8, and their variants, together with the
associated report method.
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5. Where necessary, select the appropriate report method to be associated with
each Form. When the mapping of Forms to report methods is correct, choose the
File/Save command.
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Custom Compounds Tab
It is possible to define a subset of the compound list from a Quantify Method and
associate it with a Submitter and/or Task name (one list per Task). These subsets can
be used for three purposes:
1. During quantitative processing to ensure only the specified compounds are
reported and are identified as target compounds for qualitative processing.
2. During qualitative processing to eliminate from the search for Tentatively
Identified Compounds only those peaks that are identified as targets for that
particularly Task.
The Custom Compound Lists also enable you to define a reporting limit for each
compound (i.e., set the “J” flag if the compound is between the Method Detection
Limit and the Reporting Limit, or the “U” flag if it is below both) on the Forms.
Once the Custom Compound List has been generated it will retain a reference to the
Quantify Method from which it was derived. It is not part of the method and no
automatic synchronizing of the custom list with the compound list in the method
will take place.
When a Custom Compound List is selected the status bar displays the origin of the
custom compound list: the Project name is displayed in the left–hand segment and
the Quantify Method name is displayed in the center segment.
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Item
Description
Compound list
This list shows all the compounds from the selected
Quantify Method. Each row has a check box. Checked
items will be included in the current Submitter/Task list
and unchecked items will be excluded.
If the currently selected Task does not have an associated
custom compound list then this section of the window is
empty.
It is possible to sort the compound list in one of two ways:
Reporting limits: Water
1.
1. In the order the compounds appeared originally in
the main Quantify Method compound list – by
clicking on the header of the check box column.
2.
In alphabetical (or reverse alphabetical) order – by
clicking on the header of the compound name
column.
An edit box that displays the reporting limit value (0.000 to
999,999.999) for water samples associated with the
currently selected compound (which may be checked or
unchecked).
A change made to this field is saved if you click Previous,
Modify or Next. If instead you click another compound or
another button a dialog displays with the message “Save
changes to this compound?” and includes Yes and No
buttons. Clicking Yes saves the modified value with the
compound. Clicking No leaves the compound’s reporting
limit unchanged.
Set All
664
A command button that sets the reporting limit for water
samples for all selected compounds in the list to the value
in the ‘Reporting limits: Water edit box.
Environmental Reporting
Reporting limits: Soil
An edit box that displays the reporting limit value (0.000 to
999,999.999) for soil samples associated with the currently
selected compound (which may be checked or unchecked).
A change made to this field is saved if you click Previous,
Modify or Next. If instead you click another compound or
another button a dialog displays with the message “Save
changes to this compound?” and includes Yes and No
buttons. Clicking Yes saves the modified value with the
compound. Clicking No leaves the compound’s reporting
limit unchanged.
Set All
Click this button to set the reporting limit for soil samples
for all selected compounds in the list to the value in the
‘Reporting limits: Soil edit box.
Previous
Click this button to set the reporting limit values of the
currently selected compound to the values in the Reporting
limits: edit boxes (Water and Soil) and then selects the
previous compound in the list.
Modify
Click this button to set the reporting limit values of the
currently selected compound to the values in the ‘Reporting
limits’ edit box boxes (Water and Soil).
Next
Click this button to set the reporting limit values of the
currently selected compound to the values in the ‘Reporting
limits’ edit box boxes (Water and Soil) and then selects the
next compound in the list.
To create a Custom Compound List
To create a Custom Compound List for a new Task of an existing Submitter:
1. Choose Submitter/Task Data… from the Environmental Configuration
submenu under the Tools menu in the main Sample List window.
2. In the Submitter/Task Data window select the Submitter for whom the new Task
is to be generated.
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3. Choose New Task from the Edit menu (or the context menu for the tree list),
which will display the New Task dialog.
4. Enter a name for the new Task and select the Quantify Method from which the
compound list is to be imported. The compounds are displayed and initially each
one is checked.
5. Click on the check box to deselect a compound that is not required to be
reported for this Submitter/Task. Repeat as required.
6. Select a compound for which a different reporting limit (Water or Soil) is
required. Enter the new value in the appropriate edit field below the list and
click Modify to save the change or Next to save the change and select the next
compound (or select Previous to save the change and select the previous
compound).
7. Choose Save from the File menu to save the new Custom Compound List.
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Generic TIC Names Dialog
This dialog enables an administrator (or other person with appropriate access
permission) to edit the list of generic compound names that appears in the
Tentatively Identified Compounds dialog.
This dialog displays when you choose Generic TIC Names from the Environmental
Configuration submenu of the Tools menu or clicks the New Name… button in the
Form 1 TIC Assign Tentatively Identified Compounds dialog.
Parameter
Description
<list>
A list displaying the currently defined generic names in alphabetical
order.
<edit box>
An edit box that enables you to edit an existing name or enter a new
name.
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Add
Click this button adds the current contents of the edit box to the list as
a new entry.
Modify
Click this button to set the currently selected item in the list to the
current contents of the edit box.
Delete
Click this button to delete the selected item from the list.
To create/edit a list of generic compound names
To create a list of generic compound names:
1. Choose Generic TIC Names from the Environmental Configuration submenu
of the Tools menu.
2. Type a generic name into the edit box and click the Add button.
3. Repeat step 2 for each generic name required (the list is sorted alphabetically as
each new name is added).
4. Click OK
To edit the list of generic names:
1. Choose Generic TIC Names from the Environmental Configuration submenu
of the Tools menu.
2. Edit an existing name by selecting that name, editing as required and clicking
the Modify button.
3.
Add a new name by typing the name into the edit box and clicking the Add
button.
4. Delete an existing name by selecting the name and clicking the Delete button.
5. Click OK.
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Appendix A
TurboMass Security
TurboMass Software User’s Guide
TurboMass Security
The Security application allows a system administrator to control:
•
User access to various parts of the TurboMass system.
•
Which operations can be performed within a given part of the system.
•
Which events are audited.
Security compliments the Windows protection and adds an extra layer of security
that is specific to the TurboMass data system.
This appendix defines some security-related terms, provides an overview of the
TurboMass security model, and explains how to use the Security Manager to
configure user accounts, user groups, and how to assign group privileges.
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Security Terminology
This section defines the security terms used in this appendix.
Access Rights/Privileges
By controlling access rights or privileges, administrators can control or restrict the
actions of a group of users. Access rights are assigned to groups, and users are
members of groups. Access rights cannot be assigned directly to individual users.
Users have the access rights assigned to the group(s) to which they belong. Only
users who are members of groups with the Administer User Accounts and Groups
access right can assign rights to other groups.
Administrator
The administrator is the person responsible for managing the system, adding and
removing users and groups, and assigning access rights. The administrator has
unlimited access to TurboMass and to the Security application. The Administrator
account is always present, with full access, and only the password can be changed.
This account cannot be deleted. Administrative privileges can be granted to any user
by placing that user in the Administrators group.
Audit Log
The audit log file contains a historical list of events showing which users accessed
or attempted to access objects covered by the list of access rights. Auditing can be
customized so that only certain categories of event are included, or disabled
completely. An audit log viewer is provided within the Security Manager.
Group
A group is a collection of TurboMass users. A group can have access rights assigned
to it to restrict their movements within the data system. Groups provide a convenient
way of managing the capabilities of users (it is often easier to remember which
privileges a particular group has, rather than those of an individual). The
Administrators group cannot be deleted and always has full access rights.
Group Rights
See Access Rights/Privileges.
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Logon Name
The logon name is the name by which a user is known to Security. Each logon name
has an associated password and user account. To log in to Security, a user must
provide a valid logon name and password.
Password
A specific word used to log on when Security is enabled that verifies the user’s
identity. Passwords are case-sensitive.
Right/Privilege
See Access Rights/Privileges.
Security Manager
The TurboMass application that administers the TurboMass security system. The
Security Manager cannot be run at the same time as TurboMass.
User
A TurboMass user who usually has more limited access privileges than an
Administrator.
User Account
A record maintained by Security that contains information about a particular user.
Username
The name by which a user is known to TurboMass. A user logs on to TurboMass by
providing a valid username and password. A user’s group rights determine his
individual rights.
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Security Model
The Security Model is based on user accounts. Users are members of groups, and
groups have access privileges. A user cannot be directly given an access privilege.
The Security system performs tasks such as user account management, group
management and audit log maintenance, and logs users in and out and verifies their
access privileges.
TurboMass or TurboMass Security Manager
Login
TurboMass Security Subsystem
Validate username
and password
Access Validation
Audit Log
Management
Validate Username and Password
The system within Security that verifies a username and password TurboMass
against the existing user accounts. If Security finds an account for the specified
username and the password is correct, the user is allowed to proceed. All subsequent
access requests can then be validated. Any information written to the audit log
contains a reference to the username.
Access Validation
When a user attempts to enter a TurboMass or a Security Manager-protected area,
the Access Validation subsystem determines the access rights of the groups to which
the user belongs. An entry is also written to the audit log to reflect the outcome of
the access attempt.
Audit Log Management
The audit log management system maintains the audit log.
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Security Manager
The Security Manager is used by an administrator to assign access privileges and set
up user accounts and groups.
Specifically, an administrator can perform the following tasks:
•
Create, delete, and edit user accounts.
•
Create, delete, and edit groups.
•
Assign access privileges to groups (Group rights policy).
•
Set the account policy.
•
Disable Security.
•
Set the audit policy.
•
View and manage the audit log.
NOTE: TurboMass Security and TurboMass cannot be run simultaneously. Close
TurboMass before opening the Security application.
If Security is enabled when TurboMass is opened, the user is required to log on to
TurboMass by entering a username and password into the Login dialog.
Logging on to TurboMass with Security enabled
1. Double-click the Security icon in the TurboMass program group to open the
Security Manager dialog.
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If security is enabled, TurboMass displays the Login dialog.
2. If the following message is displayed, verify the password and username.
3. If the message remains, verify that the user has a valid account with Security.
Make sure that the account has not been disabled.
The username determines the user’s level of access allowed within TurboMass
or the Security Manager. If the user does not have full administrative privileges,
the following message may be displayed:
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4. If a user needs access to a particular area, assign the user to a group that has the
necessary access privileges. See Assigning an access privilege to an individual
user on page 686 for more information.
If the username entered does not belong to a group with administrative
privileges, the user is limited to viewing their own account information.
Changing a password without administrative privileges
1. Exit TurboMass, if necessary.
2. Start the Security application to open the Security Manager dialog and display a
list of user accounts.
3. Select the account for which you want to change the password, and select
Properties from the User menu.
The User Properties dialog is displayed.
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4. If the Password fields are available, enter and confirm the new password.
5. If the Password fields are unavailable, administrative privileges are required to
change the password for the selected account.
Security Manager Toolbar
The toolbar displayed at the top of the Security Manager dialog contains the tool
buttons listed below. The tool button functions are duplicated in the Security menus.
Creates a new user.
Creates a new group.
Copies the currently selected group or user account.
Deletes the currently selected group or user account.
Edits the currently selected group account or user properties.
Reviews the user account policy options.
Reviews the group access rights.
Reviews the audit policy options.
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Setting up an Account Policy
Before you create a user account or group, you must specify an account policy to
establish the password restrictions and the policy for individual user settings. You
can also enable or disable the TurboMass Security application.
1. Select Account from the Policies menu
Or
Click
to display the Account Policy dialog.
2. Specify account policy by editing the following parameters:
Permit Blank
Password
Creates or modifies a user account to have no
password.
At Least X Characters
Specifies the minimum number of characters
that passwords must contain. This parameter
applies to new user accounts, or to modified
user accounts.
Maintain individual
user settings within
TurboMass
Allows TurboMass to maintain its settings
(parameter values, window positions) on a peruser basis. If this option is not selected, any
changes made within TurboMass affect all
users.
Disable TurboMass
Security
Disables the Security application. If Security is
disabled, no login prompt is displayed, and all
users are logged on with the Administrator
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username and with full administrative
privileges.
In order to disable Security, you must have
administrative privileges, and you must exit
TurboMass.
Creating a User Account
There are two ways to create a user account:
•
Enter the new user information into a new user account.
•
Copy an exiting user account, edit the policy options, and save the account
under a new user name.
Creating a user account
1. Select New User from the User menu
OR
Click
to open the User Properties dialog.
2. Enter the new user information.
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User Name
The name that a user enters to log on to TurboMass.
Full Name
The user’s full name.
Description
A brief user description, for example, position in the
company.
Password
A user’s default password, which a user can later change
(unless User Cannot Change Password is selected).
Confirm
Password
The user must correctly re-enter the default password to
confirm it.
User
Cannot
Change
Password
If selected, the user is not allowed to change their own
password.
Account
Disabled
Disables the account. When selected, the account’s user
name cannot be used to log on to TurboMass, but the
account information remains intact.
Currently
Assigned
Rights
The 1ist of rights that is granted to the current user. This list
depends on the rights that are assigned to the groups to
which the user belongs. When creating a new user (or
copying an existing user), this list is empty and unavailable.
NOTE: A system administrator can change a user’s password at any time.
3. Click OK.
Security adds the new user to the list, unless the name already exists in the list
of users or groups, or the password is too short. See Setting up an Account
Policy on page 679.
OR
1.
Select an existing user from the list in the Security Manager dialog.
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2.
Select Copy from the User menu to open the User Properties dialog, and
enter the new user information.
Security creates a new user with some of the User Properties information
already entered. Until assigned new rights, the new user is a member of the
same groups as the original user.
Creating a Group
When you create a user group, the individual members have those access rights
granted to the group. You can create a new group by adding members as desired, or
you can copy an existing group. Once you have created a group, you will assign
access rights to the group.
Creating a group
1. Create a new group by doing one of the following:
• Click
OR
Select New Group from the User menu to open the Group Properties
dialog.
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• Select an existing group from the list in the Security Manager window, and
select Copy from the User menu to copy the existing group.
When you copy an existing group, the Group Properties dialog contains some of
the information from the copied group, and the new group inherits all the
members and group rights from the copied group.
2. Enter the new group information:
Group Name
The name assigned to a group of users.
Description
A brief description of the group, for example,
department, or tasks performed.
Members
The list of users who belong to a group. The Members
list is empty when you are creating a new group. If you
create a new group by copying an existing group, then
Security copies the list of members from the original
group to the new group.
Currently
Assigned
Rights
The list of rights granted to the current group. When
creating a new group (or copying an existing group),
the list is empty and unavailable.
3. For each member you want to add, click Assign to open the Group Membership
dialog, select the user you want to add from the Non Members list, and click
Add to move the new member to the Members list.
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4. For each user you want to remove, select the user you want to remove from the
Members list, and click Remove to move the selected user from the Members
to the Non Members list.
5. Click OK to return to the Group Properties dialog.
6. Click OK to return to the Security Manager window.
The new group name appears in the list of groups.
Deleting a user account or group
1. To delete a user account or group, select the user or group from the relevant list
in the Security Manager dialog, and select Delete from the User menu.
2. Click OK to confirm the deletion.
Security removes all traces of the user account or group. If you create a
subsequent user or group with the same name, TurboMass treats it as a new user
account or group. For example, you will need to set up group rights and group
membership for the new group.
NOTE: The Administrator user account and the Administrators group cannot be deleted.
Assigning group rights
1. Select Group Rights from the Policies menu
OR
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Click
to open the Group Rights Policy dialog.
The dialog lists the group(s) that have access to the currently selected right.
Right
A group of access privileges that can be granted to groups.
The Administer User Accounts and Groups right refers to the
various tasks performed within the Security Manager, any
group granted this privilege can modify user accounts and
groups, and perform policy changes (such as changing group
rights). This right should only be assigned to groups that
require administrative privileges.
Grant To
The list of groups that have the currently selected right.
2. From the Right drop-down list, select the right you want to assign to the group.
3. To grant the selected right to a new group, click Assign to open the Group
Right Assignment dialog, select the group in the Non Members list, and click
Add to move the new group to the Members list.
Security moves the selected group to the Members list.
Repeat step 3 for each group to be granted a new access right.
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4. To remove a group from the Members list, select the group you want to remove,
and click Remove to move the selected group to the Non Members list.
The Administrators group cannot be removed from the Members list of any
group because administrators must have full access rights.
Assigning an access privilege to an individual user
1. Follow the procedure Creating a Group on page 682 to create a special group
for the user, and make the user a member of the new group.
2. Assign the access privilege to that group using the procedure Assigning group
rights on page 684.
Managing the Audit Log
The audit log maintains an audit trail of the TurboMass use by tracking each
occurrence of each auditable event specified in the Audit Policy. You can set up the
Security Audit policy from the Audit Policy dialog. You can monitor the audit log
from the Audit Log Viewer.
Setting up an audit policy
1. From the Security Manager window, click
OR
Select Audit from the Policies menu.
The Audit Policy dialog is displayed.
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2. Select the auditable events that you want to monitor in the audit log, and specify
the event log settings.
Enable audit trails
When selected, audit information is written to the
audit log. Deselecting this checkbox disables the
audit log, and the audit log is not updated when
an auditable event occurs.
Auditable events
The auditable events checkboxes determine
which event types are written to the audit log file.
Maximum List
Entries
Use this field to specify the maximum number of
entries allowed in the audit log. After the
specified number of entries is reached, the
Overwrite events as needed setting
automatically takes effect.
Overwrite events as
needed
If selected and the number of list entries exceeds
the Maximum List Entries specified, then
Security replaces older entries with newer ones,
as necessary. If not selected, new entries are not
added after the Maximum List Entries value is
reached.
Monitoring audit log
1. From the Security Manager window, select Audit Log Viewer from the Tools
menu.
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The Audit Log Viewer dialog is displayed.
The Audit Log Viewer displays the audit log that lists the date and time of each
auditable event. The Source column shows the type and a brief description of
each event.
2. Manage the audit log from the Audit Log Viewer dialog Log and View menus:
Log
Clear All Events
Select to completely clear the audit log. Do this
periodically because a very large audit log may slow
TurboMass processing.
View
688
Newest First
When selected, displays the most recent event first.
Oldest First
When selected, displays the events in order of
occurrence - the first event in the list is the oldest.
Detail
Displays detailed information about a selected Audit
Log entry.
Appendix A TurboMass Security
Refresh
Reopens the Audit Log.
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690
Appendix B
TurboMass
Software Installation
TurboMass Software User’s Guide
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Appendix B TurboMass Software Installation
TurboMass Software Installation
IMPORTANT: The computer on which you are installing the TurboMass Software must have the
English version of Windows XP with Service Pack 2 installed as the operating system.
The TurboMass software is preloaded on your system by your Service Engineer; however,
there may be a time when you need to reinstall the software or upgrade from a previous
version. This procedure describes how to upgrade or reinstall the TurboMass software. If you
have any questions, or you need to re-configure the Ethernet communications to the mass
spectrometer, please contact your local PerkinElmer Service Representative.
During the installation you will be prompted to do the following:
• Confirm the installation directory.
• Confirm your setup options.
• Confirm your instrument pre-configuration options.
IMPORTANT:
Before installing TurboMass v5.4, first uninstall any existing TurboMass, Communiqué, and
MATLAB programs using the Add/Remove Programs function in the Windows XP Control Panel.
When installing TurboMass v5.4, it will automatically detect a Communiqué 1.x database from
TurboMass v5.0 and export those templates to c:\turbomass\c1ExportedTemplates directory. After
installing v5.4 you can go to that directory and import the templates. Upgrading from TurboMass
v5.1, 5.2, or v5.3 will save a backup copy of your templates database.
We strongly recommend that you manually export all user-modified templates from TurboMass
to your hard drive using the Communiqué Utilities or the Communiqué Report Creator
(Template Designer), before uninstalling TurboMass v5.0, v5.1, v5.2, or v5.3.
After installing TurboMass v5.4 use the Communiqué Utilities or the Communiqué Report Creator
to Import the templates into v5.4. All PerkinElmer v5.0, v5.1, v5.2 and v5.3 TurboMass templates
have been updated in v5.4, so do not import your modified templates using the same names.
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TurboMass Software User’s Guide
Installation Summary
1. Uninstall the previous version of TurboMass 5.x software and all its components.
2. Install the TurboMass v5.4 software.
3. Reboot the Clarus MS.
4. Install Clarus MS NIST/EPA/NIH Library (2002 or 2005)
5. Configure TurboMass for GC control.
Uninstalling the TurboMass Software and all of its
Components
1. From the Windows XP desk top click on Control Panel.
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Appendix B TurboMass Software Installation
The Control Panel dialog appears:
2. Click on Add or Remove Programs.
The Add or Remove Programs dialog appears:
3. On the Add or Remove Programs dialog select TurboMass Ver5.X and click on
Change\Remove.
The Uninstall shield loads. Do not click Cancel unless you want to halt the installation.
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TurboMass Software User’s Guide
The following appears:
4. Click on OK to start the software removal.
The following appears:
5. Click on OK a second time to confirm.
The following appears:
Then, the LCD Stops if running and the following appears:
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Appendix B TurboMass Software Installation
Uninstall continues (this may take several min).
The following appears:
6. (Click the check Box) and Click on Yes.
The following appears:
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TurboMass Software User’s Guide
7. Click on OK.
The following appears:
8. Click on Finish.
9. On the Add or Remove Programs dialog select Communiqué 2.3 Customer Edition
and click on Remove.
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Appendix B TurboMass Software Installation
The following appears:
10. Click on Yes.
The following appears:
Uninstall runs when complete uninstall MatLab.
11. On the Add or Remove Programs dialog select MATLAB Component Runtime and
click on Remove.
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TurboMass Software User’s Guide
The following appears:
12. Click on Yes.
The following appears:
MATLAB is removed.
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Appendix B TurboMass Software Installation
13. Delete the Desktop icon.
14. Reboot the computer.
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TurboMass Software User’s Guide
Installing the TurboMass Software
1. Verify that all pre-installation tasks are done. See the IMPORTANT information on
the first page of this section.
2. Save all data and close all Windows programs.
3. Insert the TurboMass compact disk in the CD-ROM drive.
The installation program automatically starts and guides you through the installation
process with a series of dialogs that prompt you for your choices. The following three
buttons are always displayed at the bottom of each setup dialog:
• Back — Go to the previous screen.
• Next — Go to the next screen.
Click this button when you have completed a dialog.
• Cancel — Stop the installation process and quit the setup program.
The rest of this procedure describes the TurboMass installation process and shows the
corresponding screens. The installation process begins automatically with the Software
License Agreement.
4. Click Yes to accept the agreement or click No to cancel the setup procedure.
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Appendix B TurboMass Software Installation
After clicking Yes the Instrument Selection dialog displays.
After selecting your Mass Spectrometer, click Next and a screen appears for you to
verify that your mass spectrometer is one of those listed.
Selecting the Clarus 600, Clarus 560 D, or Clarus
500 with (A) inside the door displays this screen.
Selecting the Clarus 500 without (A) inside the
door or TurboMass Gold displays this screen.
5. Click Next to proceed with the installation.
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TurboMass Software User’s Guide
The Install Shield Welcome dialog displays:
6. Click Next.
The Destination Location screen appears.
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Appendix B TurboMass Software Installation
7. Accept the default directory by clicking Next.
If TurboMass software had previously been installed, the install wizard next prompts to
delete any existing security information. Click Yes to continue and delete any previous
password information. Clicking No will save any previous password.
The Installation Options Summary dialog opens. This dialog allows you to review
your setup choices before the installation process begins.
8. Click Next to continue the installation.
The Administrator Account Setup dialog appears:
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TurboMass Software User’s Guide
You can either create a password here or leave both boxes blank for no password.
NOTE: If the password is forgotten, the software will have to be reinstalled! Remember your
password.
9. Click OK to continue the installation.
TurboMass starts installing.
10. The .NET Framework also starts to setup.
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Appendix B TurboMass Software Installation
11. Click OK and the following appears:
12. Click I accept to start installing the .NET Framework.
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TurboMass Software User’s Guide
When complete the following appears:
13. Click OK.
If any Communiqué Reporting templates had been stored from a previous version of
TurboMass software, the following dialog appears verifying they have been saved:
14. Click OK and the Welcome to the Install Shield Wizard for Communiqué appears:
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Appendix B TurboMass Software Installation
15. Click Next to continue the installation.
The Communiqué License Agreement appears:
After accepting the terms of the license agreement, click Next. The Customer
Information dialog appears:
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TurboMass Software User’s Guide
Select the option “Anyone who uses this computer (all users)”.
16. Enter the requested information and click Next to continue the installation.
The Setup Type dialog appears:
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Appendix B TurboMass Software Installation
17. Select Complete and click Next.
The Ready to Install the Program dialog appears:
18. Click Install to continue the installation.
Communiqué installation begins.
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TurboMass Software User’s Guide
The install process continues until the Install Wizard Complete screen is displayed.
19. When complete, click Finish and start the MATLAB installation.
The MATLAB Component Runtime screen appears:
20. Click Next to continue with the installation.
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Appendix B TurboMass Software Installation
21. Click Next to continue. The Select Installation Folder dialog appears:
NOTE: Do not change the folder path. MATLAB Components only work when MATLAB is
installed in the default path.
NOTE: The default install for MATLAB specifies Just Me. Change the default setting to Everyone
and click Next to continue.
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TurboMass Software User’s Guide
The following dialog appears:
22. Click Next to continue with the installation.
When MATLAB completes, the following dialog appears:
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Appendix B TurboMass Software Installation
23. Click Close, and the following appears:
24. The installation process finishes and prompts to reboot the computer. Leave the "Yes, I
want to restart my computer now." option checked and click Finish.
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TurboMass Software User’s Guide
After the computer reboots, a screen similar to the following appears as TurboMass
registers its components.
When the system restarts, the TurboMass Software 5.4 startup icon
appears on
the desktop.
Turn on the mass spectrometer and wait until the front panel light is a blinking green.
Double click on the TurboMass icon and then pump down the mass spectrometer. For
more information see the section Vacuum on page 108
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Appendix B TurboMass Software Installation
Setting the BIOS
Your computer BIOS needs to be properly set for TurboMass.
To set up the computer BIOS for TurboMass, follow this procedure:
1. Turn on (or restart) your computer.
2. When the blue DELL™ logo appears, press F2 immediately.
If you wait too long and the operating system logo appears, continue to wait until you
see the Microsoft Windows desktop. Then shut down your computer and try again.
The system setup screen displays current or changeable configuration information for
your computer. Information on the screen is divided into three areas: the Options List,
Options Field, and Key Functions.
Options List — this field appears on the left side of the system setup window.
The field is a scrollable list containing features that define the configuration of
your computer, including installed hardware, power conservation, and security
features.
3. Scroll up and down the list by using the up and down arrow keys and press Enter to
expand the option (Performance, Power Management, and Maintenance).
4. Highlight an option setting (for example, Hyper-Threading under the Performance
option). Press Enter to make that selection active and make the following settings in
the Option Field. Use the right- and left-arrow keys to select a setting then press Enter.
Option Field — this field contains information about each option. In this field
you can view your current settings and make changes to your settings.
Option
Setting
Performance
Hyper-Threading
(default is set to on, set to off)
Speed step
(default is set to on, set to off)
Limit CPUID
(off)
HDD Acoustic Mode
(off)
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TurboMass Software User’s Guide
Power Management
Setting
AC Recovery
(off)
Auto Power On
(off)
Auto Power Time
(N\A)
Low power Mode
(off)
Remote Wake Up
(off)
Suspend Mode
(S1)
Maintenance
Setting
Dual Core
(default is set to on, set to off)
SERR DMI
(default is set to on, set to off)
5. Save and exit BIOS settings.
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Appendix B TurboMass Software Installation
Upgrading from v5.3 Using the Service Tool
When upgrading a TurboMass 5.3 version of Clarus 600 or 560 D to TurboMass 5.4 you
will need to re-flash the ICARUS flash memory in the Mass Spectrometer using the
Clarus600 Service Tool. This enables the Mass Spectrometer to properly communicate
with the TurboMass v5.4 software.
To update TurboMass by re-flashing the flash memory:
1. In Windows Explorer open the WinCE directory in the TMGOLD directory.
2. Double click on ServiceTool.exe. The program starts and displays the following:
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TurboMass Software User’s Guide
3. On the back of the Mass Spectrometer locate the label that has the last two segments of
the MAC address for the ICARUS board. Enter the values into the configuration tool.
The Set IP Address will become active.
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Appendix B TurboMass Software Installation
If the Set IP Address does not become active you have entered an incorrect MAC
address. The program will read the address off the ICARUS board as soon as it is
entered on this page.
4. Click on Set IP Address the next message appears.
If more then one network interface card is displayed select the one that you have
configured with the fixed IP address 64.1.2.1 from the software installation procedure.
5. Click on OK.
The service configuration tool will return a status of Received reply.
6. Click on the Install Tab at the top of the screen.
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TurboMass Software User’s Guide
The service configuration tool reads and displays the Package Version from the
ICARUS Update folder on Host computer.
7. Click on Connect.
The button will turn to Disconnect and the next screens will be displayed.
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Appendix B TurboMass Software Installation
8. The IP Connect Status will display Connected from “Computer Name”and
Versions will be displayed.
9. Click on the Download button and the following dialog appears:
10. Click on YES and the download begins.
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TurboMass Software User’s Guide
Progress continues until you see Download complete-flashing (may take up to 3
minutes).
11. Wait until the program completes and displays in the Last Status box Firmware
update done this may take up to 3 minutes to finish.
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Appendix B TurboMass Software Installation
12. Click on the X to close the window and return to the Windows XP desktop. Then
double-click on the TurboMass icon to connect to the instrument.
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TurboMass Software User’s Guide
Installing PerkinElmer NIST/EPA/NIH Library (2002 or 2005)
If the NIST Library is currently installed, you do not need to reinstall. These
instructions are provided for those who have not yet installed NIST.
After installing the TurboMass software, you can install the NIST Library option next. The
NIST Library software is sold and licensed separately from the TurboMass software.
NOTE: Always refer to the Release Notes supplied with the NIST Library for the most up-to-date
information.
The NIST2002 screens are used here for illustrative purposes. The same procedure applies
to NIST2005.
Installing the NIST Library
1. Insert the NIST install CD in the CD-ROM drive.
2. Right-click Start and Explore to use MS Explorer to display the contents of the CD
drive. Click on Setup.exe to begin the install process.
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Appendix B TurboMass Software Installation
The setup splash screen and setup screen are displayed:
3. Click Next> to continue.
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TurboMass Software User’s Guide
4. Click Yes to accept the terms of the licensing agreement and continue.
A screen indicating the install destination folder is displayed:
5. Click Next> to continue, and the software installation process begins.
A prompt next appears to install the NIST search; click Yes.
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Appendix B TurboMass Software Installation
A warning is next displayed reminding the installer to close any open windows when
the installation completes. These windows are left open by the install process and will
cover the final prompt to close the NIST software installation.
NOTE: Be sure to close open windows on the desktop and watch for this prompt at the end of the
installation!
6. Click OK.
The next screen prompts to continue the install process. Installation files are copied on
the hard drive:
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TurboMass Software User’s Guide
7. Click Next> to begin.
The NIST install splash screen is displayed and the install process begins. The next
screen prompts to finish the installation:
8. Click OK. When prompted for the setup type, leave the default Typical checked and
click Next>:
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Appendix B TurboMass Software Installation
9.
The next window displays the default install directories; leave the default options
checked and click Next>:
If the following folders do not exist, the system will prompt to create them:
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10. Click Yes to Confirm each new folder.
The install process will next prompt to search the hard drive for any existing installed
libraries:
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Appendix B TurboMass Software Installation
11. Click Search.
12. The next screen will prompt to connect any libraries found on the drive to the MS
search program. If any libraries are displayed in the list, highlight the libraries that
should be included in library searches, check Copy or Link and click Next> to
continue.
13. A prompt appears for the program folder location. Accept the default entry and click
Next>.
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TurboMass Software User’s Guide
A final review of the install options is displayed:
14. Click Next> to continue.
The installation of the MS Search program begins and runs to completion:
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Appendix B TurboMass Software Installation
15. When the MS Search software install is complete, a screen displays prompting you to
view Read-Me files or launch a search. Check the appropriate box(es) and click Finish.
The installation process completes and closes. Be sure to close all open windows and
find the final prompt screen indicating the install process is complete:
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TurboMass Software User’s Guide
16. Click Finish to close the NIST installation process.
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Appendix B TurboMass Software Installation
Setting Up NIST 2005 in TurboMass
To set up NIST in TurboMass, follow this procedure:
1. Start TurboMass
2. Press F1 to start NIST.
3. Click Yes.
The following dialog appears:
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TurboMass Software User’s Guide
4. Browse to the MSSearch directory located in the NIST05 directory on your C drive
and select it by double-clicking the left mouse button (this will expand its
subdirectories, as shown above).
5. Click OK.
The following appears:
6. Click Yes to run NIST now or No to run it later.
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Appendix B TurboMass Software Installation
Configuring TurboMass for GC Control
Before you begin to use TurboMass for the first time, you must first configure it (or verify
that it is configured) to interact with the Clarus 600 GC (or if you are using the Clarus 560
D MS you will be using the Clarus 500 GC).
After establishing communication between the instruments in the system and creating your
GC method, you can develop your TurboMass method.
The procedure used to configure the GC depends upon whether you are initially
configuring TurboMass for GC control or are making front panel changes to the GC.
•
Initial GC Configuration: To set up the LINK and GC for TurboMass control
for the first time.
•
Reconfiguring the GC: To make front panel or hardware changes to the GC
without changing the LINK configuration. Reconfiguration is also required if
you add an autosampler.
Configuring the GC for the First Time
The following steps summarize the procedure for configuring TurboMass for GC control
the first time:
1. Display the top level (main) window.
2.
Select an interface.
3.
Select Configure from the GC menu.
4.
Verify the Data Acquisition port.
5.
Set the LINK Configuration Options.
6.
Set the GC Configuration Options.
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To configure the Clarus 600 (or Clarus 500) GC:
In the top-level window, Select Inlet Interface from the Configure menu.
1. If the Clarus 600 is not selected (highlighted), click to select it.
2.
Click OK.
All GC commands are accessible from the GC menu in the top-level window. From
this menu you can set up your GC configuration, develop your GC method, work
interactively with the GC, and execute all other GC related procedures.
3.
From the GC menu, select Configure.
The Configuration Editor summary window is displayed. This displays the GC
information that will be defined during configuration.
Instrument
Configuration
information
LINK Box
interface
information
After configuring the GC, the area below the Configuration Editor summary list
displays key GC information. The box on the left contains information about the
LINK interface, which includes the type (model number), EPROM version number,
memory size available in the interface (in bytes), and serial number. The box on the
right contains a summary of the GC configuration.
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Appendix B TurboMass Software Installation
Summary of information displayed on the Configuration Editor window:
Field
Description
Name
The name of the GC.
Type
The GC model or type.
Acq Port
The physical data acquisition port to which the dotLINK (or 600
Series LINK) Interface is connected.
LINK Port
The physical port in the LINK interface to which the GC is
connected.
Configured
Displays YES if you provided all the information needed to
configure the GC. Otherwise, NO is displayed.
IPM
Displays YES if the Instrument Personality Module (IPM) for the
GC has been downloaded. The first time you open this window,
the IPM will not have been downloaded.
4.
From the Configuration Editor window, select Configure from the Instrument menu.
The serial port connected to GC dialog is displayed.
5.
Verify the serial port (in this example, COM1), LINK box connection, and firmware
version.
NOTE: If the mass spectrometer and your computer were configured for COM1, then COM1 is
your serial port.
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TurboMass Software User’s Guide
6. Click on the Query Port for Type button.
The Interface type is displayed in the box.
742
7.
Click the Continue button.
The LINK Configuration dialog with the COM port and instrument name displays.
8.
Select Port A from the LINK Ports and Instruments list:
inst1 is displayed in the box to the right of Port A.
9.
Select the Clarus 600 GC with Autosampler in the Instrument Module list. If you have a
Clarus 500 select all of the Clarus 500 associated selections.
If your Clarus 600 GC has an autosampler, select Clarus 600 GC with Autosampler
even if you won’t be using the autosampler. You can change this setting from the
Method Editor.
Appendix B TurboMass Software Installation
If you make a mistake, click Restart. This disconnects the GC and clears the LINK
port. Clicking Reset clears all the changes to this dialog and returns it to the state it
was in before you opened it.
When the software verifies this connection, a box appears under Configured and a
Configure button appears.
10. In the LINK Configuration dialog, click the Configure button next to the port
selection.
The GC Configuration dialog is displayed.
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TurboMass Software User’s Guide
11. To rename the GC to something other than its default name (inst1), enter the new
name in the Name text box.
This name will appear under the Name field in the Configuration Editor window.
12. Click OK.
A check mark in the LINK Configuration dialog indicates that the GC has been
configured.
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Appendix B TurboMass Software Installation
13. Click Finish.
When you first configure the GC, the following message may display:
14. If the GC is not turned on, turn it on now and then click Yes.
OR
If the GC is connected and turned on, click Yes.
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TurboMass Software User’s Guide
The following message is displayed:
15. Click OK.
The following message is displayed:
16. Click Yes.
The following message is displayed:
17. Click Yes.
The following message is displayed:
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Appendix B TurboMass Software Installation
18. Click Yes.
The following message is displayed:
19. Click Yes.
The following message is displayed:
20. Click Yes.
The following message is displayed:
21. Click Yes.
The following screen is displayed:
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TurboMass Software User’s Guide
22. Select Configure from the Instrument menu.
The following screen is displayed.
23. Click the Query Inst for Config button.
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Appendix B TurboMass Software Installation
The following screen is displayed.
24. Click OK.
The Configuration Editor window is updated and your instrument is now configured
and the GC Configuration screen displays.
25. Click Finish.
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TurboMass Software User’s Guide
26. Close the Configuration Editor by selecting Exit from the File menu.
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Appendix C
TurboMass Quantify
Calculations
TurboMass Software User’s Guide
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Appendix C TurboMass Quantify Calculations
TurboMass Quantify Calculations
Peak Response
There are two main methods of calculating peak response value, these are External
Standard and Internal Standard. The calibration base can be either Area or Height,
the examples below are shown for Area.
External
Peak Response
=
Area
Where:
Area is the area of a peak calculated by peak detection.
Internal
Peak Response
=
Area * AmountI
AreaI
Where:
Area is the area of a peak calculated by peak detection.
AmountI is the given amount of the Internal Standard in the sample
AreaI is the area of the internal standard peak calculated by peak detection.
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TurboMass Software User’s Guide
Calibration Curve Calculations
TurboMass can fit several types of calibration curves which are described below.
Weighted Calibration Curves
Calibration points used when fitting curves can be given a weighted importance, the
larger the weighting the more significant a point is treated when the curve is fitted.
Weighting (wi) of ith calibration point is calculated using one of the following, all
wi are set to 1 for no weighting.
1)
2)
3)
4)
wi
wi
wi
wi
=
=
=
=
yi-1
yi-2
xi-1
xi-2
Where:
yi is Y value ( response ) of ith calibration point
xi is X value ( concentration ) of ith calibration point
Include Origin
If Include Origin is selected as a calibration curve type an extra point with
zero concentration and response is used in the regression. The extra point has
a weighting of 1.
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Appendix C TurboMass Quantify Calculations
Average RF
The calibration curve formed is linear passing through the origin with a
gradient equal to the average response values of the calibration points.
Average RF
=
Swy
Sw
Swy
=
Sw
=
Σ yi * wi
xi
Σ wi
Where:
yi is Y value ( response ) of ith calibration point
xi is X value ( concentration ) of ith calibration point
wi is weighting of ith calibration point, all set to 1 for no weighting.
Linear
The calibration curve is formed by fitting a line using linear regression to a
set of calibration points.
Gradient
Intercept
=
=
Swxy / Swxx
yw,mean - Gradient * xw,mean
Where:
yw,mean
=
Σ yi * wi
Σwi
xw,mean
=
Σ xi * wi
Σwi
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TurboMass Software User’s Guide
Swxy
=
Σ ( xi - xw,mean ) * ( yi - yw,mean )
Swxx
=
Σ ( xi - xw,mean )2
yi is Y value ( response ) of ith calibration point
xi is X value ( concentration ) of ith calibration point
wi is weighting of ith calibration point, all set to 1 for no weighting.
If Force Origin is selected a line with zero intercept is fitted.
Gradient
=
Σ xi * yi * wi
Σ xi2 * wi
Quadratic and Higher Order Curves
TurboMass uses a general Least Squares Fit algorithm to regress a
polynomial of any order against the calibration points. The method used is
outlined below.
Polynomial regression can be described as the fitting of m "independent"
variables (Xj, j = 0 to m-1) to a single "dependent" variable y. i.e.
y = Xb + e
where y is the n x 1 vector containing the n y values (yi), X is the n x m
matrix of x values, (xij), b is the m x 1 vector of regression coefficients (bi),
and e is the n x 1 vector of residuals from the fit to each yi value.
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Appendix C TurboMass Quantify Calculations
The familiar least squares solution for the regression coefficients is given by:
b
=
(X'X)-1X'y
where -1 indicates matrix inverse, and ' indicates matrix transpose.
The above equation can then be solved using Gauss-Jordan elimination.
To implement weighted regression X and y are first multiplied by a diagonal
n x n matrix P ( i.e. X becomes PX and Y becomes PY ), before the above
equation is solved.
where each element (pij) of P is given by:
pij
=
wi1/2
for i = j
pij
=
0
for i <> k
wi is weighting of ith calibration point, all set to 1 for no weighting.
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TurboMass Software User’s Guide
Peak Amount Calculations
User Specified Response Factor
If a user response factor if selected within the quantitation method calibration
curves are not used. The following calculation is performed to obtain peak
amounts.
Amount
=
Peak Response
Response Factor
Where:
Peak Response is the response value calculated for a peak.
Response Factor is user entered response factor for that compound.
Average RF Calibration Curve
Amounts are calculated using an Average RF calibration as follows
Amount
=
Peak Response
Average RF
Where:
Peak Response is the response value calculated for a peak.
Average RF is average response factor calculated for a set of calibration
points.
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Appendix C TurboMass Quantify Calculations
Linear Calibration Curve
Amounts are calculated using a linear calibration as follows
Amount
=
Peak Response - Intercept
Gradient
Where:
Peak Response is the response value calculated for a peak.
Intercept is the intercept calculated for the linear calibration.
Gradient is the gradient calculated for the linear calibration.
Quadratic and Higher Order Calibration Curves
Amounts are calculated by solving the following equation using the NewtonRaphson Method.
Peak Response
=
P ( Amount )
Where:
Peak Response is the response value calculated for a peak.
P( ) is the polynomial function calculated for a set of calibration points.
User Parameters
User parameters can be used to multiply or divide the final quantitation
results. These factors are entered per sample in the Sample List. If a factor is
not specified of zero it is assumed to be one.
Final Amount = Amount * Dilution Factor * Extract Volume * User Factor
Initial Amount * Injection volume
The User Peak Factor is entered per compound in the Quantify Method.
Final Amount =
Amount * User Peak Factor
759
TurboMass Software User’s Guide
Calibration Curve Statistics
Coefficient of Determination
The coefficient and determination is calculated for a regressed calibration curve. In
the case of a linear unweighted curve it is equivalent to the square of the correlation
coefficient and is reported as such. Correlation coefficients are not a valid statistic
for any other type of regressed curve.
For each data point a value of y (yi,pred) can be predicted from the calibration curve
at the position xi. For each data point a residual between the actual and predicted y
value can be calculated as ( yi - yi,pred), and the residual sum of squares (RSS) can
be calculated as:
RSS
=
Σ (yi - yi,pred)2
The total variation in the data is reflected in the corrected sum of squares (CSS),
calculated as:
CSS
=
Σ (yi - ymean)2
where ymean is the mean value of y.
The model sum of squares (MSS) is the portion of the total variation accounted for
by the regression, i.e.
MSS =
CSS - RSS
The coefficient of determination (r2) is the proportion of the variation accounted for
by regression, and is given by the ration of the model sum of squares to the
corrected sum of squares, i.e.
r2
760
=
=
MSS / CSS
( CSS - RSS ) / CSS
Appendix C TurboMass Quantify Calculations
Curve Correlation Coefficient
The correlation coefficient is only a valid statistic of fit for regressed unweighted
linear curves. In this case the square of the correlation coefficient is equivalent to the
coefficient of determination described above.
Internal
Peak Response
=
Area * AmountI
AreaI
Where:
Area is the area of a peak calculated by peak detection.
AmountI is the given amount of the Internal Standard in the sample
AreaI is the area of the internal standard peak calculated by peak detection.
761
Appendix D
Sample and Compound
Table Output Fields
Appendix D Sample and Compound Table Output Fields
Compound and Sample Report Output Fields
The following table describes each output field and format. The two columns on the
right specify whether the field is available in the Compound Report (C) and/or
Sample Report (S).
Field Name
Field ID
Format
Description
Format
C S
Acquired Date
RAW_DATE
C9
Date raw data acquired
DD-MMM-YY
●
Acquired Time
RAW_TIME
C8
Time raw data acquired
HH:MM:SS
●
Blank Sub. Conc.
Concentration found in Blank which is
subtracted from final Concentration
● ●
Calibration Date
CDB_DATE
C9
Date Quantify Calibration last modified
Calibration File
CDB_NAME
C8
Name of Quantify Calibration file used to
quantify peak; excludes extension
Calibration Time
CDB_TIME
C8
Time Quantify Calibration last modified
Trace
QUAN_TRACE
C 40
Raw data file chromatogram integrated to
produce peak. A chromatogram description
can consist of 'TIC', 'BPI', mass or mass range.
To add or subtract chromatograms use '+' and
'-' operators
● ●
% error from standard concentration
100*(Conc-StdConc)/StdConc
● ●
Peak integration description flags: 1st
character= baseline start, 2nd = baseline end
●
Concentration
Deviation
Pk Flags
PK_FLAGS
C4
DD-MMM-YY
● ●
● ●
HH:MM:SS
● ●
b = starts/ends on chromatogram curve
v = starts/ends as valley dropline between two
peaks
s = starts/ends as a shoulder dropline between
two peaks
t = perk was not detected within the retention
time window
M = manually defined by user
Found Peak Scan
Injection Volume
IS Area
INJ_VOL
N 19.9
Scan number of the peak apex
●
Injection volume of sample, currently set-up to
1. Set during Quantify Locate processing,
otherwise is 0
●
Area of internal standard compound
● ●
765
TurboMass Software Guide
766
IS Compound #
Compound reference number of internal
standard
● ●
IS Found RT
Found retention time of internal standard
compound
● ●
IS Height
Height of internal standard compound
● ●
Modified Date
MOD_DATE
C9
Date peak baseline last manually modified
DD-MMM-YY
● ●
Modified Time
MOD_TIME
C8
Time peak baseline last manually modified
HH:MM:SS
● ●
Modify Comment
MOD_TEXT
C 40
Modification description entered for last peak
baseline modification
● ●
Modify User
MOD_USER
C 16
Name of user who last manually modified
peak baseline. This is the user login name
● ●
Peak Height
Height of the target compound
● ●
Peak Mass
Unused
● ●
Predicted RRT
Calculated relative retention time
●
Predicted RT
Compound retention time from Quantify
Method
●
Sample
CONDITIONS
Char
(255)
Condition information from Sample List.
Recorded in data file header
●
Sample TASK
Char
(50)
Task description from Sample List. Recorded
in data file header
●
Sample Text
(FILE_TEXT)
Char
(255)
Sample text description from Sample List.
Recorded in data file header
●
USER_DIVISOR_1
Double
Divisor used during concentration calculation
stage of Quantify. Defaults to 1 if not specified
●
USER_FACTOR_1
…
USER_FACTOR_3
Double
Multipliers used during concentration
calculation stage of Quantify. Defaults to 1 if
not specified
●
User Peak Factor
User Peak Factor set in the Quantify method
● ●
User Peak RF
User RF Value set in the Quantify method
● ●
Appendix D Sample and Compound Table Output Fields
Version
Added
Field Name
Format
Description
PKAREAPER
N 10.2
NPKAREPER
N 10.2
Quantify Mass chromatogram Integrated Peak Area
Normalized Quantify Mass chromatogram
Integrated Peak Area
5.0
QNTRATIO
N 19.9
Quantify Mass chromatogram Ratio to Largest Peak
area
5.0
QNTLOWLIM
N 19.9
Quantify Mass chromatogram Ratio Low Limit
5.0
QNTHIGLIM
N 19.9
Quantify Mass chromatogram Ratio High Limit
5.0
QNTPERTOL
N 19.9
Quantify Mass chromatogram Ratio % Tolerance
5.0
QNTMLTPAS
L
TRUE if within the limits
5.0
ION1MASS
N 10.2
5.0
ION1RT
N 8.3
ION1AREA
N 16.3
ION1HEIGHT
N 12
ION1_ST_RT
N 8.3
ION1_EN_RT
N 8.3
ION1_ST_HT
N 12
ION1_EN_HT
N 12
Qualifier Ion #1 Mass
Qualifier Ion #1 Mass Chromatogram Peak Top
Retention Time
Qualifier Ion #1 Mass chromatogram Integrated
Peak Area
Qualifier Ion #1 Mass chromatogram Integrated
Peak Height
Qualifier Ion #1 Mass chromatogram Integrated
Peak RT of Baseline Start
Qualifier Ion #1 Mass chromatogram Integrated
Peak RT of Baseline End
Qualifier Ion #1 Mass chromatogram Integrated
Peak Height of Baseline Start
Qualifier Ion #1 Mass chromatogram Integrated
Peak Height of Baseline End
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
ION1RATIO
N 19.9
Qualifier Ion #1 Ratio
5.0
ION1LOWLIM
N 19.9
Qualifier Ion #1 Ratio Low Limit
5.0
ION1HIGLIM
N 19.9
Qualifier Ion #1 Ratio High Limit
5.0
ION1PERTOL
N 19.9
Qualifier Ion #1 Percent Tolerance
5.0
ION1PASS
L
TRUE if within the limits
5.0
ION2MASS
N 10.2
5.0
ION2RT
N 8.3
ION2AREA
N 16.3
ION2HEIGHT
N 12
ION2_ST_RT
N 8.3
Qualifier Ion #1 Mass
Qualifier Ion #1 Mass Chromatogram Peak Top
Retention Time
Qualifier Ion #1 Mass chromatogram Integrated
Peak Area
Qualifier Ion #1 Mass chromatogram Integrated
Peak Height
Qualifier Ion #1 Mass chromatogram Integrated
Peak RT of Baseline Start
5.0
5.0
5.0
5.0
767
TurboMass Software Guide
768
Field Name
Format
ION2_EN_RT
N 8.3
ION2_ST_HT
N 12
ION2_EN_HT
N 12
Description
Qualifier Ion #1 Mass chromatogram Integrated
Peak RT of Baseline End
Qualifier Ion #1 Mass chromatogram Integrated
Peak Height of Baseline Start
Qualifier Ion #1 Mass chromatogram Integrated
Peak Height of Baseline End
Version
Added
5.0
5.0
5.0
ION2RATIO
N 19.9
Qualifier Ion #1 Ratio
5.0
ION2LOWLIM
N 19.9
Qualifier Ion #1 Ratio Low Limit
5.0
ION2HIGLIM
N 19.9
Qualifier Ion #1 Ratio High Limit
5.0
ION2PERTOL
N 19.9
Qualifier Ion #1 Percent Tolerance
5.0
ION2PASS
L
TRUE if within the limits
5.0
ION3MASS
N 10.2
5.0
ION3RT
N 8.3
ION3AREA
N 16.3
ION3HEIGHT
N 12.2
ION3_ST_RT
N 8.3
ION3_EN_RT
N 8.3
ION3_ST_HT
N 12
ION3_EN_HT
N 12
Qualifier Ion #1 Mass
Qualifier Ion #1 Mass Chromatogram Peak Top
Retention Time
Qualifier Ion #1 Mass chromatogram Integrated
Peak Area
Qualifier Ion #1 Mass chromatogram Integrated
Peak Height
Qualifier Ion #1 Mass chromatogram Integrated
Peak RT of Baseline Start
Qualifier Ion #1 Mass chromatogram Integrated
Peak RT of Baseline End
Qualifier Ion #1 Mass chromatogram Integrated
Peak Height of Baseline Start
Qualifier Ion #1 Mass chromatogram Integrated
Peak Height of Baseline End
ION3RATIO
N 19.9
Qualifier Ion #1 Ratio
5.0
ION3LOWLIM
N 19.9
Qualifier Ion #1 Ratio Low Limit
5.0
ION3HIGLIM
N 19.9
Qualifier Ion #1 Ratio High Limit
5.0
5.0
5.0
5.0
5.0
5.0
5.0
5.0
ION3PERTOL
N 19.9
Qualifier Ion #1 Percent Tolerance
5.0
ION3PASS
L
TRUE if within the limits
5.0
ION4MASS
N 10.2
5.0
ION4RT
N 8.3
ION4AREA
N 16.3
ION4HEIGHT
N 12.2
ION4_ST_RT
N 8.3
Qualifier Ion #1 Mass
Qualifier Ion #1 Mass Chromatogram Peak Top
Retention Time
Qualifier Ion #1 Mass chromatogram Integrated
Peak Area
Qualifier Ion #1 Mass chromatogram Integrated
Peak Height
Qualifier Ion #1 Mass chromatogram Integrated
Peak RT of Baseline Start
5.0
5.0
5.0
5.0
Appendix D Sample and Compound Table Output Fields
Field Name
Format
ION4_EN_RT
N 8.3
ION4_ST_HT
N 12
ION4_EN_HT
N 12
Description
Qualifier Ion #1 Mass chromatogram Integrated
Peak RT of Baseline End
Qualifier Ion #1 Mass chromatogram Integrated
Peak Height of Baseline Start
Qualifier Ion #1 Mass chromatogram Integrated
Peak Height of Baseline End
Version
Added
5.0
5.0
5.0
ION4RATIO
N 19.9
Qualifier Ion #1 Ratio
5.0
ION4LOWLIM
N 19.9
Qualifier Ion #1 Ratio Low Limit
5.0
ION4HIGLIM
N 19.9
Qualifier Ion #1 Ratio High Limit
5.0
ION4PERTOL
N 19.9
Qualifier Ion #1 Percent Tolerance
5.0
ION4PASS
L
TRUE if within the limits
5.0
CLSTMULTRT
L
TRUE if this is the closest Peak to the Retention
time (that does not pass the ratio tests
5.0
DATASOURCE
N2
INVALIDCNC
EPA_CONC
5.1
L
0 = MS, 1 = GC CHAN1, 2 = GC CHAN2
TRUE if there was something wrong with the
internal standard data
N 29.9
Adjusted Concentration
5.2
5.1
SPIKERECOV
N 19.9
Matrix Spike / Matrix Spike Duplicate Recovery
5.2
RPD
N 19.9
Relative Percent Difference
5.2
MATRIXTYPE
N 1
0 = Soil, 1 = Water
5.2
EPAQUALTXT
C 11
EPA Qualifier Ions
5.2
EPA_MCONC
N 29.9
Moisture Adjusted Concentration
5.2
GOODEPACAL
N 10
Bit Fields 1 if valid/operation performed, 0 if not
Valid Adjusted Concentration
0x00000001
Valid Moisture Adjusted Concentration 0x00000002
Valid Matrix Spike Recovery
0x00000004
Valid Matrix Spike RPD
0x00000008
EPA FLAG Manually Changed
0x00000010
5.2
769
TurboMass Software Guide
Sample List Data File Structure
The TurboMass Sample List files are used to store information about batches of
samples that are to be processed by the system. They are mainly used for sample
acquisition and compound quantification purposes.
The Sample Lists are held in Microsoft Access which means their contents are
readily available to numerous other windows programs. It also provides flexibility
for future expansion. Sample Lists created by the TurboMass system have the .SPL
extension.
The Sample List database is stored in Microsoft Access format. The Format fields
below give the type and, if necessary, size of each field.
770
Field Name
Format
Description
VERSION
Long int
Database version number. Current version is 1.
Index
Double
Used internally to keep samples sequenced when
editing
FILE_NAME
Char (255)
Raw data file name for this sample. Can be name or full
path.
MS_FILE
Char (255)
MS method parameter file to use when acquiring this
sample. Can be name or full path.
MS_TUNE_FILE
Char (255)
MS tuning parameter file to use when acquiring this
sample. Can be name or full path. If empty the current
tune settings will be used.
INLET_FILE
Char (255)
Inlet method parameter file to use when acquiring this
sample. Can be name or full path. Only required if a
programmable inlet acquisition system is being used to
acquire sample.
INLET_PRERUN
Char (255)
Not currently used, reserved for future use.
INLET_POSTRUN
Char (255)
Not currently used, reserved for future use.
INLET_SWITCH
Char (255)
Clarus/AutoSystem GC injector port ("A" or "B").
AUTO_FILE
Char (255)
Not currently used, reserved for future use.
SAMPLE_LOCATION
Char (50)
Defines location of sample to be acquired on
autosampler bed. Format will depend on type of
autosampler being used. (Clarus/AutoSystem Vial
number).
Appendix D Sample and Compound Table Output Fields
INJ_VOL
Double
Volume of sample to inject when acquiring with
programmable autosampler. Clarus/AutoSystem
volume is controlled by GC method. This field is thus
for information only and does not control injector.
PROCESS
Char (255)
External process to run to perform processing of sample.
Can be name or full path. Only required if external
processes are being run, if empty no process will be run
for this sample.
PROCESS_PARAMS
Char (255)
Name of external process parameter file to use when
processing samples. Available to external process via
MLCURSMP.TXT file.
PROCESS_OPTIONS
Char (255)
Options to specify on command line of external process
when it is executed.
FILE_TEXT
Char(50)
Sample text description to be used for sample. Will be
recorded in data file header.
JOB
Char(50)
Job description for sample. Will be recorded in data file
header.
TASK
Char(50)
Task description for sample. Will be recorded in data
file header.
USER
Char(50)
User name for sample. Will be recorded in data file
header.
SUBMITTER
Char(50)
Submitter for sample. Will be recorded in data file
header.
CONDITIONS
Char (255)
Condition information for sample. Will be recorded in
data file header.
TYPE
Char (50)
Sample type use during Quantify. Currently can be one
of ANALYTE, ANALYTE DUP, BLANK, QC,
STANDARD, TUNE EVAL, INIT CALIB, CONT
CALIB, METH BLANK, LAB CONTROL, SPIKE,
SPIKE DUP, DILUTION or RE-EXTRACT.
CONC_A … CONC_T
Char (50)
20 fields used to specify the concentration levels of
compounds within this sample. Used during the quantify
process.
TYPE_ANALYSIS
Char (255)
Analysis type used during environmental processing.
Currently can be one of Volatiles, Semi-volatiles or
QA/QC.
CASE_NUMBER
Char (255)
Sample analysis case number.
CONC_EXTRACT_VOL
Double
The volume of the extract concentration.
CONTRACT
Char (255)
Identifier of the sample analysis contract.
DECANTED
Char (255)
Description of whether or not the sample was decanted.
DILUTION_FACTOR
Double
The dilution factor to be used in adjusting the analyte
concentrations.
771
TurboMass Software Guide
772
EPA_SAMPLE_NUMBER
Char (255)
EPA number of the sample.
EXTRACTION_DATE
Char (255)
The date the sample was extracted.
EXTRACTION_TYPE
Char (255)
The type of the extraction performed.
GC_COLUMN
Char (255)
Description of the column type used for this sample’s
analysis.
GPC_CLEANUP
Char (255)
String description of whether or not GPC cleanup was
used for this sample.
CLEANUP_DESCR
Char (255)
Description of the cleanup procedure.
HEAT_PURGE
Char (255)
Description of whether or not heated purge was used for
this sample.
LABORATORY_CODE
Char (255)
Laboratory code description.
CONC_LEVEL
Char (255)
Concentration level of sample. Currently can be either
Low or Medium.
MATRIX
Char (255)
Matrix type used during environmental processing.
Currently can be either Soil or Water.
PERCENT_MOISTURE
Double
The moisture content of the soil sample.
PH
Double
The pH of the sample.
RECEIVED_DATE
Char (255)
The date the sample was received.
SAMPLE_WEIGHT_VOLUME
Double
The amount of sample analyzed.
SAS_NUMBER
Char (255)
Special Analytical Services number.
SDG_NUMBER
Char (255)
Sample Delivery Group number.
SOIL_ALIQUOT_VOLUME
Double
The volume of the aliquot of the sample methanol
extract.
SOIL_EXTRACT_VOLUME
Double
The total volume of the methanol extract.
SURROGATE_LOT_NUMBER
Char (255)
Lot number of the surrogate standard used.
ISTD_LOT_NUMBER
Char (255)
Lot number of the internal standard used.
VOLUME_SURROGATE_ADDED
Double
The volume of the surrogate standard added to the
sample.
FRACTION_MASS
Char (50)
Not currently used, reserved for future use.
STOCK_DIL
Double
Not currently used, reserved for future use.
USER_DIVISOR_1
Double
Divisor used during concentration calculation stage of Qua
Defaults to 1 if not specified.
USER_FACTOR_1
Double
Multiplier used during concentration calculation stage of
Quantify. Defaults to 1 if not specified.
USER_FACTOR_2
Double
Multiplier used during concentration calculation stage of
Quantify. Defaults to 1 if not specified.
Appendix D Sample and Compound Table Output Fields
USER_FACTOR_3
Double
Multiplier used during concentration calculation stage of
Quantify. Defaults to 1 if not specified.
SPARE_1 … SPARE_5
Char (255)
General purpose fields available to the User to store
extra information about the sample.
QUANT_METHOD
Char (255)
Quant method filename used during sample list
processing.
QUANT_CALFILE
Char (255)
Quant calibration file used during sample list
processing.
QUAL_METHOD
Char (255)
Qualitative method filename used during sample list
processing.
REPORT_METHOD
Char (255)
Report Method filename used by the report generator
during sample list processing.
773
TurboMass Software Guide
774
Appendix E
LIMS Import File
Example
Appendix E LIMS Import File Example
Example of a Sample List Import File
[System Description]
Description=EXAMPLE SIF FILE
MaxNoOfSamples=250
[Constant Parameters]
BatchID=InitialCalibration (Sample List Filename)
(From the list below build a cross reference map relating the items in the Data
section to Sample list entries. Build a new INTERNAL Sample record and append it
to the newly created sample list file.)
[Variable Parameter List]
NumberOfParameters=56
Parameter1=FILE_NAME
Parameter2=FILE_TEXT
Parameter3=MS_FILE
Parameter4=MS_TUNE_FILE
Parameter5=INLET_FILE
Parameter6=INLET_PRERUN
Parameter7=INLET_POSTRUN
Parameter8=INLET_SWITCH
Parameter9=AUTO_FILE
Parameter10=PROCESS
Parameter11=PROCESS_PARAMS
Parameter12=PROCESS_OPTIONS
Parameter13=SAMPLE_LOCATION
Parameter14=JOB
Parameter15=TASK
Parameter16=USER
Parameter17=SUBMITTER
Parameter18=CONDITIONS
Parameter19=TYPE
Parameter20=ID
Parameter21=CONC_A
Parameter22=CONC_B
Parameter23=CONC_C
Parameter24=CONC_D
Parameter25=CONC_E
Parameter26=CONC_F
Parameter27=CONC_G
Parameter28=CONC_H
Parameter29=CONC_I
Parameter30=CONC_J
777
TurboMass Software User’s Guide
Parameter31=CONC_K
Parameter32=CONC_L
Parameter33=CONC_M
Parameter34=CONC_N
Parameter35=CONC_O
Parameter36=CONC_P
Parameter37=CONC_Q
Parameter38=CONC_R
Parameter39=CONC_S
Parameter40=CONC_T
Parameter41=FRACTION_MASS
Parameter42=INJ_VOL
Parameter43=STOCK_DIL
Parameter44=USER_DIVISOR_1
Parameter45=USER_FACTOR_1
Parameter46=USER_FACTOR_2
Parameter47=USER_FACTOR_3
Parameter48=SPARE_1
Parameter49=SPARE_2
Parameter50=SPARE_3
Parameter51=SPARE_4
Parameter52=SPARE_5
Parameter53=QUANT_METHOD
Parameter54=QUANT_CALFILE
Parameter55=QUAL_METHOD
Parameter56=REPORT_METHOD
[Variable Parameter Data]
NumberOfDataValues=2
Data1=Filena'me,file"text,MSFile,MsTuneFile,InletFile,InletPreRun,INletPostRun,InletSwitch,
AutoFile,Process,ProcessParam,ProcessOptions,SampleLocation,Job,Task,User,Submitter,C
onditions,Standard,ID,12,1.2,1.3,1.4,1.5,1.6,1.7,1.8,1.9,2.0,2.1,2.2,2.3,2.4,2.5,2.6,2.7,2.8,2.9,3.0,12345.67890,1.25,
1.0,1.0,1.0,2.0,3.0,Spare1,Spare2,Spare3,Spare4,Spare5,QuantMethod,QuantCalfile,QualMe
thod,ReportMethod
Data2=Filename2,filetext2,MSFile2,MsTuneFile2,InletFile2,InletPreRun2,INletPostRun2,InletSwitch2
,AutoFile2,Process2,ProcessParam2,ProcessOptions2,SampleLocation2,Job2,Task2,User2,Submitter2,
Conditions2,Analyte,ID2,22,10.2,10.3,10.4,10.5,10.6,10.7,10.8,10.9,20.0,20.1,20.2,20.3,20.4,20.5,20.6,20.7,20.8,20.9,30.0,222.5
55,2.25,2.5,1.0,2.0,-22.5E.2,32.12E+3,Spare12,Spare22,Spare32,Spare42,Spare52,QuantMethod2,QuantCalfile2,QualMethod2,R
eportMethod2
778
Appendix F
Environmental
Reporting
Calculations
Appendix F Environmental Reporting Calculations
About the Calculations
The calculation of compound concentration to be employed for a given sample will
be determined by the analysis type (VOA or SV – taken from the ‘Analysis’ field in
the sample list), matrix type (water/soil – taken from the ‘Matrix’ field in the sample
list) and concentration level (low/medium – taken from the ‘Level’ field in the
sample list).
This value calculated from the equations below will be included in the data source
as the item under the TargetCompounds() collection (i.e. it will not replace the
standard TurboMass ‘Concentration’ value found in the Quantify view results.
NOTE: The equations below are shown in two forms. Firstly, the form defined in the EPA
methods and/or SOW. The TurboMass software will not perform these calculations
exactly as defined in these equations but will instead derive the ‘environmental
concentrations’ from the concentration value currently calculated and reported. The
secondary calculations required to generate the required ‘environmental
concentration’ value from the current TurboMass concentration are defined in the
equations shown in parenthesis [ ] following the EPA version.
781
TurboMass Software User’s Guide
Volatile Organic Compound Analysis
Water Samples
Concentration (µg/L) =
(Ax) (Is) (Df)
≡
(Xs) (Df)
(where Xs is TurboMass concentration 1 )
(V0)
(Ais) (RRF) (Vo)
where
Area 2 of the characteristic ion (Extracted Ion Current
Ax
profile - EICP) for the compound to be measured – from
integration results
Ais
Area of the characteristic ion (EICP) for the specific
internal standard – from integration results
Is
Amount of internal standard added in nanograms (ng) –
from appropriate Concentration column of the sample list
(as defined in the Quantify Method and the sample list)
RRF
Vo
Df
Average relative response factor from the ambient
temperature purge of the calibration standard – from
calibration file
Volume of water purged in milliliters (mL) – ‘Sample Vol’
from sample list
Dilution factor. The dilution factor for analysis of water
samples for volatiles by this method is defined as the
ratio of the number of milliliters (mL) of water purged
(i.e., Vo above) to the number of mL of the original water
sample used for purging ) – from sample list (Dilution
Factor) – ‘Dilution Factor’ from sample list)
NOTE: For compounds designated as “Surrogate”, the Concentration is calculated without
including the Dilution Factor. This is because in Volatile Analysis the Surrogates
are added following dilution and are therefore not affected by it. The equation
(starting from TurboMass concentration) for Surrogates therefore becomes:
1
Xs is the target concentration amount. This is calculated based on a concentration
entered for the internal standard in the Sample List..
2
"Area" is referenced here, since it is specified by the EPA methods, but the
software will actually use whatever response mode (area or height) is specified in
the Quantify Method. This applies to all the environmental calculation defined in
this document.
782
Appendix F Environmental Reporting Calculations
Concentration (µg/L) =
(Xs)
(Vo)
The average relative response factor ( RRF ) is the average of the relative response
factor values calculated at each calibration level:
Relative reponse factor =
where
Ax
Ais
Cis
Cx
Ax Cis
×
Ais Cx
Area of the characteristic ion (EICP) for the compound to
be measured, in the calibration standard
Area of the characteristic ion (EICP) for the specific
internal standard, in the calibration standard
Concentration of the internal standard in the calibration
standard
Concentration of the compound to be measured, in the
calibration standard
783
TurboMass Software User’s Guide
Soil/Sediment Samples (Low Level)
Concentration (µg/kg) =
(Ax) (Is) (Df)
(Ais) (RRF) (W s) (D)
≡
(Xs) (Df)
3
(where Xs is TurboMass concentration )
(W s)(D)
where
Ax
Ais
Is
RRF
D
Ws
Df
3
Area of the characteristic ion (EICP) for the compound to
be measured – from integration results
Area of the characteristic ion (EICP) for the specific
internal standard – from integration results
Amount of internal standard added in nanograms (ng) –
– from appropriate Concentration column of the sample
list (as defined in the Quantify Method)
Average relative response factor from the heated purge
of the calibration standard – from calibration file
Adjustment for dry weight basis – (100 - %moisture)/100
– calculated from % Moisture value in sample list
Weight of sample added to the purge tube, in grams (g)
– ‘Sample Wt’ from sample list
Dilution factor. [This is not included in the EPA equation
but is being included here for consistency and to avoid
the need for special cases in the software.]
Xs is the target concentration amount. This is calculated based on a concentration
entered for the internal standard in the Sample List.
784
Appendix F Environmental Reporting Calculations
Soil/Sediment Samples (Medium Level)
Concentrat ion (µg/kg) =
(Ax) (Is) (Vt) (1000) (Df)
(Ais) (RRF) (Va) (W s) (D)
≡
(Xs) (Vt) (1000) (Df) (where Xs is TurboMass concentration3 4
(Va) (W s) (D)
)
where
Ax
Ais
Is
RRF
Vt
Va
Ws
D
Df
Area of the characteristic ion (EICP) for the compound to be
measured – from integration results
Area of the characteristic ion (EICP) for the specific internal standard
– from integration results
Amount of internal standard added in nanograms (ng) – from
appropriate Concentration column of the sample list (as defined in
the Quantify Method)
Average relative response factor from the heated purge of the
calibration standard – from calibration file
Total volume of the methanol extract in milliliters (mL) – ‘Soil Extract
Volume’ from sample list
Volume of the aliquot of the sample methanol extract (i.e., sample
extract not including the methanol added to equal 100 µL) in
microliters (µL) added to reagent water for purging – ‘Soil Aliquot
Volume’ from sample list
Weight of soil/sediment extracted, in grams (g) – ‘Sample Wt’ from
sample list
Adjustment for dry weight basis – (100 – %moisture)/ 100 –
calculated from % Moisture value in sample list)
Dilution factor. The dilution factor for analysis of soil/sediment
samples for volatiles by the medium level method is defined as: [(µL
most conc. extract used to make dilution) + (µL clean solvent)] / (µL
most conc. extract used to make dilution)– from sample list (Dilution
Factor) – ‘Dilution Factor’ from sample list
4
Xs is the target concentration amount. This is calculated based on a concentration
entered for the internal standard in the Sample List.
785
TurboMass Software User’s Guide
NOTE: For compounds designated as “Surrogate”, the Concentration is calculated without
including the Dilution Factor. This is because in Volatile Analysis the Surrogates
are added following dilution and are therefore not affected by it. The equation
(starting from TurboMass concentration) for Surrogates therefore becomes:
Concentration (µg/Kg) =
(Xs) (Vt) (1000)
(Va) (W s) (D)
The calculation for results of medium-and high-level soil/sediment volatile organic
analyses preserved with methanol is in accordance with EPA SW-846, published
Method 8000C, Revision 3, 03/03. Water contained in a sample mixes with the
water-soluble methanol preservative to create a greater volume of liquid for
analysis. To account for the dilution effect of the water to the methanol in the
sample, a moisture adjustment must be applied. This will produce a more accurate
quantitation on a sample specific basis for contaminates of concern. This moisture
adjustment is not the same as reporting the data on a dry-weight basis. The data
must also be adjusted to be reported on a dry weight basis.
NOTE: This calculation will only be performed for Analysis=Volatiles, Matrix=Soil,
Level=Medium (and if all required inputs are available).
The total volume of methanol preservative and sample moisture contribution can be
calculated as follows:
Moisture =
wt of sample - wt of dry sample
(100 - Sample % solid)
or
100
wt of sample
Vt = Ve + (Moisture × wt of sample × 1000µL/mL)
where:
Moisture
Vt
Ve
The % Moisture value from the sample list expressed as
a fraction (i.e. % Moisture/100)
Total volume of methanol plus water in the sample
container for analysis
Total extract volume (usually assumed to be only the
volume of methanol)
This adjusted value for Vt will then be used in the equation shown in section
Soil/Sediment Samples (Medium Level), in place of the nominal extract volume.
786
Appendix F Environmental Reporting Calculations
Semi-Volatile Organic Compound Analysis
Water Samples
Concentrat ion (µg/L) =
(Ax) (Is) (Vt) (Df) (GPC)
(Ais) (RRF) (Vo) (Vi)
≡
(Xs) (Vt) (Df) (GPC)
(where Xs is TurboMass concentration 5 )
(Vo) (Vi)
where
Ax
Ais
Is
Vo
Vi
Vt
RRF
GPC
Df
Area of the characteristic ion for the compound to be measured –
from integration results
Area of the characteristic ion for the internal standard – from
integration results
Amount of internal standard injected in nanograms (ng) – from
appropriate Concentration column of the sample list (as defined
in the Quantify Method)
Volume of water extracted in milliliters (mL) – ‘Sample Vol’ from
sample list
Volume of extract injected in microliters (µL) – ‘Injection Volume’
from sample list
Volume of the concentrated extract in microliters (µL) –
‘Concentrated Extract Volume’ from sample list
(If GPC is not performed, then Vt = 10,000 µL. If GPC is
performed, then Vt = 5,000 µL.)
Average relative response factor. – from calibration file
GPC factor – derived from setting in sample list (GPC Y/N)
GPC = 1.0 if water sample was not subjected to GPC;
GPC = 2.0 if water sample was subjected to GPC.
Dilution factor. The dilution factor for analysis of water samples
for semi-volatiles by this method is defined as follows:
[(µL most conc. extract used to make dilution) + (µL clean
solvent)] / (µL most conc. extract used to make dilution)
– ‘Dilution Factor’ from sample list
The calculation applies to water low concentration and multi concentration. The low
concentration calculation will not contain the GPC parameter.
5
Xs is the target amount in nanograms, which assumes that the internal standard
amount is entered as nanograms in the Sample List. If the internal standard
amount is entered as a concentration then the user must enter a user multiplier to
make the necessary correction.
787
TurboMass Software User’s Guide
Soil Sediment Samples
Concentrat ion (µg/kg) =
(Ax) (Is) (Vt) (Df) (GPC)
(Ais) (RRF) (Vi) (W s) (D)
≡
(Xs) (Vt) (Df) (GPC) (where Xs is TurboMass concentration 6 )
(Vi) (W s) (D)
where
Ax
Ais
Is
Vt
Vi
Ws
GPC
RRF
D
6
Area of the characteristic ion for the compound to be measured
– from integration results
Area of the characteristic ion for the internal standard – from
integration results
Amount of internal standard injected in nanograms (ng) – from
appropriate Concentration column of the sample list (as defined
in the Quantify Method)
Volume of the concentrated extract in microliters(µL) –
‘Concentrated Extract Volume’ from sample list)
Volume of the extract injected in microliters (µL) – ‘Injection
Volume’ from sample list
Weight of sample extracted in grams (g) – ‘Sample Wt’ from
sample list
GPC factor – derived from setting in sample list (GPC Y/N)
GPC = 1.0 if water sample was not subjected to GPC;
GPC = 2.0 if water sample was subjected to GPC.
Average relative response factor – from calibration file
Adjustment for dry weight basis – (100 – %moisture)/100 –
calculated from % moisture value in sample list Df Dilution
factor. The dilution factor for analysis of soil/sediment samples
for semi-volatiles by the medium level method is defined as
follows: [(µL most conc. extract used to make dilution) + (µL
clean solvent)] / (µL most conc. extract used to make dilution)
Xs is the target amount in nanograms, which assumes that the internal standard
amount is entered as nanograms in the Sample List. If the internal standard
amount is entered as a concentration then the user must enter a user multiplier to
make the necessary correction.
788
Index
Index
Index
A
account policies, 679
acquisition
from Tune, 115
GC status, 194
MS status, 367
Acquisition
stop, 370
analysis
start, 252, 304
audit log, Security Manager, 686
Auto Refine, 523
AutoBuild, 298
automatic
shutdown, 372
startup, 371
automatic library searching, 430, 512
AutoTune, 100
AutoUltraTune, 95
B
background data files, 482
background subtract
chromatogram, 405
Spectrum, 462
BIOS settings, 717
BPI chromatograms, 389
Browser, Report template, 563, 566
C
calibration
automatic, 125
curve, 316
from data files, 135
high mass, 139
parameters, 124
process, 120
process overview, 122
saving, 148
types, 121
chemical structure, library hit, 520
chromatograms
align, 391
background subtract, 405
BPI, 389
delete displayed, 402
display, 52, 386
integration, 411
magnification ranges, 393
peak annotation, 400
printing, 449
processing, 405
real-time data, 368
real-time display, 403
smoothing, 409
text labels, 403
TIC, 389
clustered data files, 479
Collections, 571
combine
spectra, 460
Combine
data files, 491
functions, 491
output selection, 493
spectra, 425
Communiqué, 21, 571
Concentration Level, 229
configuration
GC options, 159
initial GC, 157
LINK, 159
Configuring the GC, 739
Custom Compounds, 663
D
data
printing, 57
Data Browser, 38
791
data channels, GC, 170
data file, structure, 50
data files
background, 482
clustered, 479
CODA, 480
Combine, 491
delete, 46
enhanced, 477
output, 483
processing, 480
raw, 41
subtracted, 474
Data object Indexing, 588
detection flags, peak, 325
Diffusion pump, 111
E
enhanced data files, 477
Environmental Reporting, 599
equilibration, GC, 191
error messages, GC, 199
F
files, open multiple, 45
filtering, template list, 567
Flash memory, 719
fonts, change, 32
Form 1 Tab – Organics Analysis Data
Sheet, 616
Form 1 TIC Tab – Tentatively Identified
Compounds, 619
Form 2 Tab - SMC/Surrogate Compound
Recovery, 626
Form 3 Tab - Matrix Spike/Matrix Duplicate
Recovery, 628
Form 4 Tab - Method Blank Summary, 630
Form 5 Tab - Instrument Performance
Check, 632
Form 6 Tab – Initial Calibration Data, 634
Form 7 Tab – Continuing Calibration
Check, 637
Form 8 Tab – Internal Standard Area and RT
Summary, 639
Form Specific Checks, 644
Forms Dialog, 601
Forms, Error Messages, 641
Forms, Row Colors, 614
function
add, 208
Combine, 491
list, 210
modify, 208
MS Scan, 211
remove, 208
SIR, 214
solvent delay, 209
start/end, 208
Strip, 473
G
gas controls, 107
GC
acquisition port, 163
acquisition status, 194
configuring, 739
data channels, 170
equilibration, 191
error messages, 199
instrument status, 194
keypad control, 192
method development, 168
modify active method, 201
oven temperature, 175
reconfiguration, 162
run data storage, 171
Run Log, 171
run status, 193
start and stop, 191
status messages, 197
temperature ramp, 175
GC configuration
printing, 167
user options, 164
with TurboMass control, 157
without TurboMass control, 164
GC Configuration Editor, 156
GC menu, 154
GC method
audit trail, 187
carrier parameters, 177
Index
control parameters, 172
descriptive information, 185
detector parameters, 182
instrument timed events, 184
notes, 189
oven/inlet parameters, 174
printing, 190
GC Method Editor, 168
GC status box, 155
Generic TIC Names, 667
group rights, 684
groups, 682
H
Hands On command, 200
headers, 54
help, 59
high mass calibration, 139
Hits chemical structure, 520
hits listing, 515
I
ICARUS, 720
inlet, selection, 69, 153
instrument data thresholds, 70
instrument status, GC, 194
integrating chromatograms, 411
integration parameters, 283
Interactive Data Review, 315
Interface, selecting the GC, 740
IP Address, 720
L
lab and user information, in data file, 78
Lab Infromation, 235
library
append, 527
automated search, 512
print search results, 520
search filters, 508
search parameters, 506
search process, 499
search results, 511
start search, 511
Library Compare, 523
library hits, 515
Library Locator, 532
library search
automatic, 430
Library Subtract, 523
LIMS Sample list
import worksheet, 238
LINK
information, 740
M
MAC Address, 720
magnify chromatograms, 393
magnifying spectra, 444
manual conventions, 22
Map
file, 538
intensity scaling, 545
overview, 537
range, 542
Mapping RT to RRT, 279
mass axis
Spectrum, 444
mass calculator
description, 555
user elements, 556
mass calibration, 119
mass chromatograms
display, 387
mass measure parameters, 131
Matrix, 228
Modify Active command, 201
multiple ion ratios, setting, 281
multiple samples, acquisition, 363
Multiple Solvent Delays, 209
N
Noise Reduction, 409
O
online help, 59
793
output data files, 483
oven temperature, GC, 175
P
password change, 677
peak
centering, 465
detection, 286, 411
detection flags, 325
editing detected, 418
integration, 323
matching, 133
purity, 420
printing active spectrum and
chromatogram, 449
processed data
access, 42
display, 43
processes, external, 35
processing
chromatograms, 405
projects
create, 47
predefined, 47
Q
QA/QC, 227
Qualifiers (Q-Flags), 616
Qualitative Method Editor, 352
quantification process, 268
Quantify
application, 261
calibration curve graph, 316
chromatogram display, 309
integration parameters, 283
manual peak integration, 323
peak list, 320
reports, 328
results, 307
summary results, 311
Quick Paths, 165
R
range
adjustment, 444
defaults, 396, 447
magnification, 393, 445
readbacks, 114
real-time data, 368
reference files, 137
Refine search spectrum, 522
refine spectra, 459
Release Control command, 192
Report Method, 660
Report Method Editor, 559, 560
Toolbar, 561
Report Method Usage, 650
Report Preview Window, 255
Report Template Browser, 563, 566
filtering, 567
toolbar, 567
Report template, new, 580
Reporting Calculations, 781
run status, GC, 193
run, start, 252, 304
S
Sample Information, 231
Sample list
editing, 249
formatting, 241
Sample List Wizard, 225
Sample Prep Infromation, 233
Sample Tracking, 235
scope parameters, 105
Search parameters, 354
Security Manager
account policies, 679
audit log, 686
group rights, 684
groups, 682
logon, 675
password change, 677
tasks, 675
Security Model, 674
serial port, GC, 163
Service Tool, 719
Index
Set IP Address, 720
signal to noise ratio calculation, 422
SIR function, 214
smoothing
spectra, 463
smoothing chromatograms, 409
spectra
display, 51, 443
processing, 458
real-time display, 456
refine, 459
smoothing, 463
Spectra
combine, 460
spectrum
delete displayed, 455
display parameters, 450
list, 448
peak annotation, 453
real-time data, 369
status messages, GC, 197
Strip functions, 473
Submitter/Task Data window, 654
subtracted data files, 474
peak display, 93
Standard (DFTPP/BFB, 95
zero level, 113
Tune Page, 83
TurboMass
Desktop, 30
directory structure, 49
menu commands, 28
quit, 25
system global parameters, 34
window colors and fonts, 31
window commands, 58
TurboMass.ini file, 37
U
user accounts
creating, 680
deleting, 684
user elements, 556
user libraries
append, 527
create, 525
delete entry, 530
index, 529
T
Take Control command, 192
Template, Report Browser, 563, 566
text labels
Spectrum, 456
thresholds
instrument data, 70
TIC chromatograms, 389
transputer thresholds, 70
Tune
Custom (AutoTune), 100
V
vacuum controls, 108
Vacuum system
diffusion pump, 111
Z
zero level, Tune, 113
795
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