TOC-VCPH/CPN & TOC-Control V Software
638-94241A
(M393-E189)
PC-Controlled Total Organic Carbon
Analyzer
TOC-VCPH/CPN &
TOC-Control V Software
User Manual
Read this manual carefully and keep it with the
instrument for future reference.
SHIMADZU CORPORATION
ANALYTICAL & MEASURING
INSTRUMENTS DIVISION
KYOTO, JAPAN
TOC-VCPH/CPN
Copyright  Shimadzu Corporation 2003. All rights reserved, including those to reproduce this publication or
parts thereof in any form without permission in writing from Shimadzu Corporation.
Read and understand this manual before operation. Save this manual.
Information in this publication is subject to change without notice and does not represent a guarantee on the part
of the vendor.
Any errors or omissions which may have occurred in this publication despite the utmost care taken in its production will be corrected as soon as possible, but not necessarily immediately upon detection. We appreciate notification of any errors or omissions.
Shimadzu does not have any responsibility for errors or injuries resulting from following the instructions in this
manual.
Windows is a registered trademark of Microsoft Corporation.
TOC-VCPH/CPN
0
Introduction
Thank you for purchasing the TOC-VCPH/TOC-VCPN Total Organic Carbon Analyzer and
the TOC-Control V software.
This instruction manual is a TOC-V user manual. It provides operation and maintenance
procedures for the TOC-V. The procedures related to TOC-Control V software system
administration are described in detail in the TOC-V Administrator's Manual.
Be sure to read this documentation carefully before using the instrument for the first time.
Read the Operational Precautions before operating the instrument. Follow the procedures in
the manual to avoid compromising user or instrument safety.
CAUTION
•
•
•
Do not operate this instrument before understanding the contents of this manual.
If this manual or the warning labels on the instrument become lost or damaged,
promptly obtain replacements from your Shimadzu representative.
To ensure safe operation, read and follow the procedures in Section 1.2 "Operational Precautions" before operating the instrument.
Product Warranty and Post Sale Service
Product Warranty and Post Sale Service
Product Warranty
The warranty does not cover malfunctions that result from:
• misuse
• repairs or modifications made by any company other than the manufacturer or a
manufacturer-approved company
• external factors
• operation in environments with severe conditions, such as high temperature, high
humidity, corrosive gas, or vibration
• fire, earthquake or other forces of nature
• moving or transporting the unit after its initial installation
• the consumption of items or parts that can be regarded as consumable. For
example, the service life of an LCD display panel depends on actual operating
conditions.
Post Sale Service
If any problems occur with this instrument, inspect it and take appropriate corrective action
as described in Section 5.7 "Troubleshooting". If the problem persists or symptoms not
covered in the Troubleshooting section occur, contact your Shimadzu representative.
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TOC-VCPH/CPN
Contents of This Manual
Contents of This Manual
Chapter 1 Overview
This chapter provides an overview of the instrument and operational precautions for its use.
Chapter 2 System Description
This chapter describes the TOC-V system components and optional accessories.
Chapter 3 Software Overview, Administration, and Setup
This chapter provides an overview of the TOC-Control V software and describes the
software’s Administration and Instrument Setup Wizard tools, which are used to manage
user accounts and configure new systems.
Chapter 4 Operation
This chapter describes pre-analysis preparations and instrument and software functions,
such as setting measurement parameters, starting up the instrument, generating calibration
curves, and conducting sample analysis. This chapter also includes a tutorial that covers
setup and measurement procedures.
Chapter 5 Maintenance
This chapter describes maintenance procedures and periodic checks required to ensure that
the instrument provides consistently high accuracy analyses. Troubleshooting procedures
and error messages are also included in this chapter.
Chapter 6 Reference Information
This chapter describes principles of analysis and lists specifications, standard and optional
accessories, and specialized terms associated with this instrument. This chapter also
includes the installation procedure, for use in the event that instrument is moved to another
site.
Appendix A Method Validation
This appendix describes the software’s Method Validation tool, which is used to test the
variance and linearity of a data set.
Appendix B Control Charts
This appendix describes the software’s Control Charts tool, which is used to monitor the
precision and accuracy of a data set.
TOC-VCPH/CPN
v
Notation Conventions
Notation Conventions
Precautionary Conventions Used in this Manual
The following precautionary conventions are used in this manual.
Convention
Description
CAUTION
Indicates the possibility of slight to moderate injury or equipment damage.
Note:
Provides additional information to ensure the correct use of the instrument.
Other Conventions Used in this Manual
Instrument Model Names
Descriptions in this documentation pertain to two models of the TOC-V Total Organic
Carbon Analyzer, namely the TOC-VCPH and TOC-VCPN. These models will be referred to
in relevant descriptions as the H Type and N Type, respectively.
Supplementary Conventions
In addition to the precautionary conventions, the “Tips” and “Reference” conventions are
used to supply additional information.
Convention
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TOC-VCPH/CPN
Description
TIP »
Indicates a particular technique, alternative means of operation, or useful advice.
Reference:
Indicates a reference location in the manual where more detailed information can
be found.
Warning Labels Used on this Instrument
Warning Labels Used on this Instrument
High Temperature Warning
When the electric furnace is heating up, or is at its operational temperature (680°C or
720°C), the central portion of the electric furnace is extremely hot. To prevent burns,
NEVER touch the electric furnace area with bare hands. Allow the furnace to cool before
performing any maintenance on the combustion tube or catalyst.
The internal temperature of the ozone treatment unit reaches 50°C while the instrument is
running. To prevent burns, switch off the TN unit and wait at least 2 hours for the unit to
cool sufficiently before performing any maintenance.
TOC-VCPH/CPN
vii
Warning Labels Used on this Instrument
Electric Shock Warning
Do not remove this panel, as there is danger of electric shock.
Due to the danger of electric shock, do not remove this cover. In the event that the cover
must be removed, first disconnect the TNM-1 power cord.
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TOC-VCPH/CPN
Warning Labels Used on this Instrument
Injury Warning
The sample injection components of this instrument move during operation. To prevent
injury, keep hands away from this mechanism.
During operation, the pressure in the CO2 absorber of the gas purifier is about 200kPa. To
prevent injuries, turn off the carrier gas and switch off power to the TOC main unit. Wait
until the pressure inside the container and the instrument flow lines return to normal
atmospheric pressure before performing any maintenance.
TOC-VCPH/CPN
ix
Warning Labels Used on this Instrument
Corrosion Warning
Acid and other corrosive substances are present in the liquid waste drained from this
instrument. Be careful not to touch or spill the liquid waste.
The soda lime in the CO2 absorber of the carrier gas purifier is a corrosive chemical
substance. Be careful not to touch or spill this substance.
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TOC-VCPH/CPN
Warning Labels Used on this Instrument
The liquid discharged from the drain tube connected to the TC injector contains acid and
other corrosive substances. Verify that the tip of the drain tube is securely inserted into the
Y-shaped fitting when connecting the combustion tube and sample injector.
The IC reaction solution is acidic. Be careful not to touch or spill the IC reaction solution.
TOC-VCPH/CPN
xi
Warning Labels Used on this Instrument
Hydrochloric acid is a corrosive chemical substance. Be careful not to touch or spill the
hydrochloric acid.
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Table Of Contents
Introduction............................................................................................ iii
Product Warranty and Post Sale Service .................................................... iv
Product Warranty ........................................................................................... iv
Post Sale Service ............................................................................................ iv
Contents of This Manual ............................................................................. v
Notation Conventions ................................................................................. vi
Precautionary Conventions Used in this Manual ........................................... vi
Other Conventions Used in this Manual ........................................................ vi
Warning Labels Used on this Instrument .................................................. vii
1
2
Overview ................................................................................................... 1
1.1
Overview ..................................................................................................... 2
1.2
Operational Precautions............................................................................... 3
System Description................................................................................... 7
2.1
TOC-VCPH/CPN Construction...................................................................... 8
2.1.1
2.1.2
2.1.3
2.1.4
2.1.5
2.1.6
2.1.7
2.2
Autosampler ASI-V (Option) .................................................................... 14
2.2.1
2.2.2
2.3
Front View .................................................................................................... 15
Rear View...................................................................................................... 15
TN Unit TNM-1 (Option).......................................................................... 16
2.4.1
2.4.2
2.4.3
3
Front View .................................................................................................... 14
Rear View...................................................................................................... 14
8-Port Sampler OCT-1 (Option)................................................................ 15
2.3.1
2.3.2
2.4
Front View ...................................................................................................... 8
Right Side View .............................................................................................. 8
Left Side View ................................................................................................ 9
Rear View........................................................................................................ 9
Inside Front View.......................................................................................... 10
Inside Top View............................................................................................ 11
Flow Diagrams .............................................................................................. 11
Front and Right Side Views .......................................................................... 16
Inside Front View.......................................................................................... 17
Rear View...................................................................................................... 18
Software Overview, Administration, and Setup ................................. 19
3.1
Introduction to System Administration Functions.................................... 20
3.1.1
3.1.2
3.1.3
Screen Lock Function ................................................................................... 20
Change Password .......................................................................................... 21
Add Event Log .............................................................................................. 22
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Table Of Contents
3.2
Instrument Setup and System Properties ................................................... 23
3.2.1
3.2.2
3.2.3
3.2.4
3.2.5
3.2.6
3.2.7
3.2.8
3.2.9
4
System Information Window .......................................................................
Options Window...........................................................................................
TOC Window ...............................................................................................
ASI Window.................................................................................................
SSM Window ...............................................................................................
Communication Window..............................................................................
History Function Window ............................................................................
Instrument Properties Dialog Box ................................................................
Removing a Configured System...................................................................
Operation ............................................................................................... 35
4.1
Analysis Preparation .................................................................................. 36
4.1.1
Catalyst Filling .............................................................................................
4.1.1.1 Catalyst for TOC Analysis ................................................................
4.1.1.2 TOC/TN Catalyst (Option) ...............................................................
4.1.2 Connecting the Combustion Tube ................................................................
4.1.3 Installing the Syringe....................................................................................
4.1.3.1 Syringe Pump Zero Point Detection .................................................
4.1.4 Water Supply to the Cooler Drain Container ...............................................
4.1.5 Filling the Humidifier with Water................................................................
4.1.6 Preparation of Dilution Water ......................................................................
4.1.7 Acid Preparation...........................................................................................
4.1.8 Installation of the CO2 Absorber..................................................................
4.1.9 Adjusting Sparge Gas Flow Rate .................................................................
4.1.10 Installing the Suspended Solids Kit..............................................................
4.1.11 IC Analysis Preparations ..............................................................................
4.1.12 Preparation for POC analysis .......................................................................
4.1.13 TN Analysis Preparations.............................................................................
4.1.14 Preparation and Storage of Standard Solutions ............................................
4.1.14.1 Preparation of Standard Solutions.....................................................
4.1.14.2 Storage of Standard Solutions...........................................................
4.1.15 Sample Preparation.......................................................................................
4.1.15.1 High Sensitivity Analysis..................................................................
4.1.15.2 TC Blank Check Analysis.................................................................
4.1.15.3 Pretreatment for IC Removal (Sparging) ..........................................
4.1.15.4 Analysis of Samples Containing Suspended Solids..........................
4.1.15.5 Handling Samples Containing Acids, Bases or Salts........................
4.1.16 Sample Preparation.......................................................................................
4.1.16.1 Vial Types .........................................................................................
4.1.16.2 Filling Vials with Sample..................................................................
4.1.16.3 Placing Vials in the Vial Rack ..........................................................
4.1.16.4 High Sensitivity Autosampler Analysis ............................................
4.1.16.5 Acid Addition in NPOC Analysis .....................................................
4.1.16.6 Sparging in NPOC Analysis..............................................................
4.1.16.7 Stirrer Preparation .............................................................................
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24
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31
32
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66
68
69
71
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72
72
74
75
76
77
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Table Of Contents
4.1.17 8-Port Sampler Measurement........................................................................ 80
4.1.17.1 Type of Sampler Container................................................................ 80
4.1.17.2 High Sensitivity Using the 8-Port Sampler........................................ 82
4.2
Setting General Measurement Parameters................................................. 83
4.2.1
4.2.2
4.2.3
4.2.4
4.3
TOC Parameter Settings................................................................................ 83
ASI Parameter Settings ................................................................................. 84
Setting Default Measurement Parameters..................................................... 87
Maintenance History Settings ....................................................................... 88
Measurement Procedures and Tutorial ...................................................... 89
4.3.1
Starting Up the Instrument ............................................................................ 89
4.3.1.1 Turning on the Power ........................................................................ 89
4.3.1.2 Carrier Gas Pressure .......................................................................... 89
4.3.1.3 Carrier Gas Flow Rate ....................................................................... 90
4.3.1.4 Electric Furnace ................................................................................. 90
4.3.1.5 TN Unit .............................................................................................. 91
4.3.1.6 Ozone Source Airflow Rate for the TN Unit..................................... 91
4.3.2 Tutorial.......................................................................................................... 92
4.3.3 Ending Measurement .................................................................................. 120
4.4
Sample Table Editor ................................................................................ 122
4.4.1
Sample Table Window Overview ............................................................... 122
4.4.1.1 Toolbar Functions ............................................................................ 122
4.4.1.2 Status Bar and Notification Bar ....................................................... 124
4.4.2 File Menu .................................................................................................... 125
4.4.2.1 New.................................................................................................. 125
4.4.2.2 Calibration Curve............................................................................. 126
4.4.2.3 Method Wizard ................................................................................ 135
4.4.2.4 Open................................................................................................. 143
4.4.2.5 Close ................................................................................................ 144
4.4.2.6 Save.................................................................................................. 144
4.4.2.7 Save As ............................................................................................ 145
4.4.2.8 ASCII Export Options ..................................................................... 146
4.4.2.9 Database Export............................................................................... 148
4.4.2.10 Print>Table ...................................................................................... 149
4.4.2.11 Print>Sample Report ....................................................................... 150
4.4.2.12 Print Preview>Table ........................................................................ 150
4.4.2.13 Print Preview>Sample Report ......................................................... 151
4.4.2.14 Print Setup........................................................................................ 151
4.4.2.15 Page Setup........................................................................................ 152
4.4.2.16 Exit................................................................................................... 155
TOC-VCPH/CPN
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Table Of Contents
4.4.3
Edit Menu ...................................................................................................
4.4.3.1 Undo................................................................................................
4.4.3.2 Cut/Copy/Paste................................................................................
4.4.3.3 Replace............................................................................................
4.4.3.4 Find .................................................................................................
4.4.3.5 Exclude............................................................................................
4.4.3.6 Recalculate>All...............................................................................
4.4.3.7 Recalculate>Highlighted.................................................................
4.4.3.8 Delete Data>All ..............................................................................
4.4.3.9 Delete Data>Highlighted ................................................................
4.4.3.10 Import..............................................................................................
4.4.4 View Menu .................................................................................................
4.4.4.1 Calibration Curve ............................................................................
4.4.4.2 Method ............................................................................................
4.4.4.3 Sample Window ..............................................................................
4.4.4.4 Outlier Test......................................................................................
4.4.4.5 Properties.........................................................................................
4.4.4.6 Customize........................................................................................
4.4.4.7 Toolbar ............................................................................................
4.4.4.8 Status Bar ........................................................................................
4.4.4.9 ASI / 8-Port Sampler Vials .............................................................
4.4.4.10 Data Profile .....................................................................................
4.4.5 Insert Menu.................................................................................................
4.4.5.1 Auto Generate .................................................................................
4.4.5.2 Sample.............................................................................................
4.4.5.3 Control.............................................................................................
4.4.6 Instrument Menu ........................................................................................
4.4.6.1 Background Monitor .......................................................................
4.4.6.2 Connect ...........................................................................................
4.4.6.3 Standby............................................................................................
4.4.6.4 Measurement Start ..........................................................................
4.4.6.5 Stop>Peak Stop ...............................................................................
4.4.6.6 Stop>Finish Current Sample ...........................................................
4.4.6.7 Stop>Halt ........................................................................................
4.4.7 Maintenance Menu .....................................................................................
4.4.8 Tools Menu.................................................................................................
4.4.8.1 Control Charts .................................................................................
4.4.8.2 Method Validation ..........................................................................
4.4.8.3 Administration.................................................................................
4.4.8.4 Screen Lock.....................................................................................
4.4.9 Options Menu .............................................................................................
4.4.9.1 General Information ........................................................................
4.4.9.2 Default Measurement Parameters ...................................................
4.4.9.3 Display Settings>Display Font .......................................................
4.4.9.4 Display Settings>Table Settings .....................................................
4.4.9.5 Display Settings>Notification Bar Settings ....................................
4.4.9.6 Display Settings>Floating Point Number Formats .........................
4.4.9.7 Directories .......................................................................................
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157
157
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158
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158
159
159
160
160
161
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203
205
206
207
207
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208
208
208
208
209
210
210
212
213
214
215
216
217
Table Of Contents
4.4.10 Window Menu............................................................................................. 218
4.4.10.1 Cascade ............................................................................................ 218
4.4.10.2 Tile ................................................................................................... 218
4.4.10.3 Arrange Icons................................................................................... 218
4.4.11 Help Menu................................................................................................... 218
4.5
Application Operations............................................................................ 219
4.5.1
Manual Injection Analysis .......................................................................... 219
4.5.1.1 Analysis Preparation ........................................................................ 219
4.5.1.2 Measurement.................................................................................... 221
4.5.1.3 Measurement Precautions for Low Concentration Samples............ 225
4.5.1.4 Maintenance..................................................................................... 226
4.5.2 Gas Sample Analysis................................................................................... 227
4.5.2.1 Analysis Preparation ........................................................................ 228
4.5.2.2 Measurement.................................................................................... 229
5
Maintenance ......................................................................................... 235
5.1
Daily Inspection....................................................................................... 236
5.1.1
5.1.2
5.1.3
5.1.4
5.2
Checking Dilution Water ............................................................................ 236
Checking Acid............................................................................................. 236
Checking Drain Vessel Water Level .......................................................... 236
Checking Humidifier Water Level ............................................................. 237
Periodic Inspections................................................................................. 238
5.2.1
5.2.2
Catalyst Regeneration ................................................................................. 238
Washing or Replacing Catalyst................................................................... 239
5.2.2.1 Washing Catalyst ............................................................................. 239
5.2.2.2 Replacing Catalyst ........................................................................... 240
5.2.2.3 Replacing the Carrier Gas Purification Tube and Catalyst.............. 240
5.2.3 Washing/Replacing the Combustion and Carrier Gas Purification Tubes.. 242
5.2.4 Replacing the High-Purity Air Cylinder ..................................................... 242
5.2.5 Replacing the CO2 Absorber....................................................................... 242
5.2.6 Replacing the Halogen Scrubber................................................................. 243
5.2.7 Replacing the Syringe Plunger Tip ............................................................. 244
5.2.8 Replacing Ferrules at the Combustion Tube Outlet Connection ................ 245
5.2.9 Replacing the Sliding Sample Injector O-rings .......................................... 245
5.2.10 Replacing the Syringe Pump 8-port Valve Rotor ....................................... 246
5.2.11 Replacing the CO2 Absorber for the Optional Carrier Gas Purifier ........... 248
5.2.12 Replenishing IC Reaction Solution............................................................. 249
5.2.13 Replacing the Pump Head of the IC Reaction Solution Pump.................... 250
5.2.14 Replacing the Filler of the Optional POC Analysis CO2 Absorber ............ 251
5.3
Autosampler (ASI-V) Maintenance......................................................... 252
5.3.1
5.3.2
5.3.3
5.4
Rinse Bottle Inspection ............................................................................... 252
Sample Catcher Inspection.......................................................................... 252
Replacing the Pump Head of the Rinse Pump ........................................... 253
8-Port Sampler (OCT-1) Maintenance .................................................... 254
TOC-VCPH/CPN
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Table Of Contents
5.5
TN Unit (TNM-1) Maintenance............................................................... 256
5.5.1
5.5.2
5.5.3
5.5.4
5.6
Replacing the Catalyst in the Ozone Treatment Unit.................................
Chemiluminescence Detector .....................................................................
Ozone Generator Replacement...................................................................
Replacing the NOx Absorber......................................................................
Software-Controlled Maintenance Functions .......................................... 261
5.6.1
5.6.2
5.6.3
5.6.4
5.6.5
5.6.6
5.6.7
5.6.8
5.6.9
5.6.10
5.6.11
5.6.12
5.6.13
5.6.14
5.6.15
5.6.16
5.7
Zero Point Detection...................................................................................
Regeneration of the TC Catalyst ................................................................
Regeneration of the IC Solution .................................................................
Residue Removal........................................................................................
Replace Flowline Content .........................................................................
Flowline Washing.......................................................................................
Mechanical Check ......................................................................................
ASI / 8-Port Sampler Initialization.............................................................
ASI Rack Change .......................................................................................
ASI Needle Change ....................................................................................
Change Syringe ..........................................................................................
Blank Check ...............................................................................................
Maintenance Log ........................................................................................
History ........................................................................................................
Sparge Gas Valve .......................................................................................
Adjust Sparging Flow Rate (Wet Chem.)...................................................
Error Messages ...........................................................................................
Troubleshooting..........................................................................................
5.7.2.1 TOC-V.............................................................................................
5.7.2.2 ASI-V ..............................................................................................
5.7.2.4 Corrective Actions for Poor Reproducibility ..................................
Principles of Analysis .............................................................................. 284
6.1.1
6.1.2
6.1.3
6.1.4
6.1.5
6.1.6
6.2
Principles of TC (Total Carbon) Analysis..................................................
Principles of IC (Inorganic Carbon) Analysis ............................................
Principles of NPOC (Non-Purgeable Organic Carbon) Analysis...............
Principles of POC (Purgeable Organic Carbon) Analysis..........................
Principles of Measuring TOC.....................................................................
Principles of Measuring TN (Total Nitrogen) ............................................
284
285
286
287
288
288
Analysis-Related Technical Information ................................................. 289
6.2.1
6.2.2
6.2.3
Peak Area Analysis.....................................................................................
Peak Shape..................................................................................................
Calibration Curves......................................................................................
6.2.3.1 Types of Calibration Curves ...........................................................
6.2.3.2 Shifting of Calibration Curves ........................................................
6.2.4 Sparging During Standard Solution Analysis.............................................
6.2.5 Automatic Selection of Optimum Calibration Curve.................................
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274
274
278
280
Reference Information ........................................................................ 283
6.1
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262
263
263
264
265
267
267
268
268
269
269
269
269
269
Troubleshooting ....................................................................................... 270
5.7.1
5.7.2
6
256
259
260
260
289
289
290
290
290
292
292
Table Of Contents
6.3
Specifications........................................................................................... 294
6.3.1
6.3.2
6.3.3
6.3.4
6.3.5
6.3.6
6.3.7
6.3.8
TOC-VCPH/CPN ........................................................................................... 294
ASI-V .......................................................................................................... 295
OCT-1 8-Port Sampler ................................................................................ 295
TNM-1......................................................................................................... 295
POC Kit....................................................................................................... 296
Carrier Gas Purifier Kit............................................................................... 296
Manual Injection Kit (Gas Sample Injection Kit) ....................................... 296
PC Hardware Requirements........................................................................ 297
6.4
Standard Accessories............................................................................... 298
6.5
Special Accessories ................................................................................. 303
6.6
Consumable Parts List ............................................................................. 304
6.7
Maintenance Parts List ............................................................................ 308
6.8
Installation ............................................................................................... 310
6.8.1
6.8.2
Before Installation....................................................................................... 310
Installation Site............................................................................................ 310
6.8.2.1 Installation Site Selection ................................................................ 310
6.8.2.2 Installation Site Conditions.............................................................. 311
6.8.3 Installation Procedure.................................................................................. 312
6.8.3.1 Connecting Power Supply and Ground ........................................... 312
6.8.3.2 Changing the Power Supply Voltage............................................... 313
6.8.3.3 Connecting Gas................................................................................ 313
6.8.3.4 Connecting the Drain Tubing .......................................................... 316
6.8.3.5 PC Cable Connections ..................................................................... 317
6.8.4 Installing the Autosampler .......................................................................... 317
6.8.5 OCT-1 8-Port Sampler Installation ............................................................. 325
6.8.5.1 Installation Procedure ...................................................................... 325
6.8.6 Installing the TN Unit ................................................................................. 328
6.8.6.1 Connecting the Power and Installation ............................................ 328
6.8.6.2 Connecting Ozone Source Air ......................................................... 329
6.8.6.3 Connecting Gas Exhaust Tubing ..................................................... 332
6.9
Material Safety Data Sheets .................................................................... 333
6.9.1
6.9.2
6.9.3
6.9.4
6.9.5
6.9.6
6.9.7
6.9.8
6.9.9
6.9.10
6.9.11
6.9.12
6.9.13
Hydrochloric Acid (HCl) ............................................................................ 333
Phosphoric Acid .......................................................................................... 334
CO2 Absorber, CA(OH)2, KOH, NAOH: soda lime .................................. 335
Lithium Hydroxide (monohydrate) ............................................................. 336
Halogen Scrubber........................................................................................ 337
Quartz Wool ................................................................................................ 338
High Sensitivity Catalyst............................................................................. 339
Normal Sensitivity Catalyst ........................................................................ 340
Potassium Nitrate ........................................................................................ 341
Sodium Bicarbonate .................................................................................... 342
Sodium Carbonate....................................................................................... 343
Potassium Hydrogen Phthalate ................................................................... 344
Water ........................................................................................................... 345
TOC-VCPH/CPN
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Table Of Contents
Appendix A Method Validation ................................................................. 347
A.1 Main Window .......................................................................................... 348
A.2 File Menu ................................................................................................. 349
A.2.1
A.2.2
A.2.3
A.2.4
A.2.5
A.2.6
A.2.7
A.2.8
A.2.9
New.............................................................................................................
Open ...........................................................................................................
Save ............................................................................................................
Save As.......................................................................................................
Print ............................................................................................................
Print Preview ..............................................................................................
Print Setup ..................................................................................................
Page Setup ..................................................................................................
Exit .............................................................................................................
349
350
351
351
351
352
353
353
355
A.3 Edit Menu................................................................................................. 356
A.3.1
A.3.2
A.3.3
A.3.4
A.3.5
A.3.6
A.3.7
Undo ...........................................................................................................
Cut/Copy/Paste ...........................................................................................
Insert Row ..................................................................................................
Delete Row .................................................................................................
Insert Column .............................................................................................
Delete Column............................................................................................
Recalculate .................................................................................................
356
356
356
357
357
357
357
A.4 View Menu............................................................................................... 358
A.5 Options Menu........................................................................................... 359
A.5.1
A.5.2
A.5.3
A.5.4
A.5.5
A.5.6
General Parameter ......................................................................................
Method Validation Parameter.....................................................................
Font.............................................................................................................
Floating Point Numbering Format..............................................................
ASCII Export Options ................................................................................
Validation Strictly Following DIN38402...................................................
359
360
361
362
363
364
A.6 Help Menu ............................................................................................... 365
Appendix B Control Charts........................................................................ 367
B.1
File Menu ................................................................................................. 368
B.1.1
B.1.2
B.1.3
B.1.4
B.1.5
B.1.6
B.1.7
B.1.8
B.1.9
B.1.10
B.1.11
B.2
xx
TOC-VCPH/CPN
New.............................................................................................................
Following Control Chart.............................................................................
Open ...........................................................................................................
Save ............................................................................................................
Save As.......................................................................................................
Print>Data...................................................................................................
Print>Graph ................................................................................................
Print Preview>Data/Print Preview>Graph .................................................
Print Setup ..................................................................................................
Page Setup ..................................................................................................
Exit .............................................................................................................
368
372
373
373
373
373
373
373
374
374
376
Edit Menu................................................................................................. 377
Table Of Contents
B.3
View Menu .............................................................................................. 378
B.3.1
B.3.2
B.3.3
B.3.4
B.4
Options Menu .......................................................................................... 381
B.4.1
B.4.2
B.4.3
B.4.4
B.4.5
B.5
Statistics ...................................................................................................... 378
Comparison ................................................................................................. 379
Out of Control Events ................................................................................. 380
Toolbar/Status Bar ...................................................................................... 380
Control Chart Options ................................................................................. 381
Font ............................................................................................................. 381
Floating Point Numbering Format .............................................................. 382
ASCII Export Options................................................................................. 383
Enable Exclusion......................................................................................... 383
Help Menu ............................................................................................... 384
TOC-VCPH/CPN
xxi
Table Of Contents
xxii
TOC-VCPH/CPN
1
Overview
1
This chapter provides an overview of the instrument and operational precautions for its
use.
1.1
Overview
Provides an overview of the TOC-VCPH/TOC-VCPN instrument.
1.2
Operational Precautions
Lists precautions necessary to ensure that the instrument is used correctly.
1.1
Overview
1.1
Overview
The TOC-VCPH/TOC-VCPN (hereinafter referred to as TOC-V) instrument measures the
amount of total carbon (TC), inorganic carbon (IC) and total organic carbon (TOC) in
water. Purgeable organic carbon (POC) can also be measured when the POC accessory is
installed. “Oxidative combustion-infrared analysis” is a widely-used TOC measurement
method that has been adopted by the JIS1 and other international standards. The TOC-V
instrument can also measure total water-borne nitrogen (TN) if the optional TN unit is
installed. TN is measured using the principles of “oxidative combustionchemiluminescence.”
Moreover, when the ASI-V Autosampler or OCT-1 8-Port Sampler is used in combination
with the main unit, a fully automatic system is created, allowing automatic analysis of
multiple samples.
This instruction manual covers both the TOC-VCPH and TOC-VCPN models. These models
will be referred to in relevant descriptions as the H Type and N Type, respectively.
Read this user manual carefully before using the TOC-V instrument to ensure its proper
use. The manual should be stored in a convenient location for future reference.
CAUTION
Safety may be compromised if the instrument is used in a fashion other than that
indicated in this user manual. Pay particular attention to the CAUTION sections
to ensure safety when using the instrument.
1. JIS K-0102 "Industrial Waste Water Testing", JIS K-0551: "Total organic carbon (TOC) testing methods for
ultra-pure water", U.S. Pharmacopoeia, EPA 415.1, EPA 9060A, ASTM D2575, Standard Methods for
Examination of Water and Waste Water 5310B
2
TOC-VCPH/CPN
1.2
1.2
Operational Precautions
Operational Precautions
Take the following precautions when using this instrument.
CAUTION
• Do not touch the electric furnace while it is heating. The center of the electric furnace
(near the combustion tube insertion opening) reaches very high temperatures, and burns
may result. <Burn prevention>
• To prevent high sensitivity catalyst from being forced upward in the combustion tube,
verify that carrier gas is flowing when heating the electric furnace. <Prevents the
floating of high sensitivity catalyst>
• Allow the electric furnace to cool to room temperature before removing or exchanging
the combustion tube. Burns may result if this procedure is attempted when the furnace
is at a high temperature. <Burn prevention>
• Do not heat the electric furnace without the combustion tube installed. Parts employed
by the TC injection port (slider block assembly) will be exposed to radiant heat from the
center of the electric furnace and may be deformed. If the furnace must be heated without a combustion tube installed, first remove the TC injection port parts to prevent
deformation, or close off the furnace core opening with a heat-insulating material such
as quartz wool. <Part damage prevention>
• To reduce back pressure, verify that the external drain tubing connected to the waste
port on the right side of the instrument does not touch the surface of the liquid in the
waste container. The height of the external tube must always be lower than the height of
the drain port. Excessive back pressure will result in insufficient drainage and waste will
overflow inside the instrument. <Part corrosion prevention>
TOC-V
Drain tubing (Tubing
placement should be as
indicated by the solid line.)
Drain container
(Supplied by user.)
Figure 1.1 External Drain Tubing
• Hand tighten the various connectors to the 8-port valve. Use of a tool may cause
deformation and leakage in the valve. <Part damage prevention>
TOC-VCPH/CPN
3
1.2
Operational Precautions
• Stop operation of the instrument when performing maintenance on any of the drive
components, such as connecting lines to the 8-port valve, or connecting/disconnecting
lines on the sample injector. If these parts are manipulated or if the lines are
disconnected during operation, the drive component could move and cause injury or
discharge of liquid. <Injury prevention, corrosion prevention>
• To shut down the instrument, first select “Shut down instrument” in the TOC-Control V
Standby window. Refer to Section 4.3.3 "Ending Measurement" for more information.
The electric furnace turns off and, after 30 minutes, the power supply shuts off. This
shutdown process extends the life of the TC injection port parts by preventing
unnecessary wear. This procedure does not apply to emergency shutdown.
<Maintaining durability of TC injection port parts>
• The lever of the 3-way valve at the bottom of the IC reaction vessel should normally be
turned to the left position. Refer to Figure 1.2 "Lever Position of 3-Way Valve on the IC
Reaction Vessel". The lever should never be turned to the lower position. The lower
position allows carrier gas to flow at a pressure of 200kPa upstream from the 3-way
valve, causing possible disconnection of joints and damage to parts such as the
combustion tube.
Carrier gas is discharged
to the front of the IC
reaction vessel. (Turn
the lever to this position
only when detaching an
IC reaction vessel that
contains liquid.)
Never turn the lever
to this position.
Figure 1.2 Lever Position of 3-Way Valve on the IC Reaction Vessel
• To use the ozone generator of the TN unit, verify that air is supplied at a rate of 0.5 L/
min to the ozone air source flow meter inside the instrument. Refer to Figure 2.5 "Inside
Front View". Turn ON the ozone generator. This prevents ozone leaks and line
corrosion. <Ozone leak prevention, line corrosion prevention>
• If ozone odor is detected during operation of the TN unit, stop the gas supply by turning
the ozone generator OFF, and contact your Shimadzu representative to request
maintenance. Ozone can cause respiratory organ injury and equipment damage.
<Prevention of injury to respiratory organs and equipment damage>
• To shut down the TN unit, turn the ozone generator OFF at least 3 minutes prior to
switching OFF the TN unit power to stop ozone generation. This prevents ozone leaks
and line corrosion. <Ozone leak prevention, line corrosion prevention>
4
TOC-VCPH/CPN
1.2
Operational Precautions
• The optional POC measurement circuit incorporates a carbon dioxide (CO2) absorber
packed with lithium hydroxide for removal of carbon dioxide gas. Misuse of lithium
hydroxide can cause bodily harm. During packing or replacing the CO2 absorber
container, exercise adequate precaution. After use, treat the material as industrial waste.
The properties and handling guidelines for lithium hydroxide are described in the material safety data sheets (MSDS) in Section 6.9 "Material Safety Data Sheets".
• To clean the instrument, wipe the surface with a soft cloth moistened with water. Do not
use chemicals.
• Repairs to the inside of the instrument can be dangerous. Contact your Shimadzu
representative to have a trained service engineer perform repairs.
• Do not disassemble or modify the instrument beyond the scope of the maintenance
procedures described in this manual, as safety may be compromised.
• The construction of the instrument is not explosion-proof. It must not be used in
dangerous areas.
• Use the instrument with a power supply of AC 100-127V ±10% (100V systems) or AC
220-240V ±10% (200V systems).
• The instrument backup battery will last for approximately one year. Connection to a PC
may not be possible if the instrument has been idle for more than one year. If this is the
case, turn the instrument power ON for at least 30 seconds, then turn the instrument
power OFF for 10 seconds and back ON again.
If the instrument usually remains idle for extended periods, turn the instrument power
ON for 24 hours once every six months.
• Do not use the following characters when naming files or systems to be saved:
/ , . \ (back slash) : ; (these are all normal-width characters), space (normal width, em
width)
• Turn OFF the Power Management function of the PC to prevent shutdown of the PC
power while it is controlling the TOC analyzer. A shutdown of this nature would
adversely affect performance.
• Hand-tighten the connectors to the 8-port valve of the 8-port sampler. Over-tightening
with a tool may exert excessive force to the internal valve body, causing deformation
and internal leakage. <Part damage prevention<
• Shut down the instrument before connecting or disconnecting tubing to the 8-port valve
or performing maintenance to the drive parts. Liquid may be discharged from tubes
during operation. <Part corrosion prevention>)
• When utilizing the software's printing function, set the paper size to letter or A4 and
printer graphic resolution to 600 dpi.
TOC-VCPH/CPN
5
1.2
6
Operational Precautions
TOC-VCPH/CPN
2
System Description
2
This chapter describes the components of the TOC-VCPH/CPN, autosampler (ASI-V), 8port sampler (OCT-1), and the TN unit (TNM-1).
2.1
TOC-VCPH/CPN Construction
Describes the construction of the TOC-V unit using front, right, left, rear and
internal views of the instrument, as well as flow diagrams.
2.2
Autosampler ASI-V (Option)
Describes the construction of the ASI-V unit using front and rear views of the
autosampler.
2.3
8-Port Sampler OCT-1 (Option)
Describes the construction of the 8-port sampler using front and rear views of the
unit.
2.4
TN Unit TNM-1 (Option)
Describes the construction of the TNM-1 unit using front, right and internal
views of the unit.
2.1 TOC-VCPH/CPN Construction
2.1.1 Front View
2.1
TOC-VCPH/CPN Construction
2.1.1 Front View
Start Button
Front Door
Power Switch
Stop Button
Figure 2.1 Front View
2.1.2 Right Side View
Tubing and Wiring
Opening for the
TN Unit
Drain Tubing
Figure 2.2 Right Side View
8
TOC-VCPH/CPN
2.1
TOC-VCPH/CPN Construction
2.1.3 Left Side View
2.1.3 Left Side View
Sample Tubing
Hydrochloric Acid
Dilution Water
Bottle
IC Reagent
Figure 2.3 Left Side View
2.1.4 Rear View
CO2 Absorber
Carrier Gas Inlet
AC Cord Socket
1
2
3
4
5
6
Figure 2.4 Rear View
1)
Flash ROM rewrite switch
2)
Printer cable terminal
3)
RS-232C terminal (1)
4)
RS-232C terminal (2)
5)
ASI-V/OCT-1 signal cable connector
6)
ASI-V/OCT-1 power cable connector
TOC-VCPH/CPN
9
2.1 TOC-VCPH/CPN Construction
2.1.5 Inside Front View
2.1.5 Inside Front View
1
2
3
5
4
6
16
7
8
15
9
14
10
13
Front Door
12
11
Figure 2.5 Inside Front View
1)
Sliding sample injector (H Type only)
2)
IC reagent vessel (H Type only)
3)
Solenoid valve (for IC drainage) (H Type only)
4)
Carrier gas pressure gauge
5)
Carrier gas flow adjustment knob
6)
Carrier gas flowmeter
7)
Carrier gas pressure adjustment knob
8)
Sparge gas flowmeter (option)
9)
Sparge gas flow adjustment knob (option)
10) Halogen scrubber
11) Humidifier
12) Pump (for IC reagent supply) (H Type only)
13) Syringe pump cover
14) 5mL syringe
15) 8-port valve
16) 3-way valve
10
TOC-VCPH/CPN
2.1
TOC-VCPH/CPN Construction
2.1.6 Inside Top View
2.1.6 Inside Top View
Slide Motor
Cooling Fan for
Sample Injection
Block
Slider
Sample Injection
Tubing
Sample Injection Block
Figure 2.6 Inside Top View
2.1.7 Flow Diagrams
Figure 2.7 Flow Diagram (TOC-VCPH)
TOC-VCPH/CPN
11
2.1 TOC-VCPH/CPN Construction
2.1.7 Flow Diagrams
Figure 2.8 Flow Diagram (TOC-VCPH+TNM-1)
Figure 2.9 Flow Diagram (TOC-VCPH+POC Option)
12
TOC-VCPH/CPN
2.1
TOC-VCPH/CPN Construction
2.1.7 Flow Diagrams
Figure 2.10 Flow Diagram (TOC-VCPN)
Figure 2.11 Flow Diagram (TOC-VCPN+TNM-1)
TOC-VCPH/CPN
13
2.2 Autosampler ASI-V (Option)
2.2.1 Front View
2.2
Autosampler ASI-V (Option)
2.2.1 Front View
Needle Replacement Window
Sample Tubing
Stirrer Speed
Control (option)
Sample Cover
Figure 2.12 Front View
2.2.2 Rear View
Rinse Solution Tubing
Signal Cable
Terminal
Power Cable
(attached to ASI)
Drain Tubing
Figure 2.13 Rear View
14
TOC-VCPH/CPN
2.3
2.3
8-Port Sampler OCT-1 (Option)
2.3.1 Front View
8-Port Sampler OCT-1 (Option)
2.3.1 Front View
8-Port Valve
Figure 2.14 Front View
2.3.2 Rear View
8-Port Sampler 1
Signal
Cable
Power
Cable
8-Port Sampler 2
Signal Cable
(with Power Supply)
Figure 2.15 Rear View
TOC-VCPH/CPN
15
2.4 TN Unit TNM-1 (Option)
2.4.1 Front and Right Side Views
2.4
TN Unit TNM-1 (Option)
2.4.1 Front and Right Side Views
Ozone Air Source Flowmeter
POWER: Power Lamp
REACT: Reactor Temperature
Control Heater Lamp
O3GEN: Ozone Generator
Status Lamp
PRESS: Ozone Source Air
Supply Warning Lamp
Ozone Generator Switch
Figure 2.16 Front and Right Side Views
16
TOC-VCPH/CPN
2.4
TN Unit TNM-1 (Option)
2.4.2 Inside Front View
2.4.2 Inside Front View
Reactor
Viton Joint
Flowmeter
Ozone Treatment Unit
Ozone Source Airflow
Adjustment Knob
Figure 2.17 Inside Front View
TOC-VCPH/CPN
17
2.4 TN Unit TNM-1 (Option)
2.4.3 Rear View
2.4.3 Rear View
Ozone Source Air Inlet
AC Cable Socket
Gas Exhaust Port
Figure 2.18 Rear View
18
TOC-VCPH/CPN
3
3
Software Overview, Administration,
and Setup
This chapter provides an overview of the TOC-Control V software and describes the
software’s Administration and Instrument Setup Wizard tools.
3.1
Introduction to System Administration Functions
Describes the system administration functions performed by the user.
3.2
Instrument Setup and System Properties
Describes the software’s Instrument Setup Wizard, which is used to configure
new systems by collecting information such as installed instrumentation,
instrument settings and communication parameters. Also describes procedures
for viewing the properties of and removing previously-configured systems.
3.1 Introduction to System Administration Functions
3.1.1 Screen Lock Function
3.1
Introduction to System Administration Functions
This section describes the various system administration functions in the TOC-Control V
software that are available to the user. For a description of system administration functions
that can be performed by the system administrator, refer to the TOC-V Administrator's
Manual.
3.1.1 Screen Lock Function
If user must temporarily leave the PC during measurement, the screen can be locked to
protect the data from another individual making improper or malicious operations in TOCControl V.
This function can be used only if the User ID / Password item is checked in the Security
dialog box. Consult with the system administrator to implement changes in the security
settings.
To lock the screen, select Screen Lock in the Tools menu. The screen is locked and the Reenter Password dialog box displayed. Once the screen is locked it can only be unlocked by
entering the User ID and Password of the user who was logged on at the time the screen
was locked.
Figure 3.1 Screen Lock Command
Figure 3.2 Re-enter Password Dialog Box
20
TOC-VCPH/CPN
3.1
Introduction to System Administration Functions
3.1.2 Change Password
3.1.2 Change Password
This function is used to change the password of a registered user.
Select Change Password in the TOC-Control V Administrator window to open the Change
Password dialog box. This function can be used only if the User ID/Password item is
checked in the Security dialog box. Refer to Section 3.2.4 “Security” in the Administrator’s
Manual for more information.
Figure 3.3 TOC-Control V Administrator Window
Figure 3.4 Change Password Dialog Box
TOC-VCPH/CPN
21
3.1 Introduction to System Administration Functions
3.1.3 Add Event Log
3.1.3 Add Event Log
This function is used when a comment is to be included with the operation history. This
function is useful for documenting items in the operation history, such as the replacement
of catalyst, that cannot be recorded automatically through the software. Only users with
access rights to Add Event Log can use this function.
This function can be used only if Audit Trail is checked in the Security dialog box. Refer to
Section 3.2.4 “Security” in the Administrator’s Manual for more information.
When Add Event Log is selected in the TOC-Control V Administrator window, the Add
Event Log dialog box is displayed.
Figure 3.5 Add Event Dialog Box
Select one of the items in the Select Item array, and then enter a comment in the
Comment text field. If the Comment text field is left blank, an error message is
displayed, and the comment is not added to the Event Log.
22
TOC-VCPH/CPN
3.2
3.2
Instrument Setup and System Properties
3.2.1 System Information Window
Instrument Setup and System Properties
This section describes the Instrument Setup Wizard, which is used to configure new
systems. This section also describes procedures for viewing the properties of and removing
previously-configured systems.
The TOC-Control V Instrument Setup Wizard is used to enter properties for a new system.
Access the Wizard by double-clicking the “New System” icon in the TOC-Control V main
window.
Multiple instruments can be configured for the TOC-Control V software system by
entering information into the series of Wizard screens.
TIP »
Use the Back and Next buttons to move among the various Instrument Setup Wizard
windows.
3.2.1 System Information Window
The System Information window of the Instrument Setup Wizard is used to enter basic
system information.
Figure 3.6 Instrument Setup Wizard: System Information Window
System
Enter a unique name for the system, using up to 32 characters. A name must be entered
before continuing to the next Wizard page. If a system with the entered name already exists,
an error message is displayed requesting entry of a unique name.
Serial Number
Enter the serial number of the TOC-V. The serial number of the unit is an 8-character
number (No. ********) that is printed on the plate attached to the lower right side of the
instrument.
TOC-VCPH/CPN
23
3.2 Instrument Setup and System Properties
3.2.2 Options Window
User
The name of the current user is automatically entered into the User field and cannot be
edited.
Date of Creation
The current date is automatically entered into the Date of Creation field and cannot be
edited.
Comment
Enter additional system information in the Comment text box. The Comment field is
optional and can contain up to 512 characters.
3.2.2 Options Window
The Options window of the Instrument Setup Wizard is used to specify the instrument
hardware configuration and attached accessories.
Figure 3.7 Instrument Setup Wizard: Options Window
Oxidation
Select “Combustion” from the drop-down list to specify the oxidation method.
Options
Select the installed instrument components by clicking the appropriate check boxes. The
options include TOC, ASI, SSM (solid-sampler unit), POC, IC Unit, TN, Sparge Kit,
Manual Injection Kit, 8Port Sampler-1, 8Port Sampler-2 and ESU (external scrubbing
unit). The selected options determine which Instrument Setup Wizard screens are
displayed.
Select the IC Unit for the H-type. If Manual Injection Kit is selected, the ASI, SSM, and
POC options are disabled.
24
TOC-VCPH/CPN
3.2
Instrument Setup and System Properties
3.2.2 Options Window
Option
Description
TOC
Displays the TOC screen of the Instrument Setup Wizard to allow TOC
instrument parameters to be set.
ASI
Displays the ASI screen of the Instrument Setup Wizard to allow
autosampler parameters to be set. This option is disabled if the Manual
Injection Kit option is selected.
SSM
Displays the SSM screen of the Instrument Setup Wizard to allow solid
sampler unit parameters to be set. This option is disabled if the Manual
Injection Kit option is selected.
POC
Specifies that the purgeable organic carbon accessory is installed.
IC Unit
Specifies that the instrument will be used to measure inorganic carbon.
Select this option for only instrument model TOC-VCPH. Do not select
this option for instrument model TOC-VCPN. If the IC Unit is selected as
an option, the “Auto regeneration of IC solution” check box will be
enabled on the Instrument Setup Wizard TOC screen.
TN
Specifies that the TN accessory is installed. If the TN Unit is selected as
an option, the “TN Power” check box will be enabled on the Instrument
Setup Wizard TOC screen.
Sparge Kit
Specifies that the Sparge Kit accessory is installed and that external
sparging is desired. If the Sparge Kit is selected as an option, the “Needle” parameter will be enabled on the Instrument Setup Wizard ASI
screen.
Manual Inj. Kit
Specifies that the Manual Injection Kit accessory is installed. The ASI,
SSM, and POC accessories cannot be used simultaneously with the Manual Injection Kit. If the Manual Injection Kit is selected as an option, the
options for ASI, SSM, and POC are deselected and disabled.
8-Port Sampler 1
Select this option when one 8-port sampler accessory is installed. 8-Port
Sampler 1 cannot be selected if the ASI or SSM are selected.
8-Port Sampler 2
Select this option when two 8-port sampler accessories are installed. 8Port Sampler 2 can only be selected if 8-Port Sampler 1 is selected.
TOC-VCPH/CPN
25
3.2 Instrument Setup and System Properties
3.2.3 TOC Window
3.2.3 TOC Window
The TOC window of the Instrument Setup Wizard is used to set TOC instrument
parameters.
Figure 3.8 Instrument Setup Wizard: TOC Window
Catalyst Type
Select the type of catalyst to be used in TC or TC/TN measurement from the drop-down
list. Available options are:
• Regular: for TC measurements (concentrations of 500ppb or greater)
• High Sense: for TC measurements (concentrations below 500ppb)
• TC/TN: for combined TC and TN measurements
Note: The instrument does not automatically recognize the type of catalyst that is installed. Be sure to select the catalyst type that is actually installed in the instrument.
The high sensitivity catalyst should be used when the expected sample concentrations are
below 500ppb or when detection of minute changes in concentration is necessary.
Tubing Diameter
Select the diameter size of the sample injection tubing from the drop-down list. Available
options are:
• Regular: 0.5mm diameter
• Suspended Particle: 0.8mm diameter
The typical tubing diameter is 0.5mm. Select a tubing diameter of 0.8mm if the Suspended
Solids kit is used.
Cell Length
Select the length of the NDIR detection cell from the drop-down list. Available options are:
• Long: for typical measurements
• Short: for measurements using the Suspended Solids kit
26
TOC-VCPH/CPN
3.2
Instrument Setup and System Properties
3.2.3 TOC Window
Buzzer
Enables the internal buzzer function. Select this option to allow the buzzer to sound during
measurement.
Auto regeneration of IC solution
Select this option to automatically regenerate the IC solution. This option is enabled only if
IC Unit was selected in the Options window of the Instrument Setup Wizard.
The acidity of the IC solution gradually decreases over time, as the acid is used to convert
the IC components in samples into carbon dioxide. Unless the IC solution is periodically
regenerated, it eventually loses its ability to fully convert IC into carbon dioxide, which can
affect the accuracy of analysis.
When the Auto Regeneration option is selected, the pH and volume of the IC solution are
automatically maintained at the appropriate levels. The instrument automatically pumps IC
solution from the IC reagent reservoir in the following cases:
• When the instrument is turned on
• Prior to the initial IC measurement, following a preset number of injections and preset
volume of injected samples
• If peak tailing is observed during an IC measurement. (The system notifies the user of
peak tailing by inserting a “T” into the Notes column of the Injection Table and the
Remark column of the Sample Table.)
Enable ready status check
Select this option to enable the Ready Status Check function. When the function is enabled,
the software always verifies that the instrument is in the Ready state prior to starting
measurement. Enabling the Ready Status Check function is recommended. When the
function is deselected, measurement can be performed when the instrument is not in the
Ready state, an option that is mainly for use by service personnel.
TN Power
This item is displayed if “TN” was selected as an option in the previous screen. Select this
item to perform TN analyses.
TC Furnace
Select the desired TC furnace temperature by clicking the appropriate radio button. Select
680 (°C) for regular or high sensitivity catalyst. Select 720 (°C) for TC/TN catalyst.
TOC-VCPH/CPN
27
3.2 Instrument Setup and System Properties
3.2.4 ASI Window
3.2.4 ASI Window
The ASI window of the Instrument Setup Wizard is displayed if ASI was selected in the
Options window of the Wizard. Use the ASI screen to set the autosampler parameters.
Figure 3.9 Instrument Setup Wizard: ASI Window
Tray Type
Select the ASI tray type from the drop-down list. Options are 24mL Vial and 40mL Vial.
Needle
Select the needle type from the drop-down list. Options are:
•
•
•
•
Sample: for analysis using only a sample needle
Sample+Sparge: for analysis using both a sample needle and a sparge needle
Coaxial: for analysis using an integrated sample and sparge needle
Coaxial+Sparge: for analysis using both the coaxial needle and a sparge needle,
which allows a sample to be measured while the next sample is sparged.
The Needle field is enabled only if Sparge Kit was selected in the Options window of the
Wizard.
Note:
The instrument does not automatically recognize the type of needle installed. Be
sure to select the type of needle that is actually installed in the instrument.
No. of Needle Washes
Enter the number of times (0-10) the outside of the needle will be washed with water from
the dilution water bottle, at the end of a sample run.
No. of Flow Line Washes
Enter the number of times (0-10) the flow lines will be washed after all samples listed in the
Sample Table have been measured. Water from the dilution water bottle is used to wash the
flow lines.
28
TOC-VCPH/CPN
3.2
Instrument Setup and System Properties
3.2.5 SSM Window
Rinse
Select this option to rinse the sampling needle between each sample with water from the
dilution water bottle.
Rinse After Acid Addition
Select this option to rinse the sampling needle after each acid addition with water from the
dilution water bottle.
Stirrer On
Select this item to use the optional magnetic stirrer during measurement.
3.2.5 SSM Window
The SSM window of the Instrument Setup Wizard is displayed if SSM was selected in the
Options window of the Wizard. Use the SSM screen to set the SSM parameters. Refer to
the SSM-5000A User Manual for details.
Figure 3.10 Instrument Setup Wizard: SSM Window
SSM TC Furnace On
Select this option for TC measurement.
SSM IC Furnace On
Select this option for IC measurement.
TOC-VCPH/CPN
29
3.2 Instrument Setup and System Properties
3.2.6 Communication Window
3.2.6 Communication Window
The Communication window of the Instrument Setup Wizard is used to set parameters for
communication between the instrument and the PC.
Figure 3.11 Instrument Setup Wizard: Communication Window
Com Port
Select the communication port from the drop-down list. Options include Com1, Com2,
Com3, and Com4.
Stop Bits
The Stop Bits value is determined by the hardware and is set automatically based on the
Com Port selection. This field is disabled and cannot be edited by the user.
Parity
The Parity value is determined by the hardware and is set automatically based on the Com
Port selection. This field is disabled and cannot be edited by the user.
30
TOC-VCPH/CPN
3.2
Instrument Setup and System Properties
3.2.7 History Function Window
3.2.7 History Function Window
The History Function window of the Instrument Setup Wizard is used to enable the History
Log. The History Log records all modifications to the system properties. The History Log
can be set to require users to enter comments for each modification.
Note:
Once the History Log is enabled, it cannot be disabled. All modifications to the
system properties will be tracked. If the mandatory comment option is selected,
the user will be required to enter a comment each time any system parameter is
modified.
Figure 3.12 Instrument Setup Wizard: History Function Window
Enable History Log
Select this option to enable the software to monitor all modifications to the system
properties. Once the History Log is enabled, the check box is disabled and the log cannot be
turned off. The History Log is maintained on the History tab of the Instrument Properties
dialog box. Refer to Section 3.2.8 "Instrument Properties Dialog Box". If the History Log is
not required, it need not be enabled, as the software operates properly without it.
A Comment is Required for All Modifications
Select this option to require the user to comment on or obtain approval for all
modifications. Once this option is selected, the check box is disabled and the option cannot
be turned off. If the History Log is not required, it need not be enabled, as the software
operates properly without it.
Finish Button
The History Function window is the final screen in the Instrument Setup Wizard. Make the
appropriate selections, then click the Finish button. The new instrument is created and
saved, and its icon appears in the TOC-Control V main window.
TOC-VCPH/CPN
31
3.2 Instrument Setup and System Properties
3.2.8 Instrument Properties Dialog Box
3.2.8 Instrument Properties Dialog Box
Instrument parameters can be viewed and modified using the Instrument Properties dialog
box, shown below. Open the dialog box by double-clicking the instrument icon in the TOCControl V main window.
Figure 3.13 Instrument Properties Dialog Box
System Tab
The System tab displays the System Information window for the selected system and
allows editing of the Comment field.
Options Tab
The Options tab displays the oxidation method and instrument components that were
selected in the Options window of the Instrument Setup Wizard. Information on this tab can
be viewed but not changed.
TOC Tab
The TOC tab is identical to the TOC window in the Instrument Setup Wizard. Some fields
on the TOC tab can be edited. If the History Log was enabled during setup, edits to the
TOC tab will be tracked and listed in the History tab.
ASI Tab
The ASI tab is identical to the ASI window in the Instrument Setup Wizard. Some fields on
the ASI tab can be edited. If the History Log was enabled during setup, edits to the ASI tab
will be tracked and listed in the History tab.
Communication Tab
The Communication tab is identical to the Communication window in the Instrument Setup
Wizard. Some fields on the Communication tab can be edited. If the History Log was
enabled during setup, edits to the Communication tab will be tracked and listed in the
History tab.
32
TOC-VCPH/CPN
3.2
Instrument Setup and System Properties
3.2.9 Removing a Configured System
SSM Tab
The SSM tab is identical to the SSM window in the Instrument Setup Wizard. Some fields
on the SSM tab can be edited. If the History Log was enabled during setup, edits to the
SSM tab will be tracked and listed in the History tab.
History Tab
If the History Log was not enabled during setup, the History tab is identical to the History
Function window in the Instrument Setup Wizard. Use this screen to enable the History log.
If the History Log was enabled during setup, the History tab lists all changes made to the
system parameters. The log lists modifications chronologically, with the most recent
modification at the top. If the mandatory comment option was selected during setup, all
modifications listed in the History tab window contain a comment describing the reason for
the change. View or edit previously entered comments by selecting the modification from
the list and clicking the Edit Comment button. If the History Log is not required, it need not
be enabled, as the software operates properly without it.
Figure 3.14 Comment Dialog Box
Note that if the mandatory comment option was selected in the History Function window
during instrument setup, the Comment dialog box (shown above) is displayed after any
change is made in the Instrument Properties dialog box.
3.2.9 Removing a Configured System
Systems are removed from the TOC-Control V software using the main window. To
remove a system, right-click the appropriate system icon and select Delete. Once a system
is deleted, it cannot be restored.
TOC-VCPH/CPN
33
3.2 Instrument Setup and System Properties
3.2.9 Removing a Configured System
34
TOC-VCPH/CPN
4
Operation
4
This chapter describes procedures for pre-analysis preparations, setting measurement
parameters, starting up the instrument, generating calibration curves, and conducting
sample analysis. This chapter also includes a tutorial that covers setup and measurement procedures.
4.1
Analysis Preparation
This section describes instrument preparation procedures such as catalyst filling,
combustion tube connection, and syringe replacement as well as other
preparation procedures for actual sample analysis.
4.2
Setting General Measurement Parameters
This section describes procedures for setting TOC, ASI and default measurement
parameters using the TOC-Control V software.
4.3
Measurement Procedures and Tutorial
This section describes and provides a tutorial for measurement procedures, such
as instrument startup, calibration curve generation, method development, sample
analysis, halting of analysis and instrument shutdown.
4.4
Sample Table Editor
This section provides a detailed description of the TOC-Control V Sample Table
Editor menus and commands. The Sample Table Editor is used for instrument
startup, calibration curve generation, method development, sample analysis,
halting of analysis and instrument shutdown.
4.5
Application Operations
The procedures for performing manual injection analysis and gaseous sample
analysis are described in this section.
4.1 Analysis Preparation
4.1.1 Catalyst Filling
4.1
Analysis Preparation
4.1.1 Catalyst Filling
Three types of catalyst are available: TOC standard catalyst, TOC high sensitivity catalyst
(H Type only), and TOC/TN catalyst (option). The procedures for filling the combustion
tube with catalyst are described in this section. For TOC standard and high sensitivity
catalyst filling, follow the procedure in Section 4.1.1.1 "Catalyst for TOC Analysis". For
TOC/TN catalyst filling, follow the procedure in Section 4.1.1.2 "TOC/TN Catalyst
(Option)".
CAUTION
Exercise caution when handling the combustion tube to prevent breakage, as it is
made of quartz glass.
Note:
When filling the combustion tube, verify that the catalyst does not become contaminated. Contamination will cause high blank values and abnormal analysis
values.
Using New Catalyst
Broad blank peaks are obtained when using new catalyst for the first time. The blank peaks
will become progressively smaller and more stable with repeated injections, and their size
will stabilize. If calibration or analysis is performed while the blank peaks are large, the
measurements are affected by the changing magnitude of the blank peaks, resulting in
errors in the analysis values. Such errors are especially significant for high sensitivity TC
analysis.
TC Analysis Using New Catalyst
Catalyst regeneration should be conducted 1-2 times for TC analysis using new catalyst.
This reduces the size of the blank peaks. Use continuous injections of pure water until the
blank peak area becomes small and stable. The blank peak magnitude depends on the
quality of the water (TC impurity concentration) and the TC analysis range used for
analysis. For example, a blank peak of 1mg/L has little influence on results greater than
100mg/L but has a significant influence on results equal to or less than 10mg/L. Analyses
for expected concentrations around 10mg/L must have stable blank peaks of 0.5mg/L or
less.
For TOC high sensitivity catalyst, conduct the TC blank check analysis described in
Section 4.1.15.2 "TC Blank Check Analysis".
TN Analysis Using New Catalyst
Blank peak magnitude poses no practical problems for TN analysis using new catalyst. The
blank peaks are fairly small and stable. Perform analysis with distilled or deionized water to
confirm the size of the blank peaks.
36
TOC-VCPH/CPN
4.1
Analysis Preparation
4.1.1 Catalyst Filling
4.1.1.1 Catalyst for TOC Analysis
Either standard or high sensitivity catalyst can be used for TOC analysis. The furnace
temperature is set to 680°C for TOC analysis.
¬TOC Standard Catalyst
The TOC standard catalyst is appropriate for both the TC-IC method and NPOC method of
analysis.
Note:
Analyze TOC high precision samples (with expected concentrations of about
1mg/L) using the TOC high sensitivity catalyst because smaller blank peaks are
generated.
Filling Combustion Tube with TOC Standard Catalyst
1.
2.
Insert two sheets of platinum mesh into the combustion tube.
3.
Fill the TOC standard catalyst to a height of about 100mm.
Layer about 5mm. of quartz wool onto the platinum mesh using the catalyst filling
rod.
Combustion Tube
TOC Standard Catalyst
100mm
Quartz Wool
Platinum Mesh
Figure 4.1 Combustion Tube with TOC Standard Catalyst
¬TOC High Sensitivity Catalyst (H Type only)
Use the TOC high sensitivity catalyst for low level TC analysis. The blank values are
controlled to negligible levels, and analysis is performed primarily for trace TOC in pure
water (1mg/L or less).
TOC-VCPH/CPN
37
4.1 Analysis Preparation
4.1.1 Catalyst Filling
Samples containing IC in excess of 5mg/L
The detection rate for IC decreases with increasing concentration. As a result, use the
NPOC method instead of the TC-IC method when analyzing samples that contain IC
concentrations in excess of 5mg/L.
Filling Combustion Tube with TOC High Sensitivity Catalyst
Two cylindrical containers of catalyst are required for a single load.
1.
2.
Place two sheets of platinum mesh in the combustion tube.
3.
Use the catalyst filling rod to push catalyst into the combustion tube from the other
opened end of the cylindrical catalyst container.
4.
Transfer the contents of the two cylindrical catalyst containers to achieve a catalyst
layer height of 130mm in the combustion tube.
Fit together the combustion tube opening and the opened end of the cylindrical
catalyst container.
Combustion Tube
TOC High-Sensitivity
Catalyst
130mm
Platinum Mesh
Figure 4.2 Filling of TOC Combustion Tube with High Sensitivity Catalyst
38
TOC-VCPH/CPN
4.1
Analysis Preparation
4.1.1 Catalyst Filling
4.1.1.2 TOC/TN Catalyst (Option)
TOC/TN catalyst is used for TN analysis and TOC/TN simultaneous analysis. The
detection rate is low for the IC component when it exceeds 10mg/L; as a result, TOC in
samples containing more than 10mg/L IC cannot be measured using the TC-IC method and
should be measured using the NPOC method. The furnace temperature is set to 720°C for
TOC/TN and TN analysis.
Filling Combustion Tube with Catalyst for TN Analysis
1.
2.
3.
Insert two sheets of platinum mesh into the combustion tube.
4.
5.
Introduce a small amount of ceramic fiber to cover the catalyst.
Layer about 5mm of quartz wool onto the platinum mesh using the catalyst filling rod.
Introduce the TOC standard catalyst into the combustion tube to a height of 140mm
from the top end of combustion tube.
Lightly press with a catalyst filling rod so that the thickness of the ceramic fiber is
10mm.
Note: • The thickness of the ceramic fiber must be uniform, covering the entire
surface of the catalyst, or a poor TN detection rate may result.
• The filling heights of the catalyst and ceramic fiber influence the TN
detection rate, so it is important that the dimensions are close to those
indicated below.
Catalyst: 140mm from the top end of combustion tube
Ceramic fiber: 10mm
Combustion Tube
Ceramic Fiber
10mm
140mm
TOC Standard Catalyst
Quartz Wool
Platinum Mesh
Figure 4.3 Filling Combustion Tube with Catalyst for TOC/TN Analysis
TOC-VCPH/CPN
39
4.1 Analysis Preparation
4.1.2 Connecting the Combustion Tube
4.1.2 Connecting the Combustion Tube
The procedure for installing the combustion tube differs depending on whether the
instrument is the H Type or the N Type. The procedure for each type is described below.
CAUTION
• Due to the potential for burns, maintenance of the combustion tube and catalyst
should be performed after the electric furnace temperature has cooled to room
temperature.
• When connecting the combustion tube, handle it carefully to avoid breakage. The
combustion tube is constructed of quartz glass, and injury is possible.
• Do not use a wrench or other tool. Injury could result if the combustion tube
breaks.
Installation for the H Type
40
1.
Push the capillary end of the catalyst-filled combustion tube downward, into the
center of electric furnace (about 22mm diameter).
2.
Apply an extremely thin layer of the provided high-vacuum silicone grease to the
outside of the combustion tube tip (part in contact with O-ring).
Note: Use the smallest possible amount of silicone grease. Absolutely no
grease should be applied to the interior of the combustion tube.
3.
Insert the tip of the combustion tube, with the silicone grease, securely into the
opening at the bottom of the sample injector.
Note: At this point, be sure to connect the drain tubing exiting the slide
injector to the Y-fitting of the system drain line.
4.
Connect the tubing at the bottom end of combustion tube, as shown in Figure 4.4
"Connecting Combustion Tube to the Compression Fitting". Push the narrow end of
the combustion tube into the compression fitting. Adjust the distance between the
bottom of the compression fitting and the base of the instrument to 1mm or less, and
then tighten the top compression fitting nut firmly by hand.
TOC-VCPH/CPN
4.1 Analysis Preparation
Connecting the Combustion Tube
4.1.2
TC Combustion Tube
Nut
Rear Ferrule
Front Ferrule
Sleeve Set 6F-T
(P/N 035-62994-03)
TC Combustion Tube
Stainless Tubing
(toward detector)
Compression Fitting
Figure 4.4 Connecting Combustion Tube to the Compression Fitting
CAUTION
•
•
•
•
The instrument is sealed sufficiently if the combustion tube does not move when
pulled upwards.
The quartz glass combustion tube will break if the compression fitting is overtightened.
Use only the provided Teflon ferrules for the front and rear ferrules. Do not use
any other material, such as metal.
Do not allow organic contaminants such as grease or oil to touch the inner or
outer surfaces on the tip of the combustion tube and gas connection parts of the
ferrules. This is especially important for high sensitivity analysis.
TOC-VCPH/CPN
41
4.1 Analysis Preparation
4.1.2 Connecting the Combustion Tube
Combustion
Tube
Figure 4.5 Connecting the Combustion Tube
5.
Secure the sample injector with the knurled thumbscrew.
Knurled
Thumbscrew
Figure 4.6 Securing the Sample Injector
6.
To prevent heat escape from the furnace, pack the space around the capillary part of
the combustion tube with the provided ceramic fiber.
CAUTION
Use caution to avoid inhaling ceramic fibers when inserting the fibers into the
combustion tube.
42
TOC-VCPH/CPN
4.1.2
4.1 Analysis Preparation
Connecting the Combustion Tube
7.
Verify that the gap between the adjustable base at the bottom of the instrument and the
bottom-most part of the compression fitting is 1mm or less (preferably no gap).
8.
If the gap is too large, loosen the nut at the top of the compression fitting and pull the
combustion tube upwards. Since the TC combustion tube is inserted into the
compression fitting, pulling up on the combustion tube shortens the insertion length
and ultimately lowers the compression fitting assembly. When almost no gap remains,
firmly tighten the nut at the top of the compression fitting.
Note: The sample rapidly vaporizes in the combustion tube when injected
in large quantities with a gap present between the bottom-most part
of the compression fitting and the base of the instrument. The
pressure increases, resulting in a separation at the connection
between combustion tube and sample injector.
Installation for the N Type
1.
Push the capillary part of the catalyst-filled combustion tube downward into the
center of electric furnace (about 22mm diameter).
2.
Apply an extremely thin layer of the provided high-vacuum silicone grease to the
outside of the combustion tube tip (part in contact with O-ring).
Note: Use as small amount of silicone grease as possible. Absolutely no
grease should be applied to the interior of the combustion tube.
3.
Insert the silicone grease coated tip of the combustion tube into the opening at the
bottom of the sample injector.
Note: Connect the drain tubing exiting the slide injector to the Y-fitting of
the system drain line.
4.
Connect the tubing at the bottom of the combustion tube, as shown in Figure 4.7
"Connecting the Combustion Tube".
CAUTION
•
•
•
The instrument is sealed sufficiently if the combustion tube does not move when
it is pulled upwards.
The quartz glass combustion tube will break if the compression fitting is overtightened.
Do not allow organic contaminants such as grease or oil to touch the inner or
outer surfaces on the tip of the combustion tube and gas connection parts of the
ferrules. This is especially important for high sensitivity analysis.
TOC-VCPH/CPN
43
4.1 Analysis Preparation
4.1.2 Connecting the Combustion Tube
Combustion
Tube
Figure 4.7 Connecting the Combustion Tube
5.
Secure the sample injector with the knurled thumbscrew, as shown in Figure 4.8
"Securing the Sample Injector".
Knurled
Thumbscrew
Figure 4.8 Securing the Sample Injector
6.
To prevent heat escape from the furnace, pack the space around the capillary part of
the combustion tube with the provided ceramic fiber.
CAUTION
Use caution to avoid inhaling ceramic fibers when inserting the fibers into the
combustion tube.
44
TOC-VCPH/CPN
4.1 Analysis Preparation
4.1.3 Installing the Syringe
4.1.3 Installing the Syringe
This section describes the procedure for attaching the syringe to the syringe pump
assembly.
Depending on the instrument status, flow lines are connected to each of the 8 ports of the
syringe pump valve. If the syringe is installed or removed without following the sequence
described below, acid can be released from the syringe connection port. The sequence
described below must be followed.
CAUTION
•
•
Due to the potential for injury, keep hands away from the sample injector during
operation of the syringe pump unit.
The syringe barrel is made of glass and must be handled carefully to avoid breakage.
Syringe Installation
1.
2.
Open the TOC-Control V Sample Table Editor and connect the instrument.
From the Instrument menu, select Maintenance>Change Syringe.
The Syringe Change dialog box is displayed.
Figure 4.9 Syringe Change Dialog Box
3.
Click the Preparation Start button to begin the procedure. A progress bar is active
while the syringe moves to the position where it can be replaced.
4.
When the progress bar begins blinking, remove the screw at the bottom of the syringe
pump cover, and remove the cover.
5.
6.
7.
Remove the sparge gas line from the syringe.
Remove the syringe from the syringe connection port of the 8-port valve.
Attach the new syringe to the syringe connection port of the 8-port valve.
TOC-VCPH/CPN
45
4.1 Analysis Preparation
4.1.3 Installing the Syringe
8.
Connect the sparge gas line to the syringe using the bushing and spacer.
Note: Do not use tools when replacing the syringe; hand-tighten only.
Over-tightening can deform the components of the 8-port valve and
result in leaks.
Syringe
Plunger
Retaining
Screw
Figure 4.10 Installing the Syringe
9.
Verify that the syringe moves smoothly between the upper and lower positions by
clicking the directional arrows on the Syringe Change dialog box.
10. With the syringe in this position, hand-tighten the plunger retaining screw on the
plunger holder.
11. Click the Finish Replacement button to move the syringe to its initial position.
12. Click the Close button.
Note:
46
TOC-VCPH/CPN
Once the syringe is installed, perform the syringe pump zero point
detection operation.See Section 4.1.3.1 "Syringe Pump Zero Point
Detection" for details.
4.1 Analysis Preparation
4.1.3 Installing the Syringe
4.1.3.1 Syringe Pump Zero Point Detection
This section describes the procedure for performing automatic detection of the syringe
pump zero point.
Note:
Perform the zero point detection procedure whenever a new syringe is installed
or the syringe is replaced.
Procedure
1.
2.
Open the TOC-Control V Sample Table Editor and connect the instrument.
From the Instrument menu, select Maintenance>Zero Point Detection.
The Zero Point Detection dialog box is displayed.
Figure 4.11 Zero Point Detection Dialog Box
3.
Click the Start button.
A progress bar is active while the syringe moves to the position where the zero point
can be detected. When the progress bar stops blinking, the procedure is complete.
4.
Click the Close button.
TOC-VCPH/CPN
47
4.1 Analysis Preparation
4.1.4 Water Supply to the Cooler Drain Container
4.1.4 Water Supply to the Cooler Drain Container
The drain container must be filled with water to prevent carrier gas from being released
from the drain tubing.
Procedure
1.
2.
3.
Remove the rubber cap from the drain container.
4.
5.
6.
Cap the drain container with the rubber cap.
Remove the drain container from the mounting clip.
Introduce pure water (deionized water is acceptable) into the cooler drain container up
to the level of the drain discharge tube on the side of the container.
Return the drain container to its position in the mounting clip.
Verify that the cooler drain tube reaches to the bottom of drain container.
CAUTION
Do not bend drain tubing, as this may prevent drain discharge.
Rubber Cap
Drain Discharge Tube
Drain Tubing
Mounting Clip
Drain Container
Pure Water
Figure 4.12 Filling the Cooler Drain Container with Water
48
TOC-VCPH/CPN
4.1.5
4.1 Analysis Preparation
Filling the Humidifier with Water
4.1.5 Filling the Humidifier with Water
The carrier gas must be humidified for high sensitivity analysis to ensure high analysis
precision. Water is supplied to the humidifier using the following procedure.
Procedure
1.
2.
Remove the cap from the water supply port at the top of the humidifier.
Introduce water through the water supply port to the “Hi” marking on the side of the
humidifier.
Note: Use pure water containing as little TC as possible for high
sensitivity analysis.
Water Supply
Port
Pure Water
Humidifier
“Hi” Marking
Figure 4.13 Filling the Humidifier with Water
TOC-VCPH/CPN
49
4.1 Analysis Preparation
4.1.6 Preparation of Dilution Water
4.1.6 Preparation of Dilution Water
This section describes the preparation of water used to automatically dilute samples.
Procedure
1.
Wash the provided dilution water bottle with laboratory glassware detergent, rinse
well with tap water, then wash a number of times with pure water.
2.
3.
4.
5.
Fill the container with pure water to the 2 liter level.
6.
Place the cap on the container.
Note: Verify that the tip of the intake tubing nearly reaches the bottom of
the container.
Place the container to the left of the instrument, toward the rear.
Pass the dilution water intake tubing, labeled DILUTION, through the hole in the cap.
Secure the tubing, using a wire clamp about 200mm from the end of the tubing, to
prevent the tubing and cap from separating.
Dilution Water
Intake Tubing
Dilution Water
Bottle
Figure 4.14 Preparing Dilution Water
Note:
About pure water:
• Use the purest water that can be obtained.
• Refer to Section 4.1.14.1 "Preparation of Standard Solutions" for details on
the degree of purity of “pure water”.
50
TOC-VCPH/CPN
4.1 Analysis Preparation
4.1.7 Acid Preparation
4.1.7 Acid Preparation
This section describes the preparation of acid used for IC removal in NPOC analysis or for
IC analysis with the N Type instrument.
Procedure
1.
Prepare 2 M HCl by diluting 1 part commercially available concentrated HCL (12 M)
with 5 parts pure water. A final concentration accuracy of ±2% is acceptable.
Note: The pure water used as the diluent must have a TOC concentration
no greater than 0.5 mg/L. Since the TOC value of the diluent pure
water can have a large effect on the analysis result with high
sensitivity analysis (low TOC concentrations), it is necessary to use
pure water having a very low TOC concentration.
CAUTION
Hydrochloric acid is a hazardous chemical. Use precautions to avoid contact when handling
this substance. For details, refer to Section 6.9 "Material Safety Data Sheets".
2.
Transfer the prepared acid to the 250 mL bottle provided as a standard accessory, and
place it to the left of the instrument, toward the front.
3.
4.
Pass the acid intake tubing through the hole in the cap.
5.
Place the cap on the container.
Note: Verify that the tip of the acid intake tubing nearly reaches the
bottom of the container.
Secure the tubing, using a wire clamp about 100mm from the end of the tubing, to
prevent the tubing and cap from separating.
Acid Intake Tubing
Cap
Hydrochloric Acid
Container
Figure 4.15 Acid Preparation
TOC-VCPH/CPN
51
4.1 Analysis Preparation
4.1.8 Installation of the CO2 Absorber
4.1.8 Installation of the CO2 Absorber
A CO2 absorber is used to remove CO2 from the carrier gas that purges the optical system
of the detector. The CO2 absorber is installed using the following procedure.
Procedure
1.
2.
Cut the tips of the 2 rigid tubes in the lid of the CO2 absorber with a knife.
3.
Place CO2 absorber in the holder behind the instrument.
Connect the flexible tubing that exits the rear panel of the instrument (near the top) as
follows:
Tubing labeled “L”: Connect to tube labeled “L” on CO2 absorber.
Tubing labeled “S”: Connect to tube labeled “S” on CO2 absorber.
Note: The flexible tubing should not be bent.
Flexible Tubing
Rigid Tubes
CO2 Absorber
Figure 4.16 Installation of the CO2 Absorber
52
TOC-VCPH/CPN
4.1.9
4.1 Analysis Preparation
Adjusting Sparge Gas Flow Rate
4.1.9 Adjusting Sparge Gas Flow Rate
The sparge gas flow rate should be adjusted before sparging is performed using the optional
external sparge kit. The procedure for adjusting the sparge gas flow rate is described below.
Procedure
1.
2.
Open the TOC-Control V Sample Table Editor and connect the instrument.
3.
4.
Open the front door of the instrument.
5.
Close the front door of the instrument.
From the Instrument menu, select Maintenance>Sparge Gas Valve.
The sparge gas solenoid valve opens and sparge gas begins to flow.
Adjust the flow rate to about 100mL/min using the sparge gas flow rate adjustment
knob.
Note: The flow rate should be adjusted according to the size and shape of
the sample container.
Sparge Gas Flow
Rate Adjustment Knob
Halogen
Scrubber
Figure 4.17 Sparge Gas Flow Rate Adjustment
TOC-VCPH/CPN
53
4.1 Analysis Preparation
4.1.10 Installing the Suspended Solids Kit
4.1.10 Installing the Suspended Solids Kit
To analyze samples containing suspended solids, the sample flow line diameter can be
increased from 0.5mm to 0.8mm by installing the optional Suspended Solids Kit.
This section describes the installation of the Suspended Solids Kit.
There are two kits available:
(1) For TOC-V (TOC-V main unit only)
(2) For TOC-V+ASI-V (used with TOC-V and autosampler)
CAUTION
Switch OFF the TOC-V before attempting to install the Suspended Solids Kit.
¬Replacing the Flow Line Parts and Slider
This procedure is used for both kits.
Procedure
54
1.
Remove the bushing from port 7 of the 8-port syringe pump valve, and disconnect the
TC injection tubing. For the H-type, remove the bushing from port 5, and disconnect
the IC injection tubing.
2.
Remove the slider mounting screws from the TC and IC injection blocks, and detach
the sliders.
3.
Remove the slider bushings and replace the sample injection tubing with the 0.8mm
diameter sample injection tubing provided in the kit.
4.
5.
Reinstall the sliders on the sample injection blocks.
TOC-VCPH/CPN
Connect the TC injection tubing and the IC injection tubing to port 7 and port 5,
respectively.
Note: During analysis, verify that the sample flow is normal. Refer to
Section 5.7.2.4 "Corrective Actions for Poor Reproducibility"
If the sample stream is not normal, the tip of the Teflon tube may be
deformed or scratched. Use a knife to cut off a portion of the tube.
4.1.10
4.1 Analysis Preparation
Installing the Suspended Solids Kit
¬Replacing Sample Tubing
For TOC-V (TOC-V main unit only)
1.
Remove the bushing from port 1 of the 8-port syringe pump valve and replace the
sample tubing with the 0.8mm diameter tubing provided in the kit.
2.
Connect the new sample tubing to the 8-port valve in the original position.
For TOC-V+ASI-V (TOC-V and autosampler)
Refer to Section 6.8.4 "Installing the Autosampler" to remove the autosampler sample
needle and sample tubing. Replace these with the sample needle and tubing provided in the
Suspended Solids Kit.
Precautions for Measuring Suspended Solids
•
•
•
•
When performing measurement of solid samples using the Suspended Solids
Measurement kit, follow the precautions below to ensure the best possible
conditions for measurement. Refer to Section 4.1.15.4 "Analysis of Samples
Containing Suspended Solids".
Before measurement, use a homogenizer, etc. to make the sample as uniform as
possible. After homogenizing the sample, depending on the type of suspended
substance, precipitation and coagulation may occur after a period of time. Prior
to measurement, mix the sample again using a magnetic stirrer to ensure that precipitated/coagulated material is well dispersed throughout the sample.
If the suspended material is present in large quantities, clumping of the material
and obstruction may occur inside the sample flow line even if the particles are of
smaller diameter that the sample flow line diameter. Take measures such as sample dilution to prevent flow line obstruction,
The suspended solids measurement kit employs a 0.8mm Teflon tube for sample
injection. Diminished reproducibility may occur with small sample injection volumes. Make injection volumes as large as possible.
When conducting IC measurement of suspended solid samples using the H type
instrument, obstruction of the IC measurement flow line drain tube may occur.
Sufficiently pulverize the suspended particles to allow free flow through the
drain tube.
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55
4.1 Analysis Preparation
4.1.11 IC Analysis Preparations
4.1.11 IC Analysis Preparations
Certain preparations are necessary for the H Type instrument. These include installing and
replenishing the IC reagent in the IC reaction vessel. This section describes the procedures
for installing and replenishing the IC reagent.
CAUTION
The IC reagent contains phosphoric acid. Use care while handling to prevent contact or
spills. For details, refer to Section 6.9 "Material Safety Data Sheets".
¬Preparing and Placing the IC Reagent
Procedure
56
1.
Prepare the IC reagent by diluting 50 mL of commercial 85% phosphoric acid (ACS
Reagent grade) to a final volume of 250 mL with pure water.
Note: Since the specific gravity of 85% phosphoric acid is about 1.7, the
concentration of the phosphoric acid is about 25% (weight%) in the
prepared IC reagent. A final concentration accuracy of ±2% is
acceptable.
2.
Transfer the prepared acid to the 250 mL bottle provided as a standard accessory, and
place it on the left side of instrument, toward the front.
3.
4.
Pass the tip of the IC reagent tubing through the hole in the cap.
5.
Replace the cap on the container.
TOC-VCPH/CPN
Secure the tubing, using a wire clamp at a point about 100mm from the end of the
tubing tip, to prevent the tubing and cap from separating.
4.1.11
4.1 Analysis Preparation
IC Analysis Preparations
¬Replenishing IC Reaction Vessel with IC Reagent
Use the following procedure to replenish the IC reagent.
Procedure
1.
Verify that the lever of the 3-way valve at the bottom of the IC reaction vessel is
positioned to the left as shown in Figure 4.18 "Lever Position of IC Reaction Vessel 3Way Valve".
Figure 4.18 Lever Position of IC Reaction Vessel 3-Way Valve
2.
3.
Open the TOC-Control V Sample Table Editor and connect the instrument.
From the Instrument menu, select Maintenance>Regeneration of the IC solution.
The Regeneration of IC solution dialog box is displayed.
Figure 4.19 Regeneration of IC Solution Dialog Box
4.
Click the Start button. The IC reagent will be delivered to the IC reagent vessel by the
liquid delivery pump. During the process, the Start button is disabled.
5.
A progress bar is active until the IC reagent is completely regenerated. Click the Close
button.
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57
4.1 Analysis Preparation
4.1.12 Preparation for POC analysis
4.1.12 Preparation for POC analysis
POC analysis can be performed if the optional POC analysis kit is installed on the
instrument. This section describes preparations required for POC analysis.
Installation of the CO2 Absorber for POC Analysis
1.
2.
3.
Remove the CO2 absorber.
4.
5.
6.
Place about 5mm of quartz wool on top of the lithium hydroxide.
Insert about 5mm of quartz wool into the bottom of the container.
Add commercially available anhydrous lithium hydroxide to the container on top of
the quartz wool until it reaches just below the screw threads of the container.
Note: About 6g of anhydrous lithium hydroxide is required for a single
load.
Attach the O-ring and nipple to the top of the container, and firmly tighten the cap.
Install the CO2 absorber for POC analysis in the original position.
CAUTION
• Lithium hydroxide is a corrosive (strongly basic) powder. Use care when handling to prevent contact or inhalation. Refer to Section 6.9 "Material Safety Data
Sheets" for details.
• Lithium hydroxide is available in anhydrous and hydrated forms. Since the ability of the hydrated form to absorb carbon dioxide is slightly inferior to that of the
anhydrous form, use anhydrous lithium to fill the CO2 absorber container.
• When introducing the quartz wool and lithium hydroxide into the container, do
not pack too tightly.
• The CO2 absorber container is constructed of glass. Handle it carefully to prevent
breakage.
Cap
Nipple
O-Ring
Lithium Hydroxide
Quartz Wool
Figure 4.20 Preparing the CO2 Absorber for POC Analysis
58
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4.1.13
4.1 Analysis Preparation
TN Analysis Preparations
4.1.13 TN Analysis Preparations
TN analysis can be performed if the optional TN unit is installed on the instrument. The
NOx absorber also must be connected to perform TN analysis. The CO2 absorber (soda
lime) is used as the NOx absorber. Connect it to the instrument using the following
procedure.
Procedure
1.
2.
Cut the tips of the rigid tubes (2) in the lid of the CO2 absorber with a knife.
3.
Place the NOx absorber behind the instrument.
Connect the Viton tubing to the 2 rigid tubes as follows:
Tubing labeled “L”: Connect to tube labeled “L” on the CO2 absorber.
Tubing labeled “S”: Connect to tube labeled “S” on the CO2 absorber.
Viton Tubing
TN Unit
Rigid Tubing
Figure 4.21 Connecting the NOx Absorber
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59
4.1 Analysis Preparation
4.1.14 Preparation and Storage of Standard Solutions
4.1.14 Preparation and Storage of Standard Solutions
4.1.14.1 Preparation of Standard Solutions
Zero water refers to a standard solution with zero concentration of TC, IC or TN; zero
water also refers to the water used to prepare these standard solutions. Water that is, in
theory, absolutely free of carbon (TC) or nitrogen (TN) is used as zero water. In practice, it
is difficult to obtain this type of water. Even ultra-pure water obtained using a highperformance membrane technique and water that has been repeatedly distilled will have a
TC content of about 10µg/L. This value is measured directly after manufacture, and
increases when the water is stored in a container. Carbon dioxide is contained in the
atmosphere at concentrations ranging from 300 to 500mg/L. The CO2 content of ambient
air is higher in a room with many people or where combustion equipment is used. Carbon
dioxide in ambient air dissolves in stored water, taking the form of IC. The dissolved
amount is generally about 0.2mg/L, but depends on the water temperature and carbon
dioxide content of the air in contact with the water. Refer to Table 6.2 • "CO2 Content
(ppm) in Distilled Water Equilibrated with Atmosphere Temperature (°C)". Instruments
that prevent contact with air are not incorporated in water uptake, retention or storage
processes during common distillation and purification of water. For this reason, IC is
present in most types of distilled and purified water. In some cases, the TC content of
commercially-available distilled water stored in plastic or glass containers is 1ppm.
Note:
The degree of purity required varies depending on the analysis range. Use of
commercially-available purified water is acceptable when measuring samples
with expected TC concentrations around 100ppm. The quality of the zero water
should be considered along with the analysis range.
Preparation of TC Standard Solutions
60
1.
Accurately weigh 2.125g of reagent grade potassium hydrogen phthalate that was
previously dried at 105-120°C for about 1 hour and cooled in a desiccator.
2.
3.
Transfer to a 1 L volumetric flask and dissolve in zero water.
4.
The standard stock solution is diluted with zero water to prepare standard solutions at
the required concentrations.
Note: The TC standard solution reagent need not be potassium hydrogen
phthalate. Depending on the application, other substances are also
acceptable (e.g., sucrose, etc.).
TOC-VCPH/CPN
Add zero water to the 1 L mark, and stir the solution.
The carbon concentration of the solution is 1000mgC/L (1000mgC/L = 1000ppmC).
This solution is the standard stock solution.
Note: The standard stock solution may be prepared at other
concentrations. For example, a 2000mgC/L solution can be used as
the standard stock solution.
4.1.14
4.1 Analysis Preparation
Preparation and Storage of Standard Solutions
Preparation of IC Standard Solution (HV)
1.
Accurately weigh 3.50g of reagent grade sodium hydrogen carbonate that was
previously dried for 2 hours in a silica gel desiccator, and 4.41g of sodium carbonate
previously dried for 1 hour at 280-290°C and cooled in a desiccator.
2.
3.
4.
Transfer the weighed materials to a 1L volumetric flask.
Add zero water to the 1L mark.
Stir well to mix.
In this instance, the carbon concentration of 1000mg/L is indicated as 1000mgC/L.
The concentration of this solution is 1000mgC/L (1000ppmC) and is referred to
below as the “TC Standard Solution”.
Preparation of TN Standard Solution
1.
Accurately weigh 7.219g of special reagent grade potassium nitrate dried for 3 hours
at 105-110°C and cooled in a desiccator.
2.
3.
4.
Transfer the weighed material to a 1L volumetric flask.
Add zero water to the 1L mark.
Stir well to mix.
In this instance, the nitrogen concentration of 1000mg/L is indicated as 1000mgN/L.
The concentration of this solution is 1000mgN/L (1000ppmN) and is referred to
below as the “TN Standard Solution”.
Preparation of POC Standard Solution (using the optional POC analysis kit)
IC standard solution is used as the POC standard solution with this instrument for the
following reasons.
• In POC analysis, the measured substance is an organic material that is volatile and
poorly soluble in water (for example, benzene or chloroform). Preparing a standard solution at an appropriate concentration using these types of organic substances is difficult.
• Volatile and poorly soluble organic substances tend to undergo changes in concentration during storage or handling after preparation.
• Standard solutions that are produced using volatile and poorly soluble organic substances are difficult to use.
Consequently, the IC standard solution is used for this instrument. The preparation
method is listed above.
TC/TN Mixed Standard Solution Preparation Procedure
When TC (or NPOC) and TN analyses are performed simultaneously, a mixed TC and
TN standard solution is prepared.
The mixed standard solution is prepared by mixing the TC standard solution and TN
standard solution. The mixed standard solution must contain 0.05M hydrochloric
acid.
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61
4.1 Analysis Preparation
4.1.14 Preparation and Storage of Standard Solutions
Preparation of 100mgC/L TC - 100mgN/L TN Mixed Standard Solution
1.
Prepare 1L of 1000mgC/L TC standard solution using the preparation method
described above.
2.
Prepare 1L of 1000mgN/L TN standard solution using the preparation method
described above.
3.
Introduce 100mL of each of the prepared standard solutions into a 1L volumetric
flask.
4.
5.
6.
Add 25mL of 2M hydrochloric acid to the flask
Add zero water to the 1L level.
Stir well to mix.
The hydrochloric acid concentration will be about 0.05M after dilution.
4.1.14.2 Storage of Standard Solutions
The standard solutions undergo concentration changes, particularly when lowconcentration solutions are stored even for short periods. As a result, high-concentration
standard stock solutions (for example, 1000mgC/L) should be stored in airtight containers
in a cool, dark place. Glass bottles are suitable storage containers. Dilute the stock solution
prior to each use.
Storage Time
The limitation on storage of standard solutions is about 2 months for 1000mgC/L standard
stock solutions and about 1 week for diluted standard solutions (for example, 100mgC/L).
The limitations are for cold storage in sealed containers.
Note:
IC standard solution absorbs atmospheric carbon dioxide and undergoes concentration changes. As a result, it is particularly important to store IC standard solution in a sealed container.
Prepare fresh standard solutions:
• If reproducibility of analysis values is poor or concentration fluctuates.
• If contaminants, including even small amounts of dust, are present in the standard
solution.
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TOC-VCPH/CPN
4.1 Analysis Preparation
4.1.15 Sample Preparation
4.1.15 Sample Preparation
4.1.15.1 High Sensitivity Analysis
High sensitivity analysis refers to use of the high sensitivity analysis kit to measure trace
amounts (commonly 0.5mg/L or less) of TOC in samples such as ultra-pure water. The
precautions described in the sections below should be followed when conducting trace
analysis on the order of 10 - 100µg/L.
Precautions for High Sensitivity Analysis
• Use TOC high sensitivity catalyst.
Carefully fill the combustion tube with high sensitivity catalyst to prevent contamination of the combustion tube. Measuring high-concentration samples using TOC high
sensitivity catalyst that is intended for the analysis of ultra-pure water will influence the
results of subsequent analyses on ultra-pure water samples. This is primarily caused by
remaining sample residue. The residue may be removed by running repeated analyses of
zero water.
Since removal is difficult with residual salt, alkali or highly acidic samples, a separate
combustion tube containing TOC high sensitivity catalyst should be prepared for use
only with ultra-pure water samples.
Verify that both ends of the combustion tube are sealed when storing catalyst that is to
be used only for ultra-pure water samples.
• Measure samples immediately.
Samples containing trace carbon (such as ultra-pure water) should be measured immediately after collection. If analysis cannot be performed immediately, store the sample in a
dark location at 0-10°C (without freezing) and perform analysis as soon as possible.
To collect the water, introduce water into a well-washed container, leaving no headspace, and seal the container.
• Use glass sample containers.
Glass containers are optimal for samples containing trace carbon. Commercially-available 500mL to 1 L glass screw-lid jars with Teflon seals (generally referred to as heatresistant screw-top jars or hermetic jars) are appropriate for use as water collection and
transport containers.
Note:
Exercise caution with plastic containers, as elution of TOCcontaining components can occur.
TOC-VCPH/CPN
63
4.1 Analysis Preparation
4.1.15 Sample Preparation
• Use NPOC analysis for ultra-pure water samples.
Use the NPOC method for analysis of ultra-pure water samples. Measuring TOC in
ultra-pure water samples by using the difference between TC and IC is prone to large
analysis errors for the following reasons:
• The TOC value is significantly affected since a large portion of TC often comprises
IC. Errors in TC analysis and IC analysis are additive.
• Carbon dioxide is absorbed from the atmosphere during sample collection and analysis. During the elapsed time between TC analysis and IC analysis, the sample
absorbs more carbon from the atmosphere, causing the IC result to be higher than the
IC content in the TC result. As a result, subtracting the elevated IC result from the
TC result yields a biased TOC value.
• The TOC value can also be greatly influenced if standard solutions are not prepared
and measured carefully. Errors are compounded since two calibration curves must be
generated for TC and IC.
• The calibration curves are used in sample analysis by extending a two-point calibration curve through the origin.
• In NPOC analysis, POC may be volatilized from the sample during sparging for IC
removal. This is not a problem since the ultra-pure water contains practically no
POC.
Cautions in Calibration Curve Generation and Sample Measurement Using High
Sensitivity Analysis
The case below describes the generation of a 2-point calibration curve shifted through the
origin. The calibration standard concentrations are 0µg/L and 400µg/L.
Preparation of Standard Solutions
A 2-point calibration curve using 0µg/L and 400µg/L is generated. The calibration curve is
shifted through the origin to correct for the TC contained in purified water used for
preparation of the standard solutions.
The 0µg/L and 400µg/L TC standard solutions should be prepared at the same time using
the same purified water. Wash well, two 250mL volumetric flasks with purified water
(preferably water containing low TC concentration). Carefully introduce 1mL of 100mg/L
TC standard stock solution (for a 400µg/L solution) into one of the volumetric flasks.
Distilled water is introduced up to the graduation line in both volumetric flasks.
Standard preparation procedures should be performed as quickly as possible, using caution
to avoid inclusion of external contaminants. If a water purification apparatus is the source
of purified water, allow the water to flow for a few minutes prior to use, as the initial water
will have a higher TC concentration. Alternate the flasks a number of times while filling
them with water to equalize, as much as possible, the TC concentration of the purified
water.
Use fresh purified water when filling the volumetric flask to the graduation line. Do not use
rinse bottle water that has been standing for a long period of time because the TC
concentration continually increases with time.
64
TOC-VCPH/CPN
4.1 Analysis Preparation
4.1.15 Sample Preparation
Instrument Preparation
The blank peaks present at the start of high sensitivity analysis will become progressively
smaller and gradually stabilize. As a result, calibration curves generated too soon after the
start of analysis may be inaccurate because they contain data collected during unstable
conditions. To prevent this problem, perform 5 or more measurements of purified water
containing 2-3 drops of 1M HCl per 100mL of water prior to analyzing the calibration
standards. Use the same measurement parameters (injection volume, sparge time) that will
be used for the calibration standards and samples.
Calibration Curve Analyses
Calibration curves are generated using the following two methods.
(1) Using standard solution in a 250mL volumetric flask
Insert the sample tubing directly into the volumetric flask until it reaches the bottom
of the flask. Perform analyses quickly. Four to five repeated analyses can be made
with almost no effects from the absorption of atmospheric carbon dioxide. Cover the
opening of the volumetric flask with sealing film or paraffin to prevent contamination.
Use this method when the IC value of the purified water used for standard solution
preparation (specifically, 0µg/L standard solution) is about 50µg/L or less.
(2) Sparging the standard solution
To sparge in the sample injection syringe, set the acid addition ratio to 0.5%, and the
sparge time to 2 minutes. To sparge using the optional external sparge kit, transfer
about 60mL of the standard solution to a clean sample container, add 1-2 drops of 2M
hydrochloric acid, sparge for 10 minutes and analyze.
Cover the sample container with paraffin or sealing film to prevent contamination. A
glass container with an external diameter of 24-25mm and a height of 200-250mm is
appropriate. Test tubes, stopper-equipped test tubes and chromatography tubes of
suitable size are available commercially. If the outer diameter of the container is too
large, the air-to-water contact efficiency is decreased, requiring a longer sparge time.
Ensuring that the tip of the sparge tube is near the bottom of the container will
improve the sparging efficiency.
Reference: Refer to Section 4.3.2 "Tutorial" and Section 4.4.2.2 "Calibration Curve" for detailed
descriptions of generating calibration curves using the TOC-Control V software.
Sample Analysis
Use the calibration curve generated in the previous section to measure NPOC in the sample.
Measure the sample using the same method used for the calibration standards. If the values
gradually decrease with each repeated analysis using the optional external sparge kit,
extend the sparge time to ensure sufficient sparging. The shape of the sample container, the
sample amount, the amount of sparge gas and the IC content of the sample all have a
bearing on the required sparge time. Determine the appropriate sparge time in accordance
with these parameters.
Reference: Refer to Section 4.3.2 "Tutorial" and Section 4.4.5.2 "Sample" for detailed descriptions of
conducting sample analysis using the TOC-Control V software.
TOC-VCPH/CPN
65
4.1 Analysis Preparation
4.1.15 Sample Preparation
4.1.15.2 TC Blank Check Analysis
A TOC system invariably contains substances in the instrument flow lines that produce
peaks. These peaks are referred to as blank values or system blank values, and are present
even in water samples containing absolutely no carbon. The magnitude of peaks in the
blanks differs based on various factors such as system construction and the catalyst used.
For the TOC-V, every effort has been made to minimize these peaks, which can affect the
accuracy of TC analyses. Accuracy is particularly affected when trace TOC is measured
(such as in high sensitivity analysis of ultra-pure water samples); for this type of analysis,
the blank peaks must be small and stable. To check and correct for the magnitude of the
system blank peaks, use the TOC-Control V Blank Check procedure described below.
Note:
• The Blank Check procedure is available only when the high sensitivity
catalyst is used.
• The Blank Check procedure takes approximately 8 hours to complete and
does not require continuous monitoring by the user. As a result, performing
the procedure overnight is recommended.
• Blank values measured during the Blank Check procedure should rapidly
decrease in magnitude and stabilize. If the instrument flow lines, syringe
pump interior, or catalyst have been contaminated, the blank values will not
rapidly decrease. In such instances, the Blank Check procedure should be
repeated.
• Blank peaks are negligible in the IC analysis flow line. The IC value will be
zero if the water is acidified and sparged. This can easily be confirmed by
conducting analysis using the IC flow line; however, this is not normally
necessary. Consequently, there are no special IC flow line check procedures,
as with the TC blank check.
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4.1 Analysis Preparation
4.1.15 Sample Preparation
Blank Check Procedure
1.
Open the TOC-Control V Sample Table Editor and create a blank Sample Table for
the high sensitivity system.
Note: Do not insert a sample into the Sample Table. The Blank Check
procedure only works in an empty Sample Table.
2.
3.
Connect the instrument by selecting Connect from the Instrument menu.
From the Instrument menu, select Maintenance>Blank Check.
The Blank Check Parameters dialog box is displayed.
Figure 4.22 Blank Check Parameters Dialog Box
4.
Enter the desired injection volume, and click the Start button.
The Standby dialog box is displayed.
5.
Select an option to determine the condition of the instrument after the blank check is
complete. Options are:
• Keep running
• Shut down instrument
• Auto Restart (TC furnace, carrier gas, restart time)
6.
Fill the dilution water bottle to full capacity with purified water, and place it in the
specified position. About 200mL of dilution water is used for the blank check
measurement.
7.
Click the Standby button.
The Save As dialog box is displayed.
8.
Enter a file name and click the Save button. Data from the Blank Check procedure
will be stored in the created file.
Blank check analysis begins. The procedure that the instrument executes is described
below.
Figure 4.23 Standby Dialog Box
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67
4.1 Analysis Preparation
4.1.15 Sample Preparation
Description of TC Blank Check Analysis Procedure
1.
Washing the inside of the trap
First, the trap is washed with water from the dilution water bottle. A 6mL aliquot from
the dilution water bottle is drawn into the ultra-pure water trap and the trap is emptied.
This step is repeated using another 6mL aliquot from the dilution water bottle.
Next, the trap and the system is washed with ultra-pure water. The ultra-pure water
used to wash the trap is created when a 2mL aliquot of water from the dilution water
bottle is injected through the TC injector and onto the catalyst. The ultra-pure water
resulting from the analysis fills the trap and is then drawn into the syringe and
discharged a total of 4 times.
2.
Preparation of purified water for blank check
The ultra-pure water that will be used for the Blank Check procedure is created as
follows: Six 2mL aliquots of water from the dilution water bottle are injected through
the TC injector and onto the catalyst. The ultra-pure water resulting from the analysis
is caught in the ultra-pure water trap. Water in the trap is further purified by injecting
it onto the catalyst five more times in 2mL aliquots.
3.
Blank check analysis
Using the ultra-pure water created in Step 2 and caught in the purified water trap, TC
analysis is conducted 5 times. The results of each analysis are stored in the data file.
Steps 2 and 3 are then repeated 9 more times.
Note: The magnitude and stability of the system blank value can be
evaluated from the blank check results. If the blank value is not
stable, repeat the Blank Check procedure until the magnitude of the
blank peak stabilizes.
4.1.15.3 Pretreatment for IC Removal (Sparging)
Errors for TC and IC analyses are additive. For samples that have a comparatively large IC
concentrations relative to TOC concentrations, the TOC analysis error is large if it is
determined by the difference between TC and IC results. Samples of this type include
samples from water treatment facilities or from the natural environment, such as rivers,
lakes, swamps, oceans and groundwater.
Using the difference between TC and IC to determine TOC is not appropriate for purified
water or ultra-pure water samples. The CO2 in air dissolves in the sample and is measured
as IC, causing the concentration to vary.
In such cases, the sample is pretreated with aeration or sparging before analysis to remove
the IC. The sample is then subjected to TC analysis, immediately followed by TOC
analysis using the NPOC method.
Sparge Sequence
There are two methods for sparging with this instrument.
(1) Sparging in the sample injector syringe
This is performed only when the instrument is set for automatic sparging before
analysis.
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TOC-VCPH/CPN
4.1 Analysis Preparation
4.1.15 Sample Preparation
(2) Independent sparging of sample using the optional external sparge kit
Sample is introduced into a clean sample container, acidified, and then sparged.
A glass container with an external diameter of 24-25mm and a height of 200-250mm
is appropriate for use as the sample container. Test tubes, stopper-equipped test tubes
and chromatography tubes of suitable size are available commercially. If the outer
diameter of the container is too large, the air to water contact efficiency is decreased,
requiring a longer sparge time.
Sparge Procedure
1.
Refer to Section 4.1.9 "Adjusting Sparge Gas Flow Rate" for the sparge gas delivery
procedure.
2.
3.
Add 2M hydrochloric acid to the sample to adjust the pH to 2-3.
Insert the sparge tubing into the sample.
To improve the sparging efficiency, the tip of the sparge tubing should be as close to
the bottom of the sample container as possible.
Note: In this method, sparge gas can be used independently. While the first sample is
being measured, another sample can be sparged, thereby improving analysis efficiency.
4.1.15.4 Analysis of Samples Containing Suspended Solids
Effect on Analysis
Large variations sometimes occur in TOC analyses of samples containing suspended solids
because TOC is often contained in the suspended material. This effect is evident when the
same sample is analyzed on two different TOC analyzers. Good results are not obtained if
the suspended solids are handled differently in the gathering of biochemical oxygen
demand (BOD) and TOC correlative data.
The suspended solids described here are primarily considered impurities in the sample that
will pass through a 50 mesh strainer (openings of approximately 0.28mm). When larger
solid particles are present, analysis should be performed without drawing water into the
instrument.
The procedure described below is for TOC analysis, but is also valid for TN analysis.
Analysis Restrictions
Since Teflon tubing with an inner diameter of about 0.5mm is used in the instrument for
injecting the sample, suspended solids that do not pass through cannot be measured.
Analysis reproducibility is poor for samples that do not uniformly contain such solids even
if they should pass through the tubing.
Solids that are heavy and readily form sediment, such as silt, can accumulate at the bottom
of the syringe. This can scratch the rotor of the sample injector 8-port valve, causing leaks.
Sedimentation and separation should be performed to as great an extent as possible prior to
analysis.
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4.1 Analysis Preparation
4.1.15 Sample Preparation
Countermeasures
The following types of processing operations are normally used for measuring samples
containing suspended solids.
(1) TOC Analysis of Supernatant
In situations when the suspended solids are of no great concern, sedimentation occurs
in the sample container, and the supernatant sample is used. Results depend on the
sedimentation and separation properties of the suspended solids, but usually the
dissolved TOC (DOC: dissolved organic carbon) is measured.
(2) TOC Analysis of Filtrate
The suspended solids are removed using glass fiber filter paper or a membrane filter,
and only the dissolved TOC is measured. Because the filter paper or filter itself is
likely to contain TOC, thorough washing with water or sample is performed prior to
use until no TOC is present in the eluate. Perform heat treatment on the filter for glass
fiber filter paper.
(3) TOC Analysis of Stirred Samples
To perform intentional analysis of suspended solids, the sample is stirred using a
magnetic stirrer or other instrument. Simple stirring can lead to extreme variability in
the results because the suspended solids contained in the sample may not be
distributed uniformly throughout the suspension.
(4) TOC Analysis after Homogenization of the Sample
If the application requires that the suspended solids be included in the analysis, it is
critical that the solids are as fine as possible and distributed uniformly throughout the
suspension. Accurate and reproducible TOC results can be obtained when the sample
is highly homogenized to form uniform micro-size particles.
Homogenizing systems may include a mixer to perform high-speed stirring or an
ultrasonic system. (These are homogenizers with outputs of 150-300W. Typical
washing sonicators do not have sufficient output for this use.) Ultrasonic systems are
generally more powerful, though performance varies with the type of suspended
solids.
Uniform suspension cannot always be achieved with all types of suspended solids.
Sludge-like materials are comparatively easy to process while fibrous materials are
more difficult.
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4.1 Analysis Preparation
4.1.15 Sample Preparation
4.1.15.5 Handling Samples Containing Acids, Bases or Salts
Various problems can be encountered when measuring samples that contain acids, bases or
salts. Such problems include corrosion of the NDIR analysis cell as well as detrimental
effects on analysis values and the life of the combustion tube and catalyst. If corrosion of
the inner surface of the NDIR cell occurs, baseline stability will decline and noise will
increase. Samples containing acids, bases or salts should be handled as described below.
The concentration at which adverse effects are produced varies depending on the type of
acid or salt and the TOC or TN concentration. Prior to analysis, dilute the sample so that
acid, base and salt concentrations are reduced to 1000mg/L or less. Neutralization is also
required for bases. The TOC-V is equipped with an automatic dilution function to perform
these dilutions.
Acids
Acids should be diluted to a concentration of 1000mg/L or less. Concentrations up to
5000mg/L can be used if this level of dilution cannot be reached. The acidity of
hydrochloric acid or sulfuric acid can be reduced to a pH of 2-3 with sodium hydroxide or
potassium hydroxide. This process produces thermally stable sodium chloride or sodium
sulfate, which prevent the generation of acidic gas when combusting the sample.
Neutralization of the acid is stopped at a pH of about 2-3, and TOC direct analysis (NPOC
analysis) with sparging to remove the IC is performed. It is necessary to consider the TOC
associated with impurities contained in the alkali reagents used for neutralization. All salts
of nitric acid generate acidic gas under thermal decomposition; as a result, neutralization is
ineffective. When the sample contains hydrochloric or hypochlorous acid, hydrochloric
acid gas is generated from salts that are readily subject to thermal decomposition, such as
ammonium chloride, calcium chloride and magnesium chloride. The instrument is
equipped with a halogen scrubber; however, the scrubber’s main function is absorb
hydrochloric acid gas generated by corrosion of the gold plating on the internal surface of
the NDIR cell.
Alkaline samples
When performing TC analysis on alkaline samples, the following problems can arise:
• Rapid decrease in sensitivity and loss of reproducibility
• Rapid degradation of catalyst or wear of the combustion tube
• Likelihood that IC will be high due to absorption of carbon dioxide
For these reasons, the NPOC analysis is suitable for alkaline samples.
In NPOC analysis, dilute hydrochloric acid is added to adjust the solution to a pH of 2-3,
thereby forming a salt. For example, calcium chloride will be formed as a salt if the sample
contains calcium hydroxide as the base. Since it is preferable for this salt concentration to
be low, alkaline samples should be diluted as much as possible.
Salt accumulation
Samples should be diluted as much as possible to reduce the salt concentration and extend
the life of the combustion tube and catalyst. Conducting a large number of analyses on
samples containing salts will allow the salts to accumulate in the combustion tube,
gradually increasing resistance to the flow of carrier gas and resulting in decreased analysis
reproducibility. When decreased reproducibility is observed, perform the combustion tube
maintenance procedure described in Section 5.2.3 "Washing/Replacing the Combustion
and Carrier Gas Purification Tubes".
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4.1 Analysis Preparation
4.1.16 Sample Preparation
Identifying Salt Accumulation
The following situations arise when salts accumulate and clog the catalyst:
• The sound of gas release is heard when the slider moves during analysis.
• A dramatic fluctuation in carrier gas flow is noticed after the sample is injected.
4.1.16 Sample Preparation
4.1.16.1 Vial Types
Two types of autosampler vials are available. The sample volume associated with each vial
type is shown below. Introduce the specified volume of sample into the vials; introducing
too little sample may result in insufficient sample for analysis.
Table 4.1 • Vial Types
Vial
Typical Sample Volume1
Sample Volume for NPOC Analysis2
24mL
24mL
20mL
40mL
40mL
35mL
Note 1: Sample volume when sample is introduced to the bottom of vial cap.
Note 2: Sample volume when sample is introduced to about 1cm from bottom of vial cap.
In NPOC analysis, the sample volume is decreased to reduce its contact with the sample
cap during sparging.
Note:
Vials to be used for the first time should be washed with laboratory detergent and
then rinsed well with water.
4.1.16.2 Filling Vials with Sample
In most cases, vials can be placed in the ASI-V turntable and analyzed without being
sealed. Vials must be sealed in the following situations:
(1)
(2)
(3)
(4)
(5)
(6)
(7)
(8)
(9)
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TOC-VCPH/CPN
sparging with the autosampler for NPOC analysis
measuring acidic samples
IC analysis
POC analysis
low-concentration samples (as a guideline, less than 10mg/L)
alkaline samples (pH 7 or higher)
samples that contain volatile organic hydrocarbon components
a large number of samples to be measured
standard solutions
4.1 Analysis Preparation
4.1.16 Sample Preparation
In situations (1) and (2) above, corrosion of the instrument may occur due to spattering of
sample, which contains acid. If the samples are left in the autosampler following
measurement, there is danger that the autosampler may be subjected to corrosion due to the
volatilization of acid.
In situations (3) through (9), results may be affected by either volatilization of the TOC
components in the sample or contamination from substances that absorb CO2 from the
atmosphere. If aluminum foil is used to cap the sample vial for NPOC or acidic sample
measurement, there is a danger of acid volatilization through the hole caused by insertion of
the needle. Do not use aluminum foil to cap the vials.
Methods of Sealing Vials
Two methods of sealing the vials are acceptable.
(1) Using the caps provided with the vials.
(2) Using a sealing material marketed under such names as Parafilm or Sealon Film.
Note:
Use caps only after washing them with water, or washing them with laboratory
cleaning solution and then rinsing with water.
¬Using Caps
For 24mL vials
Holed caps and seals are provided with the vials.
1.
2.
Place a seal over the vial opening.
Cap the vial over the seal.
Note: Because the seals are perforated during injection, discard the seals
after use.
For 40mL vials
Seal-equipped caps are provided with the vials.
1.
Using a seal-equipped cap provides an adequate seal for the vial.
Note: Because the seals are perforated during injection, discard the sealequipped cap after use.
¬Using Parafilm or Other Sealing Materials
Procedure
1.
2.
Cut the Parafilm or other sealing material into approximately 25 x 25mm squares.
Place a square over the opening of the vial, and stretch it to seal to the edges of the
vials.
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4.1 Analysis Preparation
4.1.16 Sample Preparation
3.
Press the edges down so that they wrap around the outside of the vial.
Be careful that
film edges do not
descend below
vial threads.
Figure 4.24 Sealing the Vial
4.1.16.3 Placing Vials in the Vial Rack
Remove the vial rack from the ASI-V before inserting the sample vials. There are three
different types of vial racks, each accommodating a different vial size.
The ASI-V permits random access of vials in the vial rack. Vials are measured according to
the sequence set in the Sample Table Editor, thus enabling analysis to start from any
position number in the vial rack, and for analysis to occur in non-sequential vial positions.
TIP »
When samples are to be sparged using the optional external sparge kit, analysis is
performed more efficiently if the vials are placed in sequential rack positions without gaps.
This allows a vial to be sparged while an adjacent vial is being measured.
Installing the Vial Rack
Install the rack using the following procedure.
1.
2.
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Insert the vials into the vial rack and place the rack on the ASI-V turntable.
Place the cover over the turntable.
Note: During analysis, the turntable must be covered. The ASI-V will not
operate if the turntable cover is not detected.
4.1 Analysis Preparation
4.1.16 Sample Preparation
4.1.16.4 High Sensitivity Autosampler Analysis
If samples with TOC concentrations of 100µg/L or less (such as purified water or ultra-pure
water) are measured using an autosampler, the following precautions associated with high
sensitivity analysis must be considered. Refer to Section 4.1.15.1 "High Sensitivity
Analysis" for additional information.
(1) NPOC analysis is recommended. TOC (TC-IC) analysis tends to have a greater
variation in measured values than the NPOC analysis because IC often accounts for a
significant portion of the TC, and the errors in the two values are additive, which
significantly affects TOC analysis.
(2) To generate a calibration curve, fill well-washed vials with standard solutions to about
5-10mm from the top of the vial, and immediately seal each vial.
Use a cap that has been washed with purified water prior to use.
When placing the vial in the rack, handle the vial carefully to avoid contact between
the standard solution and the cap.
Low-concentration standard solutions must be prepared each time they are used.
(3) To stabilize the peaks, perform 4 to 5 injections using the same analysis parameters
prior to analyzing the calibration standard solutions. For example, to generate a
400µg/L calibration curve, place a 0µg/L standard solution in vial position 1 and
measure it 4 to 5 times using the same analysis parameters that were selected for the
calibration curve. Refer to Section 4.4.4.1 "Calibration Curve". The objective at this
point is not to generate a calibration curve, but to inject water using the same injection
volume used for the calibration curve that is to be generated. This not only stabilizes
peaks but also thoroughly washes the sample needle and sparge needle with purified
water.
After the stabilizing injections are complete, place the 0µg/L and 400µg/L calibration
standard solutions in vial positions 2 and 3, insert the calibration standards into the
Sample Table Editor, and start measurement. Refer to Section 4.4.4.1 "Calibration
Curve".
(4) Acid addition for NPOC analysis can be performed automatically using the ASI-V. It
is best to perform manual addition of hydrochloric acid for NPOC analysis on the
order of 10µg/L. This is because, automatic acid addition pierces the vial seal and
allows CO2 contamination from the air.
(5) To prevent rinsing of the needle, deselect the “Rinse” option and set the “No. of
Needle Washes” field to zero in the Instrument Properties Dialog Box>ASI Window.
Refer to Section 3.2.4 "ASI Window".
Even if ultra-pure water is used as rinse water, the TOC concentration of the rinse
water will increase during the time it is exposed. For best results, do not rinse the
needle for analyses on the order of 100µg/L.
(6) Do not use the analysis value acquired from the first sample vial. In sample analysis,
particularly analysis on the order of 10µg/L, the first sample measured may yield high
results.
(7) When using the optional external sparge kit, perform sparging using a sparge gas flow
rate of 100mL/min.
As a guideline, use sparge times of 5 to 10 minutes for 24 and 40mL vials. Increase
the gas flow rate or sparge time if sparging is insufficient.
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4.1 Analysis Preparation
4.1.16 Sample Preparation
4.1.16.5 Acid Addition in NPOC Analysis
Automatic addition of acid is possible using the autosampler when the optional external
sparge kit is installed. Using the ASI-V, acidification and sparging can be performed on
samples during NPOC analysis. To perform acid addition using the autosampler, enter the
desired amount in the “Acid Addition” field on the Injection Parameters window of the
Sample Wizard (refer to Section 4.4.5.2 "Sample") or Method Wizard (refer to 4.4.2.3
"Method Wizard").
When analysis is started, acid is drawn from the acid bottle into the syringe, and the set
amount of acid is added from the sample needle into each of the vials that have been
designated for acid addition. Use 2M hydrochloric acid. The acid addition ratio (ratio of
acid with respect to sample) should be set to about 2-5%. However, a setting of about 0.5%
is used for purified water analysis.
The hydrochloric acid concentration or amount added should be adjusted in accordance
with the sample pH or buffering strength to bring the sample pH to 2-3. Prior to analysis,
verify that the pH is 2-3 using pH paper. The pH need not be checked each time if the same
type of sample is routinely measured.
CAUTION
Hydrochloric acid is a hazardous chemical. Exercise caution when handling to
prevent contact and spills. For details, refer to Section 6.9 "Material Safety Data
Sheets".
If the sample pH does not reach a value between 2 and 3, increase the acid addition ratio or
the acid concentration. Excessively increasing the acid addition ratio will result in dilution
of the sample. On the other hand, if the acid amount is too small, the size of the acid droplet
on the tip of the needle will not be large enough to drop from the needle.
Visually observe the process through the glass vial to determine if the acid droplet is
actually added to the sample.
The needle will be rinsed following each acid addition by selecting the “Rinse after acid
addition” option in the Instrument Properties Dialog Box>ASI Window. To save time
during the analysis sequence, rinsing of the needle is unnecessary if the variation in NPOC
concentration among the samples is not large.
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4.1 Analysis Preparation
4.1.16 Sample Preparation
4.1.16.6 Sparging in NPOC Analysis
Samples placed in the autosampler can be sparged by setting a sparge time if the optional
external sparge kit is installed.
If the coaxial needle is used (24mL or 40mL vials), sparging can be performed for the
specified time, followed immediately by drawing sample into the syringe and then by
analysis.
If the coaxial+sparge needle is used (24mL and 40mL vials), the next sample to be
measured can be sparged while the sample vial in the sampling position is being measured.
In this case, sparging is not performed again on the sample when it reaches the sampling
position, which does not pose a problem for ppm-level NPOC.
When measuring NPOC at the µg/L level, use the coaxial needle. This will prevent
atmospheric CO2 and other contaminants from entering the vial.
If the sparge gas flow rate is set too high, sample will be spattered onto the cap seal. Adjust
the sparge gas flow rate to avoid this undesirable spattering.
To verify that enough IC is removed during sparging using the autosampler to enable
unhindered NPOC analysis, perform IC analysis on the remaining sample following NPOC
analysis.
CAUTION
When the vials are capped and sparging is performed without automatic acid
addition via autosampler, pierce the caps before analysis by using the tip of a
provided needle or other instrument. This allows the sparge gas to vent. If sparge
gas is not vented from the vials, pressure will build inside the vials and prevent
effective sparging.
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4.1 Analysis Preparation
4.1.16 Sample Preparation
4.1.16.7 Stirrer Preparation
This section describes the procedure for enabling the optional stirrer.
Procedure
1.
2.
Open the TOC-Control V Sample Table Editor.
3.
4.
Click the ASI tab, then click in the “Stirrer On” check box to enable the stirrer.
From the Instrument menu, select Properties.
The Instrument Properties dialog box is displayed.
Click the OK button.
Adjusting the Rotation Speed
Turn the knob at the bottom of the right side of the autosampler to adjust the stirring speed.
Note:
Capabilities of the Optional ASI-V Magnetic Stirrer
• The stirrer bar rotates inside the vial to agitate and mix suspended solids in
the sample. The magnetic stirrer cannot be expected to pulverize and
homogenize suspended solids, except when they are extremely easy to crush.
Pretreatment of samples that contain suspended solids should include sample
homogenization to a point where the particles are distributed uniformly in as
small a particle size as possible. Well-homogenized samples can be measured
with good reproducibility. Stirring a non-homogeneous suspension will not
provide a uniform suspension, resulting in poor measurement reproducibility.
First apply a powerful enough homogenization process (ultrasonic waves,
etc.) to crush every particle in the sample as much as possible, and then
perform the TOC measurement.
• The ASI-V stirrer bar may not be able to sufficiently agitate and mix the
sample because of the wide variety of characteristics of suspended particles,
such as shape, specific gravity, size, strength, degree of cohesion, etc. For
example, solid particles with a high specific gravity sink to the bottom and
prevent formation of a good mixture.
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4.1 Analysis Preparation
4.1.16 Sample Preparation
Note:
Operation of the Optional ASI-V Magnetic Stirrer
• Two types of magnetic stirrers available, one for the 24mL and one for the 40mL
size vials.
• All of the vial positions may be used with 40mL vials. All positions except the
innermost row can be used with 24mL vials.
• The magnetic stirrer will only properly agitate vials in the sampling position and
the position just in front of the sampling position (advance processing position).
For example, if vial number 20 is selected, stirring is performed for vial 20 (sampling position) and vial 21 (advance processing position). The stirrer bar may not
work normally for other vial positions. The stirrer bar rotation axis may shift,
depending on the shape of the vial bottom; this has almost no effect on the effectiveness of the stirring.
• Adjust the stirrer rotation speed according to the sample properties. Use the stirrer
rotation speed adjustment control on the right side of the ASI-V.
Increasing the speed excessively may cause the stirrer bar to jump around instead
of rotate.
• Turning the stirrer on and off repeatedly, while the stirrer is set at the slowest
speed could cause the rotation speed to become uneven.
In this situation, adjust the rotation speed using the following procedure. ON /OFF
control of the stirrer is performed on the screen.
Setting the Stirrer Rotation Speed
Perform the following steps to achieve nearly equivalent rotation speeds in all of the
instruments used.
1.
2.
Turn the stirrer OFF.
3.
4.
Turn the stirrer ON and OFF several times.
Set the stirrer speed to the highest speed using the “Stirrer Rotation Speed Adjustment
Knob”.
With the stirrer ON, lower the stirrer speed.
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4.1 Analysis Preparation
4.1.17 8-Port Sampler Measurement
4.1.17 8-Port Sampler Measurement
4.1.17.1 Type of Sampler Container
There are no restrictions on the type of sample containers that can be used with the 8-Port
Sampler. It is only necessary that the containers be placed so the sample tubing from the
various ports can be inserted directly into the containers.
Note:
Wash all sample containers with an appropriate laboratory detergent, and rinse
them thoroughly with water before using them for the first time.
Loading the Sample
Although it is possible to perform measurement of a sample using the 8-Port Sampler,
while the container open, in the following situations, it is necessary to seal the sample
container.
(1)
(2)
(3)
(4)
(5)
When performing IC measurement
When performing POC measurement
When performing measurement of low concentration samples (e.g., 10 mg/L)
When performing measurement of alkali samples of pH 7 or higher
When performing measurement of samples containing volatile organic carbon
compounds
(6) When the number of samples is so great as to require a long measurement time
(7) When performing measurement of standard solutions
Note: If the sample container openings are not sealed in the situations listed above,
measurement values may be influenced by such factors as absorption of atmospheric CO2, contamination with carbon containing substances, and evaporation
of TOC constituents from the samples.
Sealing the Sample Containers
Sample containers may be sealed using commercial sealing films such as Parafilm. It is also
possible to pierce the lid of the container and insert the sample tubing into the container
through this opening.
Note:
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TOC-VCPH/CPN
In either case, wash the container with a laboratory detergent, and rinse it thoroughly with water before use.
4.1.17
4.1 Analysis Preparation
8-Port Sampler Measurement
Sealing the Container with Parafilm
1.
2.
Cut a piece of Parafilm to size according to the size of the sample vessel opening.
3.
Press the overlapping portions of the Parafilm around the neck of the opening.
Insert the tip of the sampling tube into the vessel, cover the opening with the prepared
Parafilm, and seal the opening of the vessel, stretching the Parafilm over the edges. Be
sure that a very small gap in the seal is formed to prevent creation of negative pressure
inside the vessel.
Parafilm
Figure 4.25 Sealing the Container
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4.1 Analysis Preparation
4.1.17 8-Port Sampler Measurement
4.1.17.2 High Sensitivity Using the 8-Port Sampler
If samples such as purified water or ultra-pure water, having a TOC concentration of
100ppb or less, are to be measured using the 8-Port Sampler, it is necessary to consider the
following precautions associated with high sensitivity analysis. Refer to Section 3.3.1.4
“High Sensitivity Autosampler Analysis” in the TOC-VCSH/CSN User Manual for more
information.
1)
NPOC analysis is recommended because TOC (TC-IC) analysis tends to have a
greater variation in measured values than NPOC. This is because IC often accounts
for a significant portion of the TC, and the errors in the two values are additive using
TOC (TC-IC) analysis. This affect significantly influences TOC analysis.
2)
For calibration measurement of standard solutions, fill well-washed containers
with standard solutions to about 5-10 mm from the top of the container, and
immediately seal each container. When placing the container below the 8-Port
Sampler, handle it carefully to avoid the standard solution contacting the sealing
surface. Low-concentration standard solutions must be prepared each time they
are used.
3)
To ensure that the peaks are stable for generating the calibration curve, perform
4-5 injections using the same analysis parameters prior to performing the
calibration curve analysis. For example, to generate a 400ppb calibration curve,
set 400ppb as the 1st standard solution concentration, and enter 1 as the
container number. Actually place a 0ppb solution in the container for port No. 1.
The objective at this point is not to generate a calibration curve, but to inject
water using the same injection volume that will be used to generate the
calibration curve. This not only stabilizes the instrument but also thoroughly
washes the sampling needle with purified water.
In the 2nd row of the settings screen and using the same calibration curve number
as above, set the analysis parameters for 0ppb and 400ppb. When sample measurement starts, the calibration curve to be used will be created with the correct
standard solutions.
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4.2
4.2
Setting General Measurement Parameters
4.2.1 TOC Parameter Settings
Setting General Measurement Parameters
4.2.1 TOC Parameter Settings
The following parameters must be set for analysis using the PC-controlled TOC-V
analyzer: The items available for editing change depending on the options that are installed.
•
•
•
•
•
Tubing Diameter
Buzzer
Auto regeneration of IC solution
Ready status check
TN Power Source
Setting Procedure
1.
In the TOC-Control V main window, double-click the icon for the desired instrument.
The Instrument Properties dialog box is displayed.
Figure 4.26 Instrument Properties Dialog Box: TOC Tab
2.
Click the TOC tab.
The Main Unit Version field displays the instrument version number; this field cannot
be changed by the user.
3.
Enter the parameters as described below:
Tubing Diameter
Specifies the diameter size of the sample injection tubing. Select the tubing diameter
from the drop-down list. Available options are:
• Regular: 0.5mm diameter
• Suspended Particle: 0.8mm diameter
The typical tubing diameter is 0.5mm. Select a tubing diameter of 0.8mm if the Suspended Solids kit is used.
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83
4.2 Setting General Measurement Parameters
4.2.2 ASI Parameter Settings
Buzzer
Enables the internal buzzer function. Select this option to allow the buzzer to sound
during measurement.
Auto regeneration of IC solution
Enables the automatic regeneration of IC solution. This option is enabled only when
IC measurement is being performed, and is typically selected. Refer to Section 3.2.3
"TOC Window" for a detailed description of this option.
Enable ready status check
Enables the Ready Status Check function. When the function is enabled, the software
always verifies that the instrument is in the Ready state prior to starting measurement.
Enabling the Ready Status Check function is recommended. When the function is
deselected, measurement can be performed when the instrument is not in the Ready
state, an option that is mainly for use by service personnel.
TN Power Source
Select this item if the optional TNM-1 unit is installed to perform TN analyses.
TC Furnace
Select the desired TC furnace temperature by clicking the appropriate radio button. If
“Combustion” is the selected oxidation method, select 680 or 720. If “Wet Chemical”
is the selected oxidation method, the TC Furnace field is set to Off and disabled.
4.2.2 ASI Parameter Settings
The following parameters must be set when using the ASI-V:
•
•
•
•
•
•
•
Tray type
Needle
Number of needle washes
Number of flow line washes
Rinse
Rinse after acid addition
Stirrer ON
Setting Procedure
1.
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TOC-VCPH/CPN
In the TOC-Control V main window, double-click the icon for the desired instrument.
The Instrument Properties dialog box is displayed.
4.2
2.
Setting General Measurement Parameters
4.2.2 ASI Parameter Settings
Click the ASI tab.
Figure 4.27 Instrument Properties Dialog Box: ASI Tab
3.
Enter the parameters as described below:
Tray Type
Specifies the size of the vials used in the ASI rack. Select the vial size from the dropdown list. Available options are 24mL Vial and 40mL Vial.
Needle
Specifies the type of needle used for analysis. Select the needle type from the dropdown list. Options are:
• Sample: for analysis using only a sample needle
• Sample+Sparge: for analysis using both a sample needle and a sparge needle
• Coaxial: for analysis using an integrated sample and sparge needle
• Coaxial+Sparge: for analysis using both the coaxial needle and a sparge needle,
which allows a sample to be measured while the next sample is sparged.
• The instrument does not automatically recognize the type of needle
installed. Be sure to select the type of needle that is actually installed in
the instrument.
No. of Needle Washes
Specifies the number of times the needle will be rinsed after sample injection. This
operation rinses the outside of the needle using water drawn from the dilution water
bottle. Rinsing the needle can prevent poor injection quality that results from salt
buildup at the tip of the injection tube during sample analysis. Such salt buildup is
especially problematic when analyzing samples with high salt concentrations
(1000ppm or greater).
Enter a number ranging from 0 to 10 in the No. of Needle Washes field.
Note: Needle rinsing is not required when samples contain low salt concentrations. Three rinses are recommended for samples containing
salt concentrations of 1% or more.
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4.2 Setting General Measurement Parameters
4.2.2 ASI Parameter Settings
No. of Flow Line Washes
Specifies the number of times the flow lines will be rinsed after all samples listed in
the Sample Table have been measured. This operation rinses the flow line from the
sample needle to the injection tube using water drawn from the dilution water bottle.
If the automatic acid addition option has been selected, the flow lines will be rinsed
the specified number of times following acid addition to each sample; rinsing after
acid addition removes acid that remains in the sample needle or flow lines.
Enter a number ranging from 0 to 10 in the No. of Flow Line Washes field.
Note: Typically, 2 flow line rinses are sufficient. Three to four rinses are
recommended for samples containing acid, base, or salt.
Rinse
Enables automatic rinsing of the sample needle and sparge needle between each sample using water from the dilution water bottle.
Note: • Rinsing between each sample prevents carryover from one sample to the
next. Rinsing is not necessary if all samples contain similar analyte concentrations.
• Rinsing is not recommended when analyzing ultra-pure water samples
with expected concentrations of less than a few hundred µg/L. The concentration of carbon in the rinse water may affect the sample results.
Rinsing with ultra-pure water will not reduce this effect, as the concentration of carbon in the rinse water will increase with exposure to the
atmosphere.
Rinse after acid addition
Enables automatic rinsing of the sample needle and flow lines after each acid addition.
Note: Rinsing the needle after each acid addition is not necessary if all
samples contain similar NPOC concentrations. Eliminating the
rinsing operation will save time during the analysis sequence.
Stirrer On
Enables the magnetic stirrer. Select this option to stir the samples while measurement
is being performed.
Note: Stirring a sample during measurement prevents settling or clumping of suspended solids, thereby including suspended solids when
the sample is drawn into the syringe.
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4.2 Setting General Measurement Parameters
4.2.3 Setting Default Measurement Parameters
4.2.3 Setting Default Measurement Parameters
The Default Measurement Parameters window is used to enter the default values for sample
measurement parameters. The selections made in the Default Measurement Parameters
window will be displayed as the default values when setting calibration curve and sample
measurement parameters.
Procedure
1.
2.
From the Options menu in the Sample Table Editor, select Default Measurement
Parameters.
The Default Measurement Parameters window is displayed.
Figure 4.28 Default Measurement Parameters: TC/IC/NPOC/POC/TN Tabs
Enter the following parameters on each of the applicable tabs:
• Units: Select the default concentration units for the measurement results
• No. of Injections: Enter the default minimum/maximum number of injections
• No. of Washes: Enter the default number of times the syringe is to be washed with
sample prior to the first injection. In POC analysis and IC analysis with the N-type
this refers to the number of syringe rinses using dilution water.
• Max SD: Enter the default maximum standard deviation that is acceptable for
repeat measurements. If this value is met, no additional injections are required.
However, if both this value and the Max CV value are exceeded, the samples are
automatically reinjected up to the maximum number of times specified in the No.
of Injections field. The Max SD field is disabled if the Number of Injections is 1 or
if the minimum is equal to the maximum. The default value for Max SD is 0.1.
• Max CV: Enter the default maximum coefficient of variation that is acceptable for
repeat measurements. If this value is met, no additional injections are required.
However, if both this value and the Max SD value are exceeded, the samples are
automatically reinjected up to the maximum number of times specified in the No.
of Injections field. The Max CV field is disabled if the Number of Injections is 1
or if the minimum is equal to the maximum. The default value for Max CV is 2%.
Note: The “maximum” No. of Injections field refers to the maximum
number of repeat injections to be performed when the automatic
additional measurement function is enabled. Additional measurements are performed when both the Max SD and Max CV settings
are exceeded. When both of these values are exceeded for the set
number of sample injections, the additional measurement function
is automatically activated and the sample is reinjected.
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4.2 Setting General Measurement Parameters
4.2.4 Maintenance History Settings
4.2.4 Maintenance History Settings
Enter limits for the following parameters to display a warning message when the limits are
exceeded:
• Combustion Tube Sample Injection Volume: Refers to the total volume of sample that
can be injected into the combustion tube before catalyst and combustion tube maintenance is required.
• Dilution Water: Refers to dilution water volume
• Total Acid Volume: Refers to the total volume of acid used
• Syringe Stroke: Refers to the number of syringe operations
• UV Lamp: Refers to time of operation of UV lamp
• IC Unit Pump Tubing: Refers to time of IC unit pump tubing use. The recommended
warning value is 300 hours.
• ASI Rinse Pump: Refers to time of ASI rinse pump tubing use. The recommended
warning value is 300 hours.
Procedure
1.
From the Instrument menu in the Sample Table Editor window, select
Maintenance>History.
The Maintenance History dialog box is displayed.
Figure 4.29 Maintenance History Dialog Box
TIP »
88
2.
Enter warning limits by placing the cursor in the appropriate fields and entering
numeric values.
3.
Click the OK button.
Measurement will be interrupted if the dilution water or acid reservoirs run dry during
analysis. To prevent measurement interruption, set the dilution water and total acid volume
limits to values slightly less than the remaining volume of each respective liquid. A warning
message will be generated before each liquid is completely consumed.Click the Reset
button to the right of a parameter to clear its current value.
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4.3
4.3
Measurement Procedures and Tutorial
4.3.1 Starting Up the Instrument
Measurement Procedures and Tutorial
4.3.1 Starting Up the Instrument
4.3.1.1 Turning on the Power
Turn on the power to the instrument by pressing the power key on the bottom right of the
front panel.
Note:
Press the power key again to turn off power to the instrument.
4.3.1.2 Carrier Gas Pressure
Procedure for setting the carrier gas pressure
1.
Set the supply pressure of the carrier gas to 300kPa using the pressure regulator at the
carrier gas supply source (cylinder).
Note: If compressed air or instrumentation air is used, verify that the
supply pressure is greater than 300kPa and does not exceed 600kPa.
2.
Open the front door of the instrument and adjust the carrier gas pressure to 200kPa
using the carrier gas pressure regulation knob.
Carrier Gas
Pressure Regulator
Carrier Gas Pressure
Regulation Knob
Figure 4.30 Setting the Carrier Gas Pressure
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4.3.1 Starting Up the Instrument
4.3.1.3 Carrier Gas Flow Rate
Procedure for setting the carrier gas flow rate
1.
2.
Open the front door of the instrument.
Turn the carrier gas flow adjustment knob. For H Type, adjust the flow rate to
150mL/min, as indicated on the flow rate gauge.
Carrier Gas Flow
Rate Adjustment
Knob
Flow Rate Gauge
Figure 4.31 Setting Carrier Gas Flow Rate
Note:
• Do not change the carrier gas flow rate during analysis. The peak area
changes in an inversely proportional relationship and may cause errors in
analysis precision.
• With the N Type, although the flow rate is adjusted to indicate 130mL/min on
the flow rate gauge, the actual flow rate used is 230mL/min.
4.3.1.4 Electric Furnace
The electric furnace power must be turned on for TC, TOC, NPOC, POC and TN analyses.
The electric furnace does not need to be turned on if only IC analysis is performed. When
TN analysis is conducted, the TN unit must also be turned on.
Turn On Power to the Electric Furnace
1.
In the TOC-Control V main window, double-click the icon for the desired instrument.
The Instrument Properties dialog box is displayed.
2.
3.
4.
Click the TOC tab.
Set the TC furnace temperature to either 680°C or 720°C (used for TN measurement).
Click the OK button.
The screen returns to the TOC-Control V main window.
Note: It takes 30-40 minutes after the electric furnace power is turned on for the temperature to reach the set value. Refer to Section 4.3.3 "Ending Measurement" to
turn Off the instrument,.
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Measurement Procedures and Tutorial
4.3.1 Starting Up the Instrument
4.3.1.5 TN Unit
When TN analysis is to be performed using the optional TN unit, power to the TN unit and
ozone generator must be turned on.
Turning Power to the TN Unit ON
1.
In the TOC-Control V main window, double-click the icon for the desired instrument.
The Instrument Properties dialog box is displayed.
2.
3.
4.
Click the TOC tab.
Click in the TN Power check box to select the option.
Click the OK button.
The screen returns to the TOC-Control V main window.
Turning Power to the Ozone Generator ON
1.
TIP »
Press the power switch at the lower right of the TN unit.
Power Button positions:
ON
OFF
4.3.1.6 Ozone Source Airflow Rate for the TN Unit
Adjust the ozone source airflow knob on the TN unit to indicate 500mL/min on the flow
rate gauge.
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4.3 Measurement Procedures and Tutorial
4.3.2 Tutorial
4.3.2 Tutorial
This tutorial gives step-by-step instructions on the use of the TOC-Control V software. The
tutorial assumes that the hardware and software have been installed in the manner
described in Chapters 2 and 3, and that users have a configured system that includes the
TOC-VCPH, ASI and TNM-1 unit.
Note:
• If your system does not include the ASI and TNM-1 units, please adjust the
tutorial procedure as appropriate.
In the tutorial, a three-point TC/TN calibration curve and one unknown sample will be
measured. Pure water and the following calibration standards are needed for the tutorial:
• A calibration standard mixture of 0ppm potassium hydrogen phthalate and 0ppm
ammonium chloride
• A calibration standard mixture of 50ppm potassium hydrogen phthalate and 10ppm
ammonium chloride
• A calibration standard mixture of 100ppm potassium hydrogen phthalate and 20ppm
ammonium chloride
Reference: Prepare calibration standards as described in Section 4.1.14.1 "Preparation of Standard
Solutions".
¬The following topics are covered in the tutorial:
92
Step 1
Configuring the instrument
Step 2
Connecting the instrument
Step 3
Creating a sample table
Step 4
Setting up the calibration standard runs
Step 5
Setting up an unknown sample run
Step 6
Performing measurement
Step 7
Evaluating the results
Step 8
Printing a report
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4.3
Measurement Procedures and Tutorial
4.3.2 Tutorial
¬Configuring the Instrument (Step 1)
Procedure
1.
Start the TOC-Control V software by double clicking the icon or selecting it from the
Start>Programs list.
The TOC-Control V main window is displayed.
Figure 4.32 TOC-Control V Main Window
2.
The instrument configuration must be specified in the software before the instrument
can be connected to the PC for the first time. Only users with administrative privileges
can configure the instrument. If the system has already been configured, proceed to
Step 2 of the tutorial.
3.
From the TOC-Control V main window, double-click the New System icon.
The User dialog box is displayed.
4.
Enter your user name and password as shown below.
Figure 4.33 Enter User Name and Password
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Click the OK button. The Instrument Setup Wizard opens.
Figure 4.34 Enter the Name of the System
5.
In the System Information window of the Instrument Setup Wizard, enter the System
Name and Instrument Serial Number. Click the Next button.
The Options window of the Instrument Setup Wizard is displayed.
Reference: For details on the System Name and Instrument Serial Number, refer to Section 3.2.1
"System Information Window".
Figure 4.35 Configured Options
94
6.
Specify the options that are configured on the system by clicking in the appropriate
check boxes, as shown in the above figure.
7.
Click the Next button. The TOC window of the Instrument Setup Wizard is displayed.
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8.
Measurement Procedures and Tutorial
4.3.2 Tutorial
Select the TOC analysis parameters, as shown in the figure below.
Note: Be sure that the “Enable ready status check” option is selected.
Enabling the ready status check function means that the instrument
will not begin a new injection until the instrument status is Ready.
Figure 4.36 TOC Analysis Parameters
Reference: For details on TOC parameters, refer to Section 4.2.1 "TOC Parameter Settings"
9.
Click the Next button. The ASI window of the Instrument Setup Wizard is displayed.
Verify that the ASI parameters match those shown on the figure below.
Figure 4.37 Autosampler Parameters
10. Click the Next button. The Communication window of the Instrument Setup Wizard
is displayed.
11. Verify the communication information (COM Port, Stop Bits, and Parity).
Note:
If a Shimadzu representative installed your TOC-Control V software, the correct settings for your system are already configured.
Please do not change the settings. Refer to Section 3.2.6 "Communication Window" for more information on Communication settings.
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4.3.2 Tutorial
12. Click the Next button. The History Function window of the Instrument Setup Wizard
is displayed. If desired, enable the History Log to track all changes to the method.
Refer to Section 3.2.7 "History Function Window" for more information about the
History Log.
Note: If Audit Trail was checked for the GLP/GMP 21 CFR item in
System Administration Tools of the TOC-Control V main menu,
the History Log function is automatically activated.
13. Click the Finish button.
An icon for the system now appears in the TOC-Control V main window.
TIP »
To edit the system configuration, double-click the system icon in the TOC-Control V main
window or, when in the Sample Table Editor window, select Properties from the Instrument
menu. The Instrument Properties dialog box opens, and system configuration options are
displayed on tabs in the dialog box.
¬Connecting the Instrument (Step 2)
Opening a New Sample Table
1.
In the TOC-Control V main window, double-click the Sample Table Editor
icon. The User dialog box is displayed.
2.
3.
Enter your user name and password. Click the OK button.
Open a new Sample Table by either selecting New from the File menu or clicking the
New
toolbar button. The New dialog box is displayed.
Change Graphic
Figure 4.38 Sample Run Icon
4.
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Click the Sample Run icon, then click the OK button.
The General Information dialog box opens.
4.3
5.
6.
Measurement Procedures and Tutorial
4.3.2 Tutorial
Click the System tab and select the desired system from the drop-down list.
Select Save File As in the File menu. Enter Tutorial and click the Save button.
Figure 4.39 Save As Dialog Box
7.
Click the OK button.
A new, blank Sample Table is displayed.
Figure 4.40 New Sample Table
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4.3.2 Tutorial
Connecting to the Instrument
1.
To establish communication between the software and the instrument, either select
Connect from the Instrument menu or click the Connect
toolbar button.
The Parameter Configuration dialog box is displayed. Click the Use Settings on PC
button.
The Sequence dialog box is displayed.
Figure 4.41 Connection in Progress
2.
The Sequence dialog box displays information about the attempt to establish
communication between the software and the instrument.
¬Creating a Sample Table (Step 3)
Procedure
Creating a Sample Table involves three steps. First, enter the default analysis parameters
for the Sample Table (.t32) file.
1.
2.
From the Options menu, select Default Measurement Parameters.
3.
On the TN tab change the “No. of injections” value to 3.
The other default measurement parameters should not be changed.
Three injections of each calibration standard and unknown sample will be made. On
the TC tab change the “No. of injections” value to 3.
The other default measurement parameters should not be changed.
Figure 4.42 Default Measurement Parameters Dialog Box
Note:
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The selected measurement parameters will appear as default values
when setting up calibration and method files.
4.3
Measurement Procedures and Tutorial
4.3.2 Tutorial
Reference: For details, refer to Section 4.2.3 "Setting Default Measurement Parameters".
Modify the Sample Table window display settings so that all items contained in the
Sample Table are shown on the screen. The default display settings may not include
all of the Sample Table parameters.
4.
5.
From the Options menu, select Display Settings>Table Settings.
Ensure that all items on both tabs in the Table Options window are selected. If not,
click the Select All button.
Figure 4.43 Table Options Window
Note:
6.
7.
Use this window in the future to create custom Sample Table windows that display only the desired items.
Save the Sample Table (.t32) file.
From the File menu, select Save As.
The Save As dialog box is displayed. Enter “Tutorial” as the file name and click the
Save button.
Note: The name “Tutorial” appears at the top of the Sample Table window and for the directory name after the file is saved.
The basic instrument configuration and analysis parameters have been set up.
Reference: Refer to Section 4.4 "Sample Table Editor" for detailed descriptions of the Sample Table
Editor menus and commands.
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4.3.2 Tutorial
¬Setting up the Calibration Standard Runs (Step 4)
Setting up calibration standard runs involves two steps: creating a calibration file, which
stores information about calibration standard measurements, and inserting the calibration
standard runs in the Sample Table. Separate calibration files are created for the TC and TN
analyses. The calibration is a three-point curve generated using standard mixtures of
potassium hydrogen phthalate and ammonium chloride.
Creating the TC Calibration File
1.
Open the Sample Table. From the File menu, select New.
The New dialog box is displayed. Click the Calibration Curve icon.
Figure 4.44 Creating a New Calibration File
2.
Click the OK button to open the Calibration Curve Wizard. Specific information
about the calibration will be entered in the wizard.
Figure 4.45 System for Analyses of the Calibration Standard
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4.3.2 Tutorial
Select the system to be used for the analyses from the drop-down list on page 1 of the
Calibration Curve Wizard. Click the Next button.
Page 2 of the Calibration Curve Wizard, which lists options for calibration curve type,
is displayed. The four types of calibration curves available are:
• Calibration points are distributed uniformly over the concentration range
• Edit calibration points manually
• Calibration curve according to DIN38402/P-51
• Calibration curve according to USP/EP
Figure 4.46 Calibration Curve Type
4.
Click the radio button for “Calibration points are distributed uniformly over the
concentration range.” In the future, other options may be more appropriate. Refer to
Section 4.4.2.2 "Calibration Curve" for a detailed description of the calibration curve
types.
Click the Next button.
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5.
Page 3 of the Calibration Curve Wizard is displayed. The following options for
calibration analysis are displayed:
• Analysis
• Default Sample Name
• Default Sample ID
• Calculation Method: Linear Regression or Point to Point
• Check box for Zero Shift
• Check box for Multiple Injections
• Calibration File Name
Select the following options, as shown on the figure below:
• Analysis: TC
• Default Sample Name: Standard
• Default Sample ID: Tutorial
• Calculation Method: Linear Regression
• Check box for Zero Shift: Deselect this option
• Check box for Multiple Injections: Deselect this option
• Calibration File Name: TCTutorial.cal
Figure 4.47 TC Calibration Analysis Information
6.
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Click the Next button. Page 4 of the Calibration Curve Wizard is displayed.
Notice that the No. of Injections displayed matches the number entered when setting
the default measurement parameters for the Sample Table in Step 3 of the tutorial.
4.3
7.
Measurement Procedures and Tutorial
4.3.2 Tutorial
Enter the TC calibration standard concentration range values of 0 to 100ppm.
Enter 3 as the number of calibration points.
Figure 4.48 TC Calibration Standard Information
8.
Click the Next button.
Page 5 of the Calibration Curve Wizard displays the Calibration Points List.
9.
Notice that the Calibration Points List was completed based on information entered
on the previous Wizard pages. To make any changes, select a row and click the Edit
button.
Figure 4.49 TC Calibration Points List
10. Click the Next button.
Page 6 of the Calibration Curve Wizard, which specifies peak integration parameters,
is displayed.
11. Settings can be made on this page to delay the peak detection start time or extend the
peak detection time. View but do not change the default setting on the page.
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12. Click the Next button.
Page 7 of the Calibration Curve Wizard is displayed. The History function can be
enabled on this page of the wizard. View but do not change the default setting.
13. Click the Finish button.
The Calibration Curve Wizard closes. The TC calibration curve file is now complete
and has been saved.
Creating the TN Calibration File
The TN calibration file is created by following the same steps used to create the TC
calibration file, with the exceptions described below.
1.
On page 3 of the Calibration Curve Wizard, specify the Analysis as TN and enter
“TNtutorial.cal” as the calibration file name.
Figure 4.50 TN Calibration Analysis Information
2.
On page 4 of the Calibration Curve Wizard, enter 0 to 20ppm for the Concentration
Range and 3 for the number of calibration points.
Figure 4.51 TN Calibration Measurement Parameters
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3.
Measurement Procedures and Tutorial
4.3.2 Tutorial
Page 5 of the Calibration Curve Wizard should match the following figure.
Figure 4.52 TN Calibration Points List
4.
Complete the TN calibration file by viewing but not changing pages 6 and 7 of the
Wizard and clicking the Finish button.
The TN calibration curve file is now complete and has been saved.
Reference: Refer to Section 4.4.2.2 "Calibration Curve" for a detailed description of the Calibration
Curve Wizard.
Entering the Calibration Standard Runs in the Sample Table
Now that the calibration files have been created and saved, the calibration standard runs
must be inserted into the Sample Table. The TC and TN calibration standards are inserted
separately.
1.
Insert the TC calibration standard runs by placing the cursor in the first line of the
Sample Table.
2.
3.
From the Insert menu, select Calibration Curve.
Specify the name of the TC Calibration Curve (TCtutorial.cal) and click the Open
button.
The Sparging/Acid Addition window is displayed. Notice that the TC calibration standards have been automatically added to the table.
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4.3.2 Tutorial
4.
Enter the vial positions (1-3) for the calibration standards directly into the Vial
column of the table. As vial positions are entered in the table, they are highlighted on
the tray diagram in the Sparging/Acid Addition window.
Figure 4.53 Sparging/Acid Addition Window for the ASI-V Autosampler
OCT-1 8-Port Sampler Sparging/Acid Addition Window
Figure 4.54 Sparging/Acid Window for the OCT-1 8-Port Sampler
TIP »
106
The vial position for a sample can also be entered by placing the cursor in the appropriate
row of the Sparging/Acid Addition window and then double-clicking the desired vial
position in the tray diagram.
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4.3
5.
Measurement Procedures and Tutorial
4.3.2 Tutorial
Verify the information, then click the OK button.
The Sample Table is displayed. Notice that the first row of the Sample Table now contains complete TC calibration standard measurement information.
Figure 4.55 TC Calibration Standard Information in the Sample Table
6.
Insert the TN calibration standard runs by placing the cursor in the second line of the
Sample Table.
From the Insert menu, select Calibration Curve. The Open dialog box is displayed.
Specify the name of the TN Calibration Curve (TNtutorial.cal) and click the Open
button.
Figure 4.56 Select the TN Calibration File
The Sparging/Acid Addition window is displayed. Notice that the TN calibration
standards have been automatically added to the table.
7.
Enter the vial positions for the calibration standards directly into the Vial column of
the table. Because the calibration standards are TC/TN mixtures, enter the same vial
positions (1-3) for the TN standards that were entered for the TC standards.
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4.3.2 Tutorial
8.
Click the OK button to display the Sample Table window. Notice that the second row
of the Sample Table now contains complete TN calibration standard measurement
information.
Take a moment to scroll through the completed Sample Table. Notice that the columns in the left portion of the Sample Table contain the specified analysis parameters.
Actual measurement information will appear in the columns in the right portion of the
Sample Table once the measurements are completed.
9.
Save the Sample Table by selecting Save from the File menu or by clicking the Save
button
in the toolbar.
¬Setting up an Unknown Sample Run (Step 5)
In Step 4 of the tutorial, you learned that information about calibration standard
measurement is saved in a calibration file. You also learned that setting up a calibration
standard run involves two steps: creating a calibration file and then inserting the calibration
standards into the Sample Table.
By contrast, information about unknown sample measurement is saved in a method file.
Setting up an unknown sample run involves two steps: creating a method file and then
inserting the unknown sample into the Sample Table. In this tutorial, one “unknown”
sample will be analyzed. The “unknown” sample is actually the mid-level calibration
standard (50ppm TC/10ppm TN).
Creating a Method File
1.
2.
Open the Sample Table. From the File menu, select New.
3.
Select the system to be used for the analysis from the drop-down list on page 1 of the
Method Wizard. Click the Next button.
Page 2 of the Method Wizard lists options for the analysis.
4.
Select TC/TN from the Analysis drop-down menu. Enter “Sample” in the Default
Sample Name field and “Tutorial” in the Default Sample ID field. In the File Name
field, enter “Tutorial.met” as the name of the Method File.
The New dialog box is displayed. Click the Method icon and then click the OK
button. The Method Wizard opens.
Figure 4.57 Method Wizard (Page 2) Analysis Information
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Measurement Procedures and Tutorial
4.3.2 Tutorial
5.
Click the Next button.
Page 3 of the Method Wizard specifies the calibration curves to be used to calculate
unknown sample results.
Note: It is possible to enter the calibration curve file in this screen since it
contains the data that needs to be entered on this page.
6.
Place the cursor in the Calibration Curve 1 field. Click the Browse
button.
Select the file for the TC calibration curve created previously (TCtutorial.cal).
Figure 4.58 Method Wizard (Page 3) Calibration Curves
7.
Click the Next button.
Page 4 of the Method Wizard is displayed.
Figure 4.59 Method Wizard (Page 4) Injection Parameters
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4.3.2 Tutorial
8.
The following TC analysis parameters can be entered.
• Analysis (disabled)
• Units
• Injection Volume (disabled)
• Number of Injections
• SD Max
• CV Max
• Number of Washes
• Auto Dilution
• Acid Addition
• Expected Concentration Range
• Multiple Injections
• Use blank check area
• Auto reinjection If both the CV max and SD max values have been exceeded.
9.
Click the Next button.
Page 5 of the Method Wizard is displayed. View but do not change the default settings
for options on this page.
10. Click the Next button.
The Method Wizard (Page 3) Calibration Curve screen is displayed. Enter the TN
measurement parameters.
11. Click the box beside [Calibration 1], and either select the TNtutorial.cal file or enter
the calibration curve file.
12. Click the Next button.
The Method Wizard (Page 4) Measurement Parameters screen is displayed. Set the
TN measurement parameters in the same way as for TC measurement.
13. Click the Next button.
The Method Wizard (Page 5) Peak Detection Time screen is displayed. Do not change
the default settings on this page.
14. Click the Next button.
Page 6 of the Method Wizard is displayed. View but do not change the default settings
for options on this page.
15. Click the Next button.
Page 7 of the Method Wizard is displayed. View but do not change the default settings
for options on this page.
16. Click the Finish button.
The Method Wizard closes. The method file is now complete and has been saved.
Insert the sample into the Sample Table.
Reference: Refer to Section 4.4.2.3 "Method Wizard" for a detailed description of the Method Wizard.
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4.3.2 Tutorial
17. Insert the unknown sample by placing the cursor in the third line of the Sample Table.
From the Insert menu, select Sample.
Page 1 of the Sample Wizard (Parameter Source) is displayed.
TIP »
To set up multiple analyses using a previously created method, select the Auto Generate
Table command from the Insert menu. Refer to Section 4.4.5.1 "Auto Generate".
Figure 4.60 Sample Wizard (Page 1) Parameter Sources
18. Click the Method radio button. By selecting this option, the sample will be analyzed
using the measurement parameters specified in the method file we created previously.
Enter the name of the method file (Tutorial.met) or click the Browse button to search
for the file.
Click in the “Skip remaining Wizard pages and use measurement parameters from the
source” check box. By selecting this option, the analysis parameters for the unknown
sample are copied from the source (method) file. The parameters do not need to be
entered manually and the remaining pages of the Sample Wizard do not need to be
displayed.
19. Click the Finish button.
The Sparging/Acid Addition window is displayed.
20. Enter the vial position (2) for the unknown sample (the 50ppm TC/10ppm TN
calibration standard) directly into the Vial column of the table.
21. Verify the information, then click the OK button.
The third row of the Sample Table now contains the measurement parameters for the
unknown sample. (Note that a value will not be displayed in the Result column until
measurement is complete.)
22. Save the Sample Table by selecting Save from the File menu or by clicking the Save
button
in the toolbar.
Measurement can now be performed.
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4.3.2 Tutorial
¬Performing Measurement (Step 6)
Procedure
1.
Prepare the three calibration standards (0ppm potassium hydrogen phthalate/0ppm
ammonium chloride, 50ppm potassium hydrogen phthalate/10ppm ammonium
chloride, and 100ppm potassium hydrogen phthalate/20ppm ammonium chloride) and
place them in autosampler tray vial positions 1, 2, and 3.
Note: Calibration standards and unknown samples can be placed in any
vial position when controlling the instrument with the TOC-Control
V software.
2.
Check the status of the instrument detectors before starting analysis. From the
Instrument menu, select Background Monitor, or click the Background Monitor
button on the toolbar.
The Background Monitor window is displayed; this window is used to monitor the
real time signal from the ASI and the detectors. On the TOC tab, the status of the
baseline should be OK for each parameter (position, fluctuation, and noise).
3.
Click the TN tab to check the status of the nitrogen detector.
Figure 4.61 Background Monitor
4.
5.
Close the Background Monitor window. It cannot be open during analysis.
Place the cursor in the first row of the Sample Table; this allows the measurement
sequence to begin with the TC calibration. From the Instrument menu, select Start, or
click the Start button
on the toolbar.
The Standby window is displayed.
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6.
Measurement Procedures and Tutorial
4.3.2 Tutorial
The Standby window displays 3 options:
• Keep running
• Shut down instrument
• Auto restart
Figure 4.62 Standby Window
Reference: Refer to Section 4.4.6.3 "Standby" for detailed descriptions of the Standby window options.
7.
Click the Keep Running radio button. Then Click the Standby button.
The Sparging/Acid Addition window is displayed.
8.
9.
Verify the vial positions, then click the OK button.
The Start ASI measurement window is displayed. Click the Start button to begin the
analysis.
10. The status of the measurements can be monitored during analysis by viewing the
Sample Window. To open the Sample Window, either select Sample Window from the
View menu or select the Sample Window
button on the toolbar.
Figure 4.63 Sample Window
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4.3.2 Tutorial
Note:
• The Sample Window is divided into 3 sections, as shown in the above figure.
The Graph is in the upper left corner, the Parameter Table is in the upper right
corner, and the Injection Table is the bottom half of the window. The current
injection is displayed with asterisks in the Injection Table. As each
measurement occurs, information in the appropriate Injection Table row is
completed. Previous injections are shown above the current row. Use the
scroll bar to see all of the information, and use the tabs at the bottom of the
table to toggle between analysis types (between TC and TN, in this case).
• To view the peak profile of the measurement in progress, click the asterisk of
Sample No. To view a previous measurement, click that row.
• When the Sample Window is opened, the text on the graph may be overly
enlarged. In that situation, close the Sample Window and then open it again.
• During measurement, even if “All Peaks” is selected, because it takes time for
the screen to update, the peak display may not change. In this case, select “All
Peaks” following measurement.
• When the measurement Type is TC/TN, NPOC/TN, TOC/TN or
POC+NPOC/TN, the peak profile of the selected measurement type may not
be displayed even after clicking the measurement type (for example, TC and
TN toggle) tab in the Sample Window. In that situation, click the data in the
Sample Window corresponding to the peak you wish to display.
11. Statistical information about the current set of injections is calculated and displayed in
the Sample Window. As a result, preliminary decisions about the measurements can
be made while the analysis is still in progress.
Note: Information about the current injection is shown in the status box in
the upper right portion of the Sample Window.
TIP »
The drop-down list above the graph is used to set the graph display. When Current Peak is
selected, the peak profile of the current injection is drawn in the graph as the measurement
is performed. Use this window to monitor the analysis as it occurs. The blue peak denotes
carbon, while the red peak denotes nitrogen. To see the peak profile of a previous injection,
click its row in the Injection Table. To see the peak profile of all the injections for a sample,
select All Peaks from the drop-down list at the top of the graph. Use the graph right-mouse
menu to customize the peak profile graph.
Reference: Refer to Section 4.4.4.3 "Sample Window" for a detailed description of the Sample Window
options.
12. When the measurements are complete, the autosampler moves to the rinse well for a
flow line rinse and the instrument status tab displays a Ready status. Close the Sample
Window.
¬Evaluating the Results (Step 7)
The Sample Table now contains measurement information in the columns in the right
portion of the table. Use the scroll bars to view the measurement information.
We will check the calibration curve results and then evaluate the results for the unknown
sample.
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Measurement Procedures and Tutorial
4.3.2 Tutorial
Checking the TC Calibration Curve Results
1.
Place the cursor in the first row of the Sample Table, which contains analysis
information for the TC calibration.
2.
From the View menu, select Calibration Curve, or click the Calibration Curve button
on the toolbar.
The Calibration Curve Properties window for the TC calibration is displayed.
3.
Select the Graph tab to view the TC calibration curve data in graph form.
Figure 4.64 Calibration Curve Properties: Graph Tab
The coefficient of determination (r2) value is a measure of the linearity of the
relationship between concentration and area. An r2 value was calculated for the TC
calibration and displayed in the window because we selected the linear regression
calculation when we created the calibration file. Use the r2 value to determine the
success of the calibration. A r2 value of 1 indicates a perfectly linear relationship
between concentration and area. Application methods used for future analyses may
specify an acceptable limit for the r2 value.
4.
TIP »
Select the Data tab to view calibration statistics such as Standard Deviation (SD) and
Coefficient of Variation (CV). These statistics can also be used to evaluate the success
of the calibration.
A successful calibration can be used for future analyses by specifying the calibration file
name (*.cal) in the method.
5.
Close the TC Calibration Curve Properties window when the evaluation is complete.
Checking the TN Calibration Curve Results
Evaluate the TN calibration curve results by placing the cursor in the second row of the
Sample Table, which contains analysis information for the TN calibration. Then follow
Steps 2 through 5 in the procedure listed above for evaluating the TC calibration curve
results.
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4.3 Measurement Procedures and Tutorial
4.3.2 Tutorial
Viewing Peak Profiles
1.
View peak profiles by placing the cursor in the desired row of the Sample Table and
either selecting Sample Window from the View menu or clicking the Sample button
on the toolbar.
The Sample Window is displayed; this is the same window we used to observe the
real-time injections.
2.
TIP »
To view the peak profiles for all injections in a Sample Table row, select All Peaks
from the drop-down list at the top of the graph.
All peak profiles for the selected row are displayed in the graph.
When All Peaks is selected from the drop-down list at the top of the graph, clicking in
another row of the Sample Table will automatically update the Sample Window display with
the peak profiles for that row.
3.
To view the peak profile for individual injections, click in the appropriate row of the
Injection Table and select Current Peak from the drop-down list at the top of the
graph.
Evaluating the Sample Results
1.
Place the cursor in the third row of the Sample Table, which contains analysis
information for the sample.
2.
Examine the concentration results by scrolling to the Result column in the Sample
Window.
Note: The results should be close to 50ppm for the TC analysis and
10ppm for the TN analysis.
Figure 4.65 View Sample Results
TIP »
Use the TC and TN tabs at the bottom of the Sample Information table to view the results
for both analyses.
3.
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Close the Sample Window when the evaluation is complete.
4.3
Measurement Procedures and Tutorial
4.3.2 Tutorial
Outlier Test
The Outlier Test is used to provide additional information about the measurement result.
1.
Place the cursor in the third row of the Sample Table, which contains analysis
information for the unknown sample.
2.
From the View menu, select Outlier Test.
Note: The Outlier Test is conducted to identify suspect results. The test
statistically compares all unknown samples that have the same
sample name. Because this tutorial includes only one measurement
of the unknown sample, the outlier test calculation is not
meaningful.
¬Printing a Report (Step 8)
Print a report after measurement is complete and the results have been evaluated.
Selecting the Report Items
1.
2.
From the File menu, select Page Setup.
The Page Setup window is displayed. Each tab in the window represents a section of
the report and contains several items. Selections will be made on each tab to print a
typical report for the calibration standards and unknown sample.
Reference: Refer to Section 4.4.2.15 "Page Setup" for detailed descriptions of the Page Setup options.
3.
On the Instrument tab, ensure that the Print system information check box is selected,
then select the options shown in the figure below.
Figure 4.66 Page Setup: Instrument Tab
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4.3.2 Tutorial
4.
Click the Calibrations tab and select the options shown in the figure below.
5.
Click the Samples tab and select the options shown in the figure below.
Figure 4.67 Page Setup: Calibrations Tab
Figure 4.68 Page Setup: Samples Tab
Note:
6.
TIP »
Use the default selections on the Header and Grid tabs.
Click the Miscellaneous tab and enter “Tutorial” in the Organization name field.
Select the Footer check box to include page numbers on the report.
A company logo can be added to the report header by selecting the Logo check box and
specifying the logo graphic file.
Figure 4.69 Page Setup: Miscellaneous Tab
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Measurement Procedures and Tutorial
4.3.2 Tutorial
Previewing the Report
1.
TIP »
Select the Preview button from any of the Page Setup tabs to preview the entire report
before printing.
The report can also be previewed from outside the Page Setup window by selecting Print
Preview>Sample Report from the File menu.
The Preview feature displays each page of the report exactly as it will be printed.
Notice that each item that was selected in the Page Setup window appears in the
report.
Figure 4.70 Report Appearance
TIP »
Magnify the view by clicking the magnifying glass tool, or on the Zoom In button. Move
from page to page by clicking the Next Page and Previous Page buttons.
2.
Print the report by clicking the Print button.
This ends the Tutorial.
Reference: The tutorial provided instructions for setting instrument configuration and analysis
parameters, adding calibration standard and unknown sample information to the Sample
Table, creating calibration curves and method files, conducting measurements, and
checking and printing results. More details on all of these procedures are discussed in
Section 3.2 "Instrument Setup and System Properties", Section 4.2 "Setting General
Measurement Parameters", and Section 4.4 "Sample Table Editor".
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4.3 Measurement Procedures and Tutorial
4.3.3 Ending Measurement
4.3.3 Ending Measurement
Follow the procedure below to end measurement.
Procedure
1.
From the Instrument menu, select Standby.
Figure 4.71 Standby Window
2.
Two procedures are available for ending measurement:
• Shut down instrument
• Auto restart
These procedures are described below.
Shut Down Instrument
Use the “Shut down instrument” option to end measurement and switch off power to the
instrument.
120
1.
Select “Shut down instrument” in the Standby window, then click the Standby button.
A 30-minute countdown to instrument shutdown begins. During the shutdown process, the carrier gas flow and power to the furnace are automatically turned off and
after 30 minutes, the power to the instrument is switched off.
2.
To end TN measurement, manually switch off the TN unit using the power switch
located in the lower right area of the ozone generator.
Note: When “Shut down instrument” is selected, the instrument power is
turned off and the power to the autosampler exhaust fan is turned
off. If acidic samples are being measured or if sparging is being
performed using the autosampler in NPOC measurement, there is a
danger that following measurement, volatilization of acid in the
sample could cause corrosion of the autosampler. Do not switch off
the power to the instrument. (Do not select Shutdown.)
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4.3
Measurement Procedures and Tutorial
4.3.3 Ending Measurement
Auto Restart
The Auto Restart function is used to shut down the instrument and then restart it at a
specified time. Selections are made for the date and time that measurement will next be
performed, as well as for the instrument restart settings. After shutting down the
instrument, the carrier gas flow and power to the furnace are automatically turned off.
Approximately one hour before the restart time, the furnace and the carrier gas will
automatically be turned on to allow the instrument to achieve a Ready state by the restart
time.
1.
2.
3.
Select Auto Restart in the Standby window.
Select the appropriate instrument restart settings (TC furnace, carrier gas, ozone
generator) and set the restart date and time. If a check is placed in the box beside a
unit, the furnace power remains on and the carrier gas continues to flow. In order to
have the power turned off automatically, do not place a check mark in any of these
boxes.
Click the Standby button.
Power to the instrument is automatically switched off and will be automatically
switched on approximately one hour before the restart date and time. Using Auto
Restart, measurement can be performed immediately at the specified startup time.
Reference: Refer to Section 4.4.6.3 "Standby" for detailed descriptions of the available instrument
shutdown options.
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4.4 Sample Table Editor
4.4.1 Sample Table Window Overview
4.4
Sample Table Editor
The TOC-Control V Sample Table Editor menus and commands are described in this
section.
4.4.1 Sample Table Window Overview
4.4.1.1 Toolbar Functions
If the Toolbar is not visible, select Toolbar from the View menu, then specify the desired
Toolbar options.
Note:
Many of the Toolbar functions are disabled until a Sample Table is opened or
communication is established with an instrument.
TIP »
A description of each Toolbar button’s function appears when the mouse pointer is
positioned over the button.
TIP »
All of the Toolbar commands are also accessible through the Sample Table Editor menus.
New File
Opens a new, blank Sample Table.
Open File
Opens a saved Sample Table. Clicking the button displays the Open dialog box,
in which a *.t32 file can be selected.
Save File
Saves the data in the open Sample Table. If the open Sample Table is new and has
not yet been saved, the Save As dialog box is displayed.
Cut
Removes data from highlighted cells in a table and saves them to the clipboard.
Copy
Copies data from highlighted cells in a table and saves them to the clipboard.
Paste
Copies the contents of the clipboard to a selected location in a table.
Print
Sends the data from the currently displayed window to the printer. Clicking the
button starts printing immediately using the current printer settings.
Help - About
Provides information about the TOC-Control V software.
Background Monitor
Displays the Background Monitor window, which displays the status of the ASI
and the instrument detector(s).
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4.4.1
4.4 Sample Table Editor
Sample Table Window Overview
Connect
Opens or closes the electronic connection between the instrument and the PC.
Standby
Shuts down or reactivates the instrument.
Start/Continue
Starts measurement. Either the Manual Injection Parameter or Sparging/Acid
Addition window is displayed, depending on the instrument settings.
Stop
Stops the measurement sequence after all injections of the current sample are
complete.
Halt
Immediately stops the current measurement and discards data from the interrupted measurement.
Peak Stop
Stops the measurement sequence and aborts analysis of the current sample. The
peak in progress is treated as if it were a completed analysis.
Properties
Displays the Sample/Method Properties dialog box.
Calibration Curve (View)
Displays the calibration curve data. Highlight the calibration standard row in a
Sample Table to select the calibration curve to examine.
Sample
Opens the Sample Window, which displays detailed information for each sample
injection and can be used to view measurement data in real time.
Method
Opens the Method Properties window, which contains the method parameters for
a selected sample.
Exclude
Excludes a selected sample or injection from the calculation. Toggles to include
an excluded sample.
Recalculate Highlighted
Recalculates the highlighted sample results after applying a new calibration
curve or excluding injections.
Recalculate All
Recalculates all sample results after applying a new calibration curve or excluding injections.
Delete Highlighted Data
Deletes the highlighted measurement data. This function does not change the
structure of the Sample Table.
Delete All Data
Deletes the measurement data for all samples. This function does not change the
structure of the Sample Table.
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4.4 Sample Table Editor
4.4.1 Sample Table Window Overview
Format
Displays the Floating Point Format dialog box, where options for numeric formats can be modified.
Font
Displays the Font dialog box, where options for fonts can be modified.
Insert Sample
Opens the Sample Wizard, and allows a sample to be inserted in the active position of the Sample Table.
Autogenerate
Opens the Sample Group Wizard, and allows a specified group of samples to be
inserted in the active position of the Sample Table.
Insert Control
Displays the Open dialog box, and allows a selected control sample template to
be added to the Sample Table.
Insert Calibration Curve
Displays the Open dialog box, and allows a selected calibration curve to be added
to the Sample Table.
4.4.1.2 Status Bar and Notification Bar
The Status Bar displays the status of various software functions and is displayed at the
bottom of the open window for all applications. If the Status Bar is not visible, select Status
Bar from the View menu.
The Notification Bar displays information about the status of the TOC-Control V software,
the connection between the instrument and the PC, measurement events, and operation
errors. Use the Options>Display Settings>Notification Bar Settings window to enable,
disable, or select settings for the Notification Bar. Refer to Section 4.4.9.5 "Display
Settings>Notification Bar Settings".
Notification
Bar
Status Bar
Figure 4.72 Status Bar and Notification Bar
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4.4
Sample Table Editor
4.4.2 File Menu
4.4.2 File Menu
Figure 4.73 File Menu
4.4.2.1 New
The New command opens the New dialog box, which displays the options for all new file
types. The options are Sample Run, Calibration Curve, Method, Control Sample Template,
and Parameter File, as shown in the figure below and described in the text following the
figure.
Figure 4.74 New Dialog Box
TIP »
A new file can also be created by clicking the New File button on the Toolbar and typing in
the new file name.
Sample Run
Displays the General Information window, which can also be accessed by selecting General Information from the Options menu. Refer to Section 4.4.9.1 "General Information" for a detailed description of the General Information window.
Calibration Curve
Opens the Calibration Curve Wizard, which can also be accessed by selecting
Calibration Curve from the Insert menu. Refer to Section 4.4.2.2 "Calibration
Curve" for a detailed description of the Calibration Curve Wizard.
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4.4 Sample Table Editor
4.4.2 File Menu
Method
Opens the Method Wizard. Refer to Section 4.4.2.3 "Method Wizard" for a
detailed description of the Method Wizard.
Control Sample Template
Opens the Control Sample Wizard. Refer to Section 4.4.5.3 "Control" for a
detailed description of the Control Sample Wizard. Refer to Appendix B for a
description of the Control Charts function.
Parameter File
Displays the Save As dialog box, which can be used to save a parameter file.
OK Button
Opens a new file for the selected icon, and closes the New dialog box.
Cancel Button
Press the Cancel button to close the New dialog box without making a new file.
4.4.2.2 Calibration Curve
The Calibration Curve command is used to insert a calibration curve into the Sample Table.
Selecting the command displays the File>Open dialog box.
Figure 4.75 Selecting Insert>Calibration Curve displays the File>Open dialog box
A table of calibration information is displayed in the window at the bottom of the Open
dialog box after a calibration curve is selected. Click the OK button to insert the selected
calibration curve into the Sample Table. Click the Cancel button to abort the operation.
Note:
• The Insert>Calibration Curve command is not available during sample
analysis.
• An error message is displayed if the selected file does not have the correct
format or is not a calibration curve.
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4.4
Sample Table Editor
4.4.2 File Menu
To create a new calibration curve for insertion into the Sample Table, click the New button
to open the Calibration Curve Wizard. The Calibration Curve Wizard consists of several
windows, each of which defines specific parameters for the calibration curve, as described
below.
TIP »
The Calibration Curve Wizard can also be accessed by selecting File>New and doubleclicking the Calibration Curve icon in the New dialog box.
Calibration Curve Wizard (Page 1) System Information
Figure 4.76 Calibration Curve Wizard (Page 1) System Information
Parameter
Description
System
Select the system to be used.
User
Displays the user name. This field cannot be changed.
Date of Creation
Displays the current system date and time. This field cannot
be changed.
Comment
Enter a comment (512 characters maximum).
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4.4 Sample Table Editor
4.4.2 File Menu
Calibration Curve Wizard (Page 2) Calibration Curve Type
The Calibration Curve Type window is used to specify the calibration curve type.
Figure 4.77 Calibration Curve Wizard (Page 2) Calibration Curve Type
Calibration Curve Wizard (Page 3) Analysis Information
Parameter
Description
Calibration points are distrib- Select this option to calculate the calibration point concentrauted uniformly over the con- tions automatically. The software will calculate the concencentration range
trations by distributing them in equal amounts over the
measuring range of the calibration curve.
Edit calibration points manu- Select this option to enter the calibration point concentrations
ally
manually on a subsequent Wizard page, the Calibration
Points List.
Calibration curve according
to DIN 38402/P-51
Select this option to create a calibration curve according to
DIN 38402. This type of curve consists of 10 calibration standards, with 10 injections of the lowest and highest standards
and a single injection of the intermediate standards.
Calibration curve according
to USP/EP
Select this option to create a calibration curve that consists of
2 calibration standards with concentrations between 0 and
500µg/L and one control sample with a concentration of
500µg/L.
Calibrations using automatic dilution
Dilution Factor Manual Setting
For manually setting dilution factor of standard solution.
Enter the dilution factor.
Dilution Factor Automatic
Setting
Automatically calculates dilution factor for standard solution,
and performs measurement using that dilution factor.
Use Source Dilution Function Prepares standard solution automatically inside the instrument, and performs measurement using that diluted standard
solution.
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4.4
Note:
Sample Table Editor
4.4.2 File Menu
In the case of the TOC-VCPN, dilution measurement cannot be performed for IC
measurement. Therefore, since the dilution function will not work even if Use
Source Dilution Function or Dilution Factor Manual Setting are selected, select
Dilution Factor Automatic Setting. In IC measurement using the TOC-VCPH, the
dilution function can be used.
The Analysis Information window is used to specify the type of analysis and the standard
name for the calibration curve.
Figure 4.78 Calibration Curve Wizard (Page 3) Analysis Information
Parameter
Description
Analysis
Select the analysis type.
Default Sample Name
Enter the sample name for the calibration standards (64 characters maximum).
Default Sample ID
Enter the default sample identification for the calibration
standards (64 characters maximum).
Calculation Method
Select the calculation method to be used for the calibration
from the drop-down list. Available calculation methods are
point-to-point and linear regression. Refer to Section 4.4.4.5
for detailed descriptions of the calibration methods.
Zero Shift
Select this option to shift the calibration curve through the
origin. Refer to Section 4.4.4.5 for a detailed description of
the Zero Shift option.
Multiple Injections
Select to enable the syringe to draw up a single aliquot with a
volume equal to that required for all injections of the standard. When this option is not selected, the syringe will draw
up a separate aliquot for each injection; as a result, selecting
this option reduces analysis time.
File Name
Enter the file name of the calibration curve.
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4.4 Sample Table Editor
4.4.2 File Menu
Calibration Curve Wizard (Page 4) Calibration Measurement Parameters
The Calibration Measurement Parameters window is used to specify measurement
parameters for the calibration standards.
Figure 4.79 Calibration Curve Wizard (Page 4) Calibration Measurement Parameters
130
Parameter
Description
Units
Select the concentration units from the options on the dropdown list.
Concentration Range
Enter the maximum and minimum concentrations of the calibration curve standard solutions.
No. of Cal. Points
Enter the number of calibration standards that will be used to
create the calibration curve.
No. of Injections
Enter the minimum/maximum number of injections for the
calibration standards.
No. of Washes
Specifies the number of times the syringe is to be washed
with standard prior to the first injection. Note that if the Auto
Dilution option was selected, the standard will be diluted and
the syringe will then be washed with the diluted standard.
Enter an integer from 0 to 10.
SD Max and CV Max
Specifies the maximum standard deviation and coefficient of
variation that is acceptable for the injections. Enter a value
ranging from 0 to 9999 for SD Max and from 0 to 100 for CV
Max. If either of these values are met, no additional injections are required. However, if both of these values are
exceeded, the calibration standards are automatically reinjected up to the maximum number of times specified in the
No. of Injections field. The SD Max and CV Max fields are
disabled if the No. of Injections is 1 or if the minimum is
equal to the maximum.
Sparge Time
Enter the length of time sparging will occur. (0 - 20 minutes)
Acid Addition
Enter the desired quantity of acid to be added. This option is
available only for NPOC or related analyses.
TOC-VCPH/CPN
4.4
Sample Table Editor
4.4.2 File Menu
Calibration Curve Wizard (Page 5) Calibration Points List
The Calibration Points List window displays a list of parameters for each calibration point.
The parameters can be edited by using the buttons below the list. A user must have access
rights for updating data to edit calibration information.
Figure 4.80 Calibration Curve Wizard (Page 5) Calibration Points List
Parameter
Description
No.
Displays the calibration point number. Note that the standards
will be analyzed in the order shown. To add a calibration
point at a certain position, click the desired number in the
“No.” column, then click the Add button and enter the appropriate information. The new point will be added in the specified position, and the point that was previously in that
position will move down the list to the next position.
Inj. Volume
Displays the injection volume for the calibration standards.
Calibration Points
Displays a table of measurement parameters (such as those
entered in the previous page of the Calibration Curve Wizard)
for each calibration point. To edit the parameters for a calibration point, highlight the point in the table and click the
Edit button. To add a calibration point, click the appropriate
number in the No. column to specify the insertion point, then
click the Add button. To delete a calibration point, highlight
the point in the table and click the Delete button. To delete all
calibration points, click the Delete All button.
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4.4 Sample Table Editor
4.4.2 File Menu
Click the Edit and Add buttons to display the Edit Calibration Point Parameters window.
This window is used to enter calibration points manually and to edit the parameters of
existing calibration points.
Figure 4.81 Edit Calibration Point Parameters Window
132
Parameter
Description
Calibration Point No.
Displays the calibration point number. This field will reflect
the number selected by clicking in the “No.” field in the Calibration Points List. The number cannot be changed directly in
the window.
Standard Solution Conc.
Enter the concentration of the calibration standard solution.
When creating a calibration curve from a single standard
solution by using the Auto Dilution function, enter the concentration of the original standard solution in this field.
Auto Dilution
Enter the factor by which the instrument should automatically dilute the calibration standard solution to obtain the
desired concentration for the calibration point.
Cal. Point Conc.
Displays the actual concentration of the calibration point. The
concentration is calculated automatically based on the values
entered into the Standard Solution Conc. and Auto Dilution
fields.
No. of Injections
Enter the minimum and maximum number of injections.
SD Max and CV Max
Enter the maximum standard deviation or coefficient of variation values.
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4.4
Sample Table Editor
4.4.2 File Menu
Calibration Curve Wizard (Page 6) Peak Time Parameters
The Peak Time Parameters window is used to set peak detection parameters.
Figure 4.82 Calibration Curve Wizard (Page 6) Peak Time Parameters
Setting Item
Description
Use default settings
Select this option to use the default peak detection parameters. When this option is selected, all other options in this
window are disabled.
Allowed peak start delay
The allowed peak start delay is the amount of time (in minutes) that can elapse before the analysis is stopped because a
peak is not detected. Enter a number between 0 and 20:00.
Total integration time
The total integration time is the amount of time (in minutes)
that analysis continues after the end of the peak is detected.
Enter a number between 4:50 and 20:00.
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4.4 Sample Table Editor
4.4.2 File Menu
Calibration Curve Wizard (Page 7) History
The History window is used to enable the History Log. The History Log records all
modifications to the calibration curve properties. The History Log can be set to require
users to enter comments for each modification.
If the History Log is not required, it need not be enabled, as the software operates properly
without it.
Note:
Once the History Log is enabled, it cannot be changed. All modifications to the
calibration curve properties will be tracked. If the mandatory comment option is
selected, the user will be required to enter a comment each time any parameter in
the calibration curve is modified.
Figure 4.83 Calibration Curve Wizard (Page 7) History
134
Setting Item
Description
Enable history log
Select this option to enable the software to monitor all modifications to the system. Once the History Log is enabled, it
cannot be changed if GLP is selected during installation. The
GLP laboratory guidelines require that a history of changes
be maintained for the system.
User has to comment all
modifications
Select this option to require the user to comment all modifications.
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4.4
Sample Table Editor
4.4.2 File Menu
4.4.2.3 Method Wizard
The Method Wizard is used to set method parameters and is accessed by selecting
File>New>Method. The Method Wizard consists of several windows, each of which is
described below. The Back and Next buttons are used to navigate between windows. Note
that each set of parameters selected for a specific method applies only to that method.
Note:
Selected windows in the Method Wizard will be repeated for combined analysis
types such as TOC, POC + NPOC. Each duplicate window represents one analysis type. Parameters that are not applicable to an analysis type will not appear in
the Method Wizard window.
Method Wizard (Page 1) System Information
Figure 4.84 Method Wizard (Page 1) System Information
Setting Item
Description
System
Select one of the configured instruments.
Operator
Displays the current operator name.
Date of Creation
Displays the current system time.
Comment
Enter a comment (512 characters maximum), if desired.
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4.4 Sample Table Editor
4.4.2 File Menu
Method Wizard (Page 2) Analysis Information
The Analysis Information window is used to set analysis parameters for the method being
created.
Figure 4.85 Method Wizard (Page 2) Analysis Information
136
Setting Item
Description
Analysis
Select the analysis type from the drop-down list.
Default Sample Name
Enter the default sample name (64 characters maximum).
Default Sample ID
Enter the default sample ID (64 characters maximum).
Dilution
Enter the preparation dilution factor, which will be used to
calculate concentration results. The default value is 1.
No. of Determinations
Enter the number of times each sample is to be measured.
Note that determinations and injections are different; each
determination is made up of one or more injections.
File Name
Enter the name of the new method. Click the Browse button
to save the file in a directory other than the default directory.
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4.4
Sample Table Editor
4.4.2 File Menu
Method Wizard (Page 3) Calibration Curves
The Calibration Curves window is used to specify the calibration curves that will be used to
calculate results for samples analyzed by the method. Up to 3 calibration curves can be
entered and, during analysis, the system automatically determines which curve is most
suitable for the sample. Refer to Section 6.2.5 "Automatic Selection of Optimum
Calibration Curve".
Figure 4.86 Method Wizard (Page 3) Calibration Curves
Setting Item
Description
Analysis
Displays the previously selected analysis type.
Calibration Curve 1/2/3
Enter the name of the calibration curve or click the Browse
button to select a file using the File>Open dialog box.
Skip the injection parameter
pages of the wizard
Select this item to skip the Injection Parameters window of
the Method Wizard. Use this option when the sample injection parameters will be the same as those used for calibration
curve measurements.
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4.4 Sample Table Editor
4.4.2 File Menu
Method Wizard (Page 4) Injection Parameters
The Injection Parameters window is used to specify the injection parameters for the
method.
Figure 4.87 Method Wizard (Page 4) Injection Parameters
138
Setting Item
Description
Analysis
Displays the previously selected analysis type.
Units
Select the concentration units to be used for samples.
Injection Volume
Enter the injection volume.
Expected Conc. Range
Enter the expected sample concentration if it is known.
No. of Injections
Enter the minimum/maximum number of injections for the
samples that will be analyzed using this method.
SD Max
Enter the maximum standard deviation that is acceptable for
the injections. If this value is met, no additional injections are
required. However, if both this value and the CV Max value
are exceeded, the samples are automatically reinjected up to
the maximum number of times specified in the No. of Injections field. The SD Max field is disabled if the No. of Injections is 1 or if the minimum is equal to the maximum.
CV Max
Enter the maximum coefficient of variation that is acceptable
for the injections. If this value is met, no additional injections
are required. However, if both this value and the SD Max
value are exceeded, the samples are automatically reinjected
up to the maximum number of times specified in the No. of
Injections field. The CV Max field is disabled if the No. of
Injections is 1 or if the maximum and minimum values are
the same.
No. of Washes
Enter the number of times the syringe is to be washed with
sample prior to the first injection. Note that if the Auto Dilution option was selected, the sample will be diluted and the
syringe will then be washed with the diluted sample.
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4.4
Sample Table Editor
4.4.2 File Menu
Setting Item
Description
Auto Dilution
Enter a dilution factor for the samples. The instrument will
automatically dilute the samples by this factor, and the result
will be multiplied by the factor to obtain the final concentration. The default Auto Dilution value is 1.
Sparge Time
Enter the desired sparge time. This option is available only
for POC, NPOC, and related analyses. The default Sparge
Time value is 1.
Acid Addition
Enter the desired quantity of acid to be added. This option is
available only for NPOC or related analyses.
Multiple Injections
Select to enable the syringe to draw up a single sample aliquot with a volume equal to that required for all injections of
the sample. When this option is not selected, the syringe will
draw up a separate sample aliquot for each injection. Selecting this option reduces analysis time.
Use blank check area
Select to include blank check result in the concentration calculation.
Auto correction of inj. vol.
and dilution
Select to enable the instrument to automatically adjust the
injection volume and dilution factor when the peak height for
the initial injection exceeds full scale. After the adjustment,
measurement will be repeated.
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4.4 Sample Table Editor
4.4.2 File Menu
Method Wizard (Page 5) Peak Time Parameters
The Peak Time Parameters window is used to set peak integration parameters.
Figure 4.88 Method Wizard (Page 5) Peak Time Parameters
140
Setting Item
Description
Analysis
Displays the previously selected analysis type.
Use default settings
Select this option to use the default integration parameters.
When this option is selected, all other options in this window
are disabled.
Allowed peak start delay
The allowed peak start delay is the amount of time (in minutes) that can elapse before the analysis is stopped because a
peak is not detected. Enter a number between 0 and 20:00.
Total integration time
The total integration time is the amount of time (in minutes)
that analysis continues after the end of the peak is detected.
Enter a number between 4:50 and 20:00.
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4.4
Sample Table Editor
4.4.2 File Menu
Method Wizard (Page 6) USP/EP
The USP/EP window is displayed only for TC or NPOC methods, and is used to enable
samples to be checked in accordance with USP standards. Select the check box to enable
the function.
Figure 4.89 Method Wizard (Page 6) USP/EP
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4.4 Sample Table Editor
4.4.2 File Menu
Method Wizard (Page 7) History
The History window is used to enable the History Log. The History Log records all
modifications to the method. The History Log can be set to require users to enter comments
for each modification.
Note:
Once the History function is enabled, it cannot be changed. All modifications to
the method will be tracked. If the mandatory comment option is selected, the user
will be required to enter a comment each time any method parameter is modified.
Figure 4.90 Method Wizard (Page 7) History
142
Setting Item
Description
Enable history log
Select this option to enable the software to monitor all modifications to the system. Once the history log is enabled, it
cannot be changed.
User has to comment all
modifications
Select this option to require comments or approval for all
method modifications. If the History Log is not required, it
need not be enabled, as the software operates properly without it.
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4.4
Sample Table Editor
4.4.2 File Menu
4.4.2.4 Open
The Open command is used to select and open a Sample Table, Method, Calibration Curve,
Parameter, or Control Sample Template file. Save the open Sample Table before executing
the Open command. More than one Sample Table can be opened at the same time.
Selecting the Open command displays the Open dialog box shown below.
Figure 4.91 Open Dialog Box
TIP »
The Open dialog box can also be displayed by clicking the Open File button on the Toolbar.
Table 4.2 displays the types of files that can be opened using this function. No other file
types should be opened using this menu command.
Table 4.2 • Acceptable File Types for Open Function
File Extension
Description
.t32
Sample Table
.met
Method
.cal
Calibration Curve
.tpl
Control Sample Template
.trd
Data Profile
The opened file replaces the currently displayed table or function, depending on the type of
file selected.
Dialog Box Options
Description
File name
Enter the name of the file to be opened.
Look in
Find the file to be opened by choosing the appropriate folder
or accessing other directories. The selected file will appear in
the File name text box.
Files of type
Select the type of file from the drop-down list. Choose only
files of type *.t32 when opening a Sample Table.
Open button
Opens the selected file.
Cancel button
Aborts the Open operation.
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4.4 Sample Table Editor
4.4.2 File Menu
4.4.2.5 Close
The Close command is used to close the current window and is an option only when a file is
open. If the open file has not been saved and the Close command is selected, the Save As
dialog box is displayed. Refer to Section 4.4.2.7 "Save As". Enter a name for the file and
click the OK button to save the file. If the open file has been modified but not saved and the
Close command is selected, a dialog box is displayed as shown below. Click the Yes button
to save the file before closing. Click the No button to close the file without saving the
modified information. Click the Cancel button to abort the Close command.
Figure 4.92 Dialog box for Saving Modified Data
4.4.2.6 Save
The Save command is used to save data in the current active file. If the file has not yet been
saved and the Save command is selected, the Save As dialog box is displayed. Refer to
Section 4.4.2.7 "Save As".
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The Save command can also be executed by selecting the Save File button on the Toolbar.
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4.4
Sample Table Editor
4.4.2 File Menu
4.4.2.7 Save As
The Save As command is used to save the current active file with a new file name.
Selecting the command opens the Save As dialog box shown below. Button options in the
dialog box are similar to those in the Open dialog box. Refer to Section 4.4.2.4 "Open".
Click the Save button to save the data under the specified file name. Click the Cancel
button to abort the Save As operation.
Figure 4.93 Save As Dialog Box
Dialog Box Options
Description
File name
Enter a name for the file. The applicable file extension will
automatically be added if it is not entered.
Save in
Select the directory in which the file is to be saved by choosing the folder or accessing other directories from the dropdown list. The currently selected directory appears in the
Save in text field.
Save as type
Select the type of file from the drop-down list. A list of available file types is listed in Table 4.2.
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4.4 Sample Table Editor
4.4.2 File Menu
4.4.2.8 ASCII Export Options
The ASCII Export function is used to export Sample Table data to an ASCII file. Open a
Sample Table that contains completed measurement data. Select ASCII Export from the
File menu. The Save As dialog box is displayed. Refer to Section 4.4.2.7 "Save As". Enter
a file name for the ASCII file to be created and confirm that the “Save as type” field
contains the ASCII file type (*.txt). If the entered file name matches a file that already
exists, a confirmation message is displayed.
Figure 4.94 Save As Confirmation Message
Click the Yes button to overwrite the existing file and close the dialog box. Click the No
button to redisplay the Save As dialog box and enter a new file name.
Select the ASCII Export Options command from the File menu. The ASCII Export Options
dialog box, which contains several tabs, is displayed. Each tab contains a list of export
options, as shown in the figures below. Note that on each tab, certain items are selected by
default. Individual options can be selected or deselected by clicking in the check box. Use
the Select All and Select None buttons to quickly select and deselect all options on a tab.
Use the Default button to select the default options on a tab. Click the Cancel button to exit
the ASCII Export Options dialog box without saving changes. Click the OK button to save
changes and exit the ASCII Export Options window.
Header Tab
Figure 4.95 ASCII Export Options Window: Header Tab
146
Setting Item
Description
Export header information
Select to enable export of the selected header options. This
option is selected by default.
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4.4
Sample Table Editor
4.4.2 File Menu
System Tab
Figure 4.96 ASCII Export Options Window: System Tab
Setting Item
Description
Export system information
Select to enable export of the selected system options. This
option is selected by default.
Data Tab
Figure 4.97 ASCII Export Options Window: Data Tab
Setting Item
Description
Export data
Select to enable export of the selected data options. This
option is selected by default.
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4.4 Sample Table Editor
4.4.2 File Menu
Miscellaneous Tab
Figure 4.98 ASCII Export Options Window: Miscellaneous Tab
The Miscellaneous tab contains additional options for the format of exported data. To
change data format, open a Sample Table, select File>ASCII Export Options, then select
the file to which changes should be made. On the Miscellaneous tab, select the desired type
of Separator from the drop-down list. The Separator is the type of delimiter that will be
used to separate items of data. Select the “Export strings in quotation marks” option to
enclose all of the character string items in quotation marks.
4.4.2.9 Database Export
The Database Export command is used to enable automatic export of data to an external
(Microsoft Access) database during analysis. Selecting the command displays the
Database Options window.
Figure 4.99 Database Options Window
148
Setting Item
Description
Enable automatic database
export
Select this option to enable the database export function
Database
Enter the name and filepath of the database, or click the
Browse button to select the database using the File>Open
dialog box.
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4.4
Sample Table Editor
4.4.2 File Menu
4.4.2.10 Print>Table
The Print>Table command is used to print the active Sample Table in a table format. Select
this command to open the Print dialog box, which may have a variable display depending
on the installed printer driver. Specify items to be included in the printout by using the Page
Setup command. Refer to Section 4.4.2.15 "Page Setup" for more information.
Figure 4.100 Print Dialog Box
The Name text field identifies the printer that will be used to print the table. Specify a
different printer by selecting it from the Name drop-down list.
Setting Item
Description
Properties
Modify the printer settings using standard Windows procedures.
Print range
Click the All radio button to print all pages of the table. Click
the Pages radio button and enter the page numbers to be
printed if all pages are not desired.
Number of copies
Enter the number of copies to be printed.
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4.4 Sample Table Editor
4.4.2 File Menu
4.4.2.11 Print>Sample Report
The Print>Sample Report command is used to open the Print dialog box to print the Sample
Table in report format. The print dialog box is the same as that described in Section
4.4.2.10 "Print>Table".
Figure 4.101 Print Dialog Box
4.4.2.12 Print Preview>Table
The Print Preview>Table option is used to display the sample table before printing. Use the
buttons at the top of the Print Preview window to change the display or print the table, as
described below.
Button
Description
Next Page and Previous Page Click the Next Page button to display the next page of the
report. Click the Previous page button to display the previous
page of the report. Note that the Next Page button is disabled
when the last page of the report is displayed, and the Previous
Page button is disabled when the first page of the report is
displayed.
150
One Page/Two Page
Click the One Page button to display one page at a time in the
Print Preview window. After selection, the button toggles to
the Two Page button. Click the Two Page button to display
two pages side by side.
Zoom In and Zoom Out
Click the Zoom In and Zoom Out buttons to change the magnification of the displayed pages. Three different zoom factors are available. Repeated selection of either option will
continue to increase or decrease the magnification, as applicable.
Close
Click the Close button to close the Print Preview window and
return to the previous window. Note that the Print Preview
window must be closed to edit the report.
Print
Click the Print button to print the report.
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4.4
Sample Table Editor
4.4.2 File Menu
4.4.2.13 Print Preview>Sample Report
The Print Preview>Sample Report option is used to display the sample report before
printing. Use the buttons at the top of the Print Preview window to change the display or
print the report, as described in Section 4.4.2.12 "Print Preview>Table".
Figure 4.102 Print Preview>Report Window
4.4.2.14 Print Setup
The Print Setup command is used to set print options. Select this command to open the
Print Setup dialog box, which may have a variable display depending on the installed
printer driver. Modifications to the Print Setup dialog box are saved until the TOC-Control
V software is exited.
Figure 4.103 Print Setup Dialog Box
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4.4 Sample Table Editor
4.4.2 File Menu
4.4.2.15 Page Setup
The Page Setup command is used to select items to be printed on a report or table and to
specify format parameters such as margins, headers, and footers. Selecting the command
displays the Page Setup window, which consists of several tabs. Each tab contains a list of
page setup options shown in the figures below. On each tab, certain options are selected by
default. Individual options can be selected or deselected by clicking in the check box. Use
the Select All and Select None buttons to quickly select and deselect all options on a tab.
Use the Default button to select the default options for a tab. Click the Cancel button to exit
the Page Setup window without saving changes. Click the OK button to save changes and
exit the Page Setup window.
Instrument Tab
The Instrument tab displays a list of instrument information items that can be printed on the
report.
Figure 4.104 Page Setup Window: Instrument Tab
Calibrations Tab
The Calibrations tab displays a list of calibration information items that can be printed on
the report.
Figure 4.105 Page Setup Window: Calibrations Tab
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4.4
Sample Table Editor
4.4.2 File Menu
Samples Tab
The Samples tab displays a list of sample information items that can be printed on the
report.
Figure 4.106 Page Setup Window: Samples Tab
Header Tab
The Header tab displays a list of header items that can be printed on the report.
Figure 4.107 Page Setup Window: Header Tab
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4.4 Sample Table Editor
4.4.2 File Menu
Miscellaneous Tab
The Miscellaneous tab displays a list of format items for the report, as described below.
Figure 4.108 Page Setup Window: Miscellaneous Tab
Setting Item
Description
Margins
Use the spin controls to enter the page margins (in mm).
Footer, Page No.
Select this option to print the page number in the footer of
each page.
Header
Organization: Select this option and enter the name of the
organization in the text box to print the organization name in
the page header.
Logo: Select this option to print a bitmap in the page header.
Use the Browse button to select the bitmap file.
Date/Time: Select this option to print the current system date
and time in the page header.
User: Select this option to print the current user name in the
page header.
Document name: Select this option to print the document file
name in the page header.
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4.4
Sample Table Editor
4.4.2 File Menu
4.4.2.16 Exit
The Exit command is used to exit the Sample Table Editor. If the active file has been
modified but not saved and the Exit command is selected, a dialog box is displayed as
shown below. Click the Yes button to save the file before exiting. Click the No button to
exit without saving the modified information. Click the Cancel button to abort the Exit
command.
Figure 4.109 Prompt to Save Data Changes
If the software is connected to an instrument and the Exit command is selected, a dialog
box is displayed as shown below. Click the OK button to disconnect the instrument before
exiting the software. Click the Cancel button to abort the Exit command.
Figure 4.110 Prompt to Disconnect Instrument
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4.4 Sample Table Editor
4.4.3 Edit Menu
4.4.3 Edit Menu
The Edit menu contains functions that allow a user to modify data. To change data using the
Edit menu functions, a user must have the appropriate access rights. Options such as Cut,
Copy, and Paste are available only when a content selection from an open file is made.
Figure 4.111 Edit Menu
4.4.3.1 Undo
The Undo function is used to reverse the last change made in the active Sample Table and is
only available after the user changes the content of a cell in the table. The Undo function is
not available during actual measurement or when the user has inserted or deleted completed
samples, calibration curves, or control samples.
4.4.3.2 Cut/Copy/Paste
The Cut, Copy, and Paste functions are used to edit selected Sample Table cells and rows.
The Cut command deletes selected information from rows or cells and stores it on the
clipboard. Note that the Cut command cannot be used to delete entire samples after
measurement is completed. The Copy command copies selected data from rows or cells and
stores it on the clipboard. The Paste command copies the contents of the clipboard to the
selected cells or rows of the table. When pasting an entire row, click the destination row
number to highlight the entire destination row, then execute the Paste command.
Note:
• When pasting, do not select a destination row that currently contains data.
The data will be overwritten!
• The Cut, Copy, and Paste commands can also be accessed by clicking the
icons on the Toolbar.
156
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4.4
Sample Table Editor
4.4.3 Edit Menu
4.4.3.3 Replace
The Replace function is used to replace text in Sample Table cells with specified text.
Select the Replace function to open the Replace dialog box. The Replace command can be
used to replace data in the Sample Name, Sample ID, Dilution, and Comment fields of the
Sample Table. The command cannot be used to replace data for samples after measurement
is complete.
Figure 4.112 Replace Dialog Box
Setting Item
Description
Find what
Enter the text to be searched for.
Replace with
Enter the text that the searched-for text should be replaced
with.
Match case
Select to perform a case-sensitive text search.
Find Next
Select to begin the search and to continue a search that has
already begun.
Replace
Select to replace the found text with the text in the “Replace
with” field.
Replace All
Select to replace all occurrences of found text with the text in
the “Replace with” field.
Cancel
Select to close the Replace dialog box.
4.4.3.4 Find
The Find function is used to search for specified text. Selecting the Find command opens
the Find dialog box, which is similar to the Replace dialog box.and displays the options
described below. Refer to Section 4.4.3.3 "Replace".
Setting Item
Description
Find what
Enter the text to be searched for.
Match case
Select to perform a case-sensitive text search.
Direction
Click the Up radio button to search the table backwards from
the current location. Click the Down radio button to search
the table forward from the current location.
Find Next
Select to begin the search and to continue a search that has
already begun.
Cancel
Select to close the Find dialog box.
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4.4 Sample Table Editor
4.4.3 Edit Menu
4.4.3.5 Exclude
The Exclude function is used to exclude selected injections from the calculations. A user
must have access rights for updating data to use the Exclude function. To exclude data,
highlight the desired injection shown in the Sample Window Injection Table and select
Exclude from the Edit menu. A confirmation dialog box is displayed. Click the Yes button
to exclude the selected data. Click the No button to abort the operation.
Figure 4.113 Exclude Confirmation Dialog Box
4.4.3.6 Recalculate>All
The Recalculate>All function is used to recalculate the data for all measured samples in a
Sample Table after applying a new calibration curve or excluding injections. To execute the
command, open the appropriate Sample Table and select Recalculate All from the Edit
menu. A message is displayed in the Notify folder of the Notification Bar when the
recalculation is complete.
4.4.3.7 Recalculate>Highlighted
The Recalculate>Highlighted function is used to recalculate the data for selected samples
after applying a new calibration curve or excluding injections. The function is similar to the
Recalculate All function described in Section 4.4.3.6 "Recalculate>All". To execute the
command, open the appropriate Sample Table, highlight the samples to be recalculated, and
select Recalculate Highlighted from the Edit menu.
4.4.3.8 Delete Data>All
The Delete Data>All function can only be used if the GLP conformity was disabled during
system installation. The function is used to delete all measurement data in the Sample
Table. The Sample Table structure can then be used to enter new data. A user must have
access rights for updating data to use the Delete Data>All function.
To use the Delete Data>All function, open a Sample Table that contains measurement data
and select Delete Data>All from the Edit menu. A confirmation dialog box is displayed, as
shown in the figure below. Click the Yes button to delete the data. Click the No button to
abort the operation. A message is displayed on the Notifications tab in the Notification Bar
when the data has been deleted.
Figure 4.114 Delete Data Confirmation Dialog Box
158
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4.4
Sample Table Editor
4.4.3 Edit Menu
4.4.3.9 Delete Data>Highlighted
The Delete Data>Highlighted function is used to delete the measurement data for selected
samples. To execute the command, open the appropriate Sample Table, highlight the
samples to be deleted, and select Delete Data>Highlighted from the Edit menu. A message
is displayed on the Notifications tab in the Notification Bar when the selected data has been
deleted.
4.4.3.10 Import
The Import function is used to import data from an ASCII file into a Sample Table. Note
that the Import function is not available during sample analysis. To import data, open the
destination Sample Table and place the cursor in the row of the table into which data will be
imported. Select the Import function from the Edit menu. The Open dialog box is
displayed. Select the ASCII file from which data will be imported. The data is inserted in
the current position of the active Sample Table.
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4.4 Sample Table Editor
4.4.4 View Menu
4.4.4 View Menu
The View menu contains options for viewing calibration, method, and sample information,
and for selecting settings for the display screen.
Figure 4.115 View Menu
4.4.4.1 Calibration Curve
The View>Calibration Curve command is used to view the calibration curve information
associated with a sample. Place the cursor in the desired row of the Injection Table and
select the Calibration Curve command from the View menu. The Calibration Curve
Properties window is displayed. Refer to Section 4.4.4.5 "Properties".
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The Calibration Curve Properties window can also be displayed by clicking the
Calibration Curve (View) button on the Toolbar.
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4.4
Sample Table Editor
4.4.4 View Menu
4.4.4.2 Method
The View>Method command is used to view the properties associated with a method.
Selecting the command displays the Sample/Method Properties window, which consists of
several tabs, including a separate tab for each applicable method. Each tab lists options for
method properties, as shown in the figures below. Individual options can be selected,
deselected, or edited by clicking in the check boxes or entering information into the text
fields. Note that certain options will be disabled if sample analysis is complete. Each tab
contains the same command buttons: OK, Cancel and Apply. Click the OK button to save
changes and exit the Sample/Method Properties window. Click the Cancel button to exit the
Sample/Method Properties window without saving changes. Click the Apply button to save
changes without exiting the Sample/Method properties window.
Figure 4.116 Sample/Method Properties Window: Common Tab
Common Tab
Setting Item
Description
System
Displays the system currently in use. Changes cannot be
made to this field.
User
Displays the name of the user who created the method.
Changes cannot be made to this field.
Date of Creation
Displays the date on which the method was created. Changes
cannot be made to this field.
Comment
Enter a comment (512 characters maximum).
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4.4 Sample Table Editor
4.4.4 View Menu
Parameter Tab
Figure 4.117 Sample/Method Properties Window: Parameter Tab
Setting Item
162
Description
Analysis
Displays analysis type. Changes cannot be made to this field.
Dilution
Displays the preparation dilution factor, which will be used to
calculate sample concentrations. This field can be edited.
Sample Name
Displays the default sample name (64 characters maximum).
This field can be edited.
Sample ID
Displays the default sample ID (64 characters maximum).
This field can be edited.
No. of Determinations
Displays the number of times (1-10) the sample is to be measured. Note that determinations and injections are different;
each determination is made up of one or more injections. This
field can be edited.
Perform sample checking
according to USP/EP
Select to enable USP sample checking.
Current Method
Displays the file name of the current method. Changes cannot
be made to this field.
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4.4
Sample Table Editor
4.4.4 View Menu
TC Tab
Figure 4.118 Sample/Method Properties Window: TC Tab
Setting Item
Description
Analysis Parameters
Units: Displays the concentration units. This field can be edited by selecting
another option from the drop-down list.
No. of Injections: Displays the minimum/maximum number of injections for the
samples analyzed with this method. This field can be edited.
No. of Washes: Displays the number of times the syringe is to be washed with
sample prior to the first injection. Note that if the Auto Dilution option was
selected, the sample will be diluted and the syringe will then be washed with the
diluted sample. This field can be edited.
SD Max: Displays the maximum standard deviation. If this value is met, no
additional injections are required. However, if both this value and the CV Max
value are exceeded, the samples are automatically reinjected up to the maximum number of times specified in the No. of Injections field. This field can be
edited.
CV Max: Displays the maximum coefficient of variation. If this value is met, no
additional injections are required. However, if both this value and the SD Max
value are exceeded, the samples are automatically reinjected up to the maximum number of times specified in the No. of Injections field. This field can be
edited.
Acid Addition: Displays the quantity of acid to be added to each sample. This
value is expressed as a percent or the sample volume and is available only for
NPOC and related analyses. This field can be edited.
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4.4 Sample Table Editor
4.4.4 View Menu
Setting Item
Description
Peak Time Parameters
Use default settings: Select this option to use the default settings for peak integration.
Allowed peak start delay: Displays the amount of time (in minutes) that can
elapse before the analysis is stopped because a peak is not detected. This field
can be edited by entering a number between 0 and 20:00. This option is disabled
when Use default settings is selected.
Total integration time: Displays the amount of time (in minutes) that analysis
continues after the end of the peak is detected. This field can be edited by entering a number between 4:50 and 20:00. This option is disabled when Use default
settings is selected.
Multiple Injections
Select this option to enable the syringe to draw up a single sample aliquot with a
volume equal to that required for all injections of the sample. When this option
is not selected, the syringe will draw up a separate sample aliquot for each
injection; as a result, selecting this option reduces analysis time.
Auto correction of inj.
volume and dilution
Select this option to enable the instrument to automatically adjust the injection
volume and dilution factor when the peak height for the initial injection exceeds
full scale. After the adjustment, measurement will be repeated.
Auto Dilution
Displays the factor by which the instrument will automatically dilute the sample. This field can be edited.
Inj. Volume
Displays the injection volume. This field can be edited.
Expected Conc. Range
Enter the expected concentration if it is known.
Use area retrieved from Select to include blank check result in the concentration calculation.
the blank check
Calibration Curve 1/2/3 Displays the name(s) of calibration curve(s) used to quantitate samples analyzed by the method. These fields can be edited by entering a calibration curve
file name or clicking the Browse button to search for the file.
IC Tab
The IC tab options are similar to those described above for the TC tab.
Figure 4.119 Sample/Method Properties Window: IC Tab
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4.4
Sample Table Editor
4.4.4 View Menu
NPOC and POC Tabs
The NPOC and POC tab options are similar to those described above for the TC tab.
Figure 4.120 Sample/Method Properties Window: NPOC Tab
TN Tab
The TN tab options are similar to those described above for the TC tab, except that some
options (such as Use area retrieved from blank check) are not available for TN
measurements.
Figure 4.121 Sample/Method Properties Window: TN Tab
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4.4 Sample Table Editor
4.4.4 View Menu
History Tab
If the History Log was enabled when the method was created, the History tab displays a list
of changes made to the method parameters. If the History Log was not enabled previously,
it can be enabled on the History tab.
Figure 4.122 Sample/Method Properties Window: History Tab
Setting Item
Description
Enable history log
Select this option to enable the software to monitor all modifications to the system. If the History Log is not required, it
need not be enabled, as the software operates properly without it. Once this is enabled, it cannot be disabled.
User has to comment all
modifications
Select this option to require comments or approval for all
modifications. If the History Log is not required, it need not
be enabled, as the software operates properly without it. Once
this is enabled, it cannot be disabled.
ACSII Export
The displayed items in the list are exported as tab-deliminated text files.
A list of the Comment dialog box contents is shown below:
Table 4.3 • Comment dialog box contents
166
Item
Description
Date/Time
Displays the date and time of the modification.
User
Displays the user who made the modification.
Changed item
Describes the parameter that changed.
From
Displays the previous parameter value.
To
Displays the new parameter value.
Comment
Lists the reason for the modification.
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4.4
Sample Table Editor
4.4.4 View Menu
4.4.4.3 Sample Window
The Sample Window is used to display detailed measurement information. The information
displayed in the Sample Window varies based on the type of analysis performed. To view
the Sample Window, open a Sample Table, place the cursor in the row of the Sample Table
that contains the desired sample, and select Sample Window from the View menu. The
Sample Window is displayed.
TIP »
To view measurement data in real time, place the cursor in the row of the Sample Table that
contains the current sample, then open the Sample Window.
The Sample Window is divided into 3 sections: the Graph, the Parameter Table, and the
Injection Table. Note that the sections can be resized by dragging the dividers between
sections.
Figure 4.123 Sample Window
Graph
The upper left section of the Sample Window displays the peak profile graph. Change the
graph type by choosing from the options on the drop-down list.
Setting Items
Description
Current Peak
Displays the peak profile of the highlighted injection.
All Peaks
Displays all injection peaks for the selected sample.
Calibration curve
Displays calibration curves (for calibration standards only).
This function is not available during real-time analysis
Note:
To view the peak profile of the measurement in progress, click the row with the
asterisk in the Sample No. column. To view a previous measurement, click the
desired row.
Parameter Table
The upper right section of the Sample Window displays sample parameters.
Setting Item
Description
Sample Name
Displays the name of highlighted sample.
Sample ID
Displays the sample identification from the Sample Table.
Analysis
Displays the analysis method used for the sample.
Result
Displays the sample concentration.
Dilution Factor
Displays the dilution factor. The result will be multiplied by
this factor to calculate the final concentration. If the sample
was not diluted, do not change the default value of 1.
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4.4 Sample Table Editor
4.4.4 View Menu
Injection Table
The lower section of the Sample Window displays the Injection Table, which contains
detailed information about the injections performed for the selected sample. Asterisks are
displayed in the Injection Table for the injection that is currently being measured. Some
columns in the Injection Table use the Merge Cell function to display information that is
common to all the injections of a particular sample. If the sample has been analyzed by
more than one analysis method, the Injection Table contains several folders displayed as
tabs at the bottom of the window. The columns in the Injection Table are described below.
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Setting Items
Description
Spl. No.
Displays the sample number.
Inj. No.
Displays the injection number.
Area
Displays the area value.
Mean area
Displays the mean area value for all injections of the sample.
Conc.
Displays the concentration obtained for the injection.
Mean Conc.
Displays the mean concentration obtained for all injections of
the sample.
Result
Displays the analysis result.
Notes
Displays any analysis flags or notations associated with that
sample.
SD Area
Displays the standard deviation calculated from the area.
CV Area
Displays the coefficient of variation calculated from the area.
SD Conc.
Displays the standard deviation calculated from the concentration.
CV Conc.
Displays the coefficient of variation calculated from the concentration.
Status
Displays the analytical status, either “measuring” or “finished”.
Vial
Displays the vial number (for ASI samples only).
Excluded
Displays the exclusion flag, denoted as “E” for user exclusion
of the sample, “ES” for exclusion by the system, or “Not
Excluded”.
Modified
Displays the modification flag of “M” if the sample was
modified.
Inj. Volume
Displays the injection volume for each injection.
Dilution Factor
Displays the dilution factor used in measurement.
Calibration curve
Displays the calibration curve used.
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Sample Table Editor
4.4.4 View Menu
4.4.4.4 Outlier Test
The Outlier Test (also known as the Grubb test) is used to determine whether a selected
injection is an outlier. The test also determines whether the injection with the highest
deviation from the mean value is still within an acceptable range. The Outlier Test can only
be performed if the sample contains at least three non-excluded injections.
Figure 4.124 Outlier Test Window
To perform the Outlier Test, open the Sample Window and select the cells containing the
data to be tested. From the View menu, select Outlier Test. The Outlier Test window is
displayed. Select either Conc. or Area (CNV) for the data source. Exclude the injection that
is suspected of being an outlier, then select OK to close the dialog box.
If the sample does not contain enough injections for the test to be performed, an error
message is displayed and the Outlier Test window will not open.
The Outlier Test window contains the parameters listed below.
Setting Items
Description
Result List
Displays the result of the Outlier Test.
Conc. radio button
Select to indicate that test calculations are to be performed
based on the concentration data.
Area (CNV) radio button
Select to indicate that test calculations are to be performed
based on the area data.
Result
Displays the result of the test.
Exclude button
Click this button to exclude a suspect sample and recalculate
the test result.
Suspicious inj.
Indicates the injection suspected of being an outlier, which is
identified as the sample with the highest deviation from the
mean value.
SD
Displays the standard deviation for all of the injections.
CV
Displays the coefficient of variation for all of the injections.
Grubb Value
Displays the corresponding value from the Grubb table.
Test Value
Displays the calculated Outlier Test value.
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4.4 Sample Table Editor
4.4.4 View Menu
4.4.4.5 Properties
The View>Properties function displays various windows. The display depends on the
content of the cell selected in the Sample Table. If a range of cells is selected, the upper left
cell is considered the active cell. The table below shows the possible selections and the
corresponding Properties windows.
Table 4.4 • Properties Windows
Content of Active Cell
Properties Window
Calibration Curve
Calibration Curve Properties window
Method
Sample/Method Properties window
Any other cell for a sample
Sample/Method Properties window
Any other cell of a control
sample
Control Sample Properties window
The Properties window contains options for viewing and modifying the method, calibration
curve, and sample properties. Each Properties window consists of several tabs. The
Calibration Curve Properties window tabs are shown and described below.
Calibration Curve Properties Window
Figure 4.125 Calibration Curve Properties Window: The Common Tab
Common Tab
The Common tab of the Calibration Curve properties window contains the following
information about the calibration curve.
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Setting Item
Description
System
Displays the system used to create the calibration curve. This
field cannot be edited.
User
Displays the name of the user who created the calibration
curve.
Date of Creation
Displays the date and time the calibration curve was created.
Comment
A comment regarding the calibration curve may be entered
here.
Print
Prints the calibration curve information.
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4.4
Sample Table Editor
4.4.4 View Menu
Parameter Tab
Figure 4.126 Calibration Curve Properties Window: Parameter Tab
Setting Item
Description
Analysis
Displays the analysis method used to create the calibration curve. This field cannot be edited.
Unit
Displays the concentration units. This field cannot be edited.
Sample Name
Displays the default sample name used for the calibration standards (64 characters
maximum). This field can be edited.
Sample ID
Displays the default sample ID (64 characters maximum). This field can be edited.
No. of Cal. Points
Displays the number of calibration standards used. This field cannot be changed.
Catalyst Type
Displays the type of catalyst used.
Calibration Curve
Type
Displays the calibration curve type. This field cannot be changed.
Calculation Method
Displays the calibration curve calculation method. This field can be edited by
selecting a different option from the drop-down list. Two calculation methods are
available: point-to-point and linear regression. For both types, a curve representing the relationship between detector response and concentration is displayed.
The point-to-point curve fit draws a straight line between adjacent data points and
considers each line segment to be a separate calibration line governed by its own
equation. A linear regression statistically determines the line that best fits the pattern of all data points. The number used to describe the agreement between the
calculated line and the data points is called the Coefficient of Determination (r2).
A coefficient of 1 indicates that the line fits the data points perfectly.
The general equation for a straight line is:
Y = mX + b
where: Y = Y-axis data point
X = X-axis data point
m = slope of line
b = Y-axis intercept point
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4.4 Sample Table Editor
4.4.4 View Menu
Setting Item
Description
Zero Shift
Select Zero Shift to shift the regression curve through the origin. Note that this
option does not change the slope of the line. Use this option as a correction when
the TC content in the Zero water used to prepare the calibration standards is too
large to ignore.
Multiple Injections
Select to enable the syringe to draw up a single aliquot with a volume equal to that
required for all injections of the standard. When this option is not selected, the
syringe will draw up a separate aliquot for each injection; as a result, selecting this
option reduces analysis time.
Calibration Curve
File
Displays the file name of the calibration curve. This field cannot be changed.
Analysis Tab
The Analysis tab displays additional analysis parameters.
Figure 4.127 Calibration Curve Properties Window: Analysis
Analysis Parameters
172
Setting Item
Description
No. of Washes
Displays the number of times (0-10) the syringe is washed with standard
prior to the first injection. Note that if the Auto Dilution option was
selected, the standard will be diluted and the syringe will then be washed
with the diluted standard. This option is not available for SSM. This field
can be edited.
Acid Addition
Displays the quantity of acid to be added to each standard prior to injection. This value is expressed as a percent of the sample volume and is
available only for NPOC or related analyses. This field can be edited.
Sparge Time
Displays the pre-sparge time (0-20 minutes). This option is only available when the external sparge kit is installed and the analysis type is
NPOC. This field can be edited.
Density:
Displays the sample density. This option is available only for SSM.
By Weight/Volume:
Displays the basis (Weight or Volume) for sample calculations. This
option is available only for SSM.
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4.4
Sample Table Editor
4.4.4 View Menu
Peak Time Parameters
Setting Item
Description
Use default settings
This option is selected if the default settings are used for peak
integration.
Allowed peak start delay
Displays the amount of time (in minutes) that can elapse
before the analysis is stopped because a peak is not detected.
Total integration time
Displays the amount of time (in minutes) that analysis continues after the end of the peak is detected.
Data Tab
The Data tab displays information about each calibration standard used in the calibration
curve.
Figure 4.128 Calibration Curve Properties Window: Data Tab
Setting Item
Description
Auto Dilution
Displays the auto dilution factor.
Inj. Volume
Displays the injection volume, which varies depending on the
analysis type.
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4.4 Sample Table Editor
4.4.4 View Menu
Columns of data are displayed in a window below the Inj. Volume selection, as described
below.
Table 4.5 • Data Tab Columns
Column Name
Description
Auto Dilution
Displays the dilution factor for auto dilution.
Standard Solution Concentra- Displays the concentration of the standard solution used for
tion
analysis.
No.
Displays the calibration point number.
Conc.
Displays the concentration of calibration point.
Mean Area
Displays the mean area value from all non-excluded injections
No. of Injections
Displays the minimum and maximum number of injections.
Excluded
“E” indicates calibration point has been excluded.
SD Max
Displays the maximum standard deviation.
CV Max
Displays the maximum coefficient of variation.
SD
Displays the standard deviation.
CV
Displays the coefficient of variation.
Additional buttons are displayed, below the data columns and can be used to manipulate the
calibration parameters. The buttons are described below. Refer to Section 4.4.2.2
"Calibration Curve" for more detailed descriptions.
174
Button
Function
Edit
Edit the parameters for the selected calibration point.
Add
Add a new calibration point.
Delete
Delete the selected calibration point.
Delete All
Delete all calibration points.
Exclude
Exclude the selected calibration point.
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4.4
Sample Table Editor
4.4.4 View Menu
Graph Tab
The Graph tab displays the calibration curve in a graphic format.
Figure 4.129 Calibration Curve Properties Window: Graph Tab
Setting Item
Description
Slope/Intercept/r^2
The values for Slope, Intercept, and r2 are displayed for the
selected calibration curve.
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4.4 Sample Table Editor
4.4.4 View Menu
History Tab
If the History Log was enabled when the calibration curve was created, the History tab
displays a list of changes made to the calibration curve parameters. If the History Log was
not enabled previously, it can be enabled on the History tab.
Figure 4.130 Calibration Curve Properties Window: History Tab
Setting Item
Description
Enable history log
Select this option to enable the software to monitor all modifications to the system. If the History Log is not required, it
need not be enabled, as the software operates properly without it. Once this is enabled, it cannot be disabled.
User has to comment all
modifications
Select this option to require comments or approval for all
modifications.f the History Log is not required, it need not be
enabled, as the software operates properly without it. Once
this is enabled, it cannot be disabled.
ACSII Export
The displayed items in the list are exported as tab-deliminated text files.
A list of the Comment dialog box contents is shown below:
Table 4.6 • Comment dialog box contents
176
Item
Description
Date/Time
Displays the date and time of the modification.
User
Displays the user who made the modification.
Changed item
Describes the parameter that changed.
From
Displays the previous parameter value.
To
Displays the new parameter value.
Comment
Lists the reason for the modification.
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4.4
Sample Table Editor
4.4.4 View Menu
4.4.4.6 Customize
The View>Customize window contains two tabs, one that displays or hides the toolbars and
one that customizes the toolbar content.
Figure 4.131 Customize Window: Toolbars Tab
Toolbars Tab
Select the desired toolbars from the list. All items are selected by default.
Option
Description
Show Tooltips
Displays tooltips when the mouse cursor is positioned over
the toolbar button.
Cool Look
Select this option to display the toolbar buttons as flat buttons. This item is selected by default.
Large Buttons
Select this option to display the toolbar buttons in a larger
size.
New button
Click this button to create a user-defined toolbar button.
Reset/Delete button
Click this button to reset the toolbar display to its original
state or delete a user-defined toolbar button.
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4.4 Sample Table Editor
4.4.4 View Menu
Command Tab
Figure 4.132 Customize Window: Command Tab
Option
Description
Categories
Displays the available toolbars.
Buttons
Displays the buttons in the selected toolbar. The buttons can
be moved by dragging them to another toolbar.
Description
Displays a description of the selected button.
4.4.4.7 Toolbar
The View>Toolbar function is used to select or deselect individual toolbars for display.
Toolbar display options (such as button size or appearance) can also be set using this
command.
Figure 4.133 Toolbar Window
4.4.4.8 Status Bar
The View>Status Bar function toggles the display state of the status bar between Show and
Hide. If the status bar is currently displayed, selecting this option will hide the status bar. If
the status bar is not displayed, selecting this option will display the status bar.
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4.4
Sample Table Editor
4.4.4 View Menu
4.4.4.9 ASI / 8-Port Sampler Vials
This function displays the ASI or 8-Port Sampler dialog box, and allows the user to enter
vial numbers for measurement using the ASI or the 8-Port Sampler. To access this
command, either create or open a sample table, and select View > ASI / 8-Port Sampler
Vials. The Sparge / Acid Addition dialog box opens automatically when the Start command
is made. The OK button saves the changes and closes the dialog box.
Using the Autosampler
Figure 4.134 Sparge / Acid Addition Dialog Box for the ASI-V Autosampler
Using One 8-Port Sampler
Figure 4.135 Sparge / Acid Addition Dialog Box for One 8-Port Sampler
Using Two 8-Port Samplers
Figure 4.136 Sparge / Acid Addition Dialog Box for Two 8-Port Samplers
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4.4 Sample Table Editor
4.4.4 View Menu
When the mouse is positioned over a vial in the drawing of the of ASI or 8-Port Sampler, a
tool-tip showing the vial number is displayed. Click the vial to display the following items.
Parameter
TIP »
Description
Vial No.
Displays the currently selected vial number.
Acid Addition rate
Displays the acid addition rate for each vial.
Sparge time
Displays the sparge time for each vial.
Total injection volume
Displays the total injection volume for each vial.
The desired vial position for a sample can be entered either directly into the Vial column or
by placing the cursor in the appropriate row of the Sparging/Acid Addition window and
then double-clicking the desired position in the tray diagram.
4.4.4.10 Data Profile
Displays the raw measurement data. The data profile is never modified or processed
following the initial collection. It includes the corresponding measurement parameters. The
files which were created and named using the object ID, each occupy a row in the sample
table, and are stored within the RawData folder in folders named using the date of creation.
The View>Data Profile function is used to view the data profile for a sample. Highlight the
desired row of the Sample Table, then select the command.
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4.4
Sample Table Editor
4.4.5 Insert Menu
4.4.5 Insert Menu
The Insert menu contains options for inserting sample groups, calibration curves,
individual samples, and control samples into the Sample Table.
Figure 4.137 Insert Menu
4.4.5.1 Auto Generate
The Auto Generate command opens the Sample Group Wizard, which is used to create a
group of unknown samples, control samples, and calibration standards, and then insert the
group into the active position of the Sample Table.
Sample Group Wizard (Page 1) Sample Source
The Sample Source window is used to specify the source of sample measurement
parameters.
Figure 4.138 Sample Group Wizard (Page 1) Sample Source
Setting Item
Description
Method radio button
Click this option to analyze the samples using the measurement parameters from a specified method. This is the default
option.
Method text field
Enter the desired method or select the method using the
Browse button.
Calibration curve radio button
Click this option to analyze the samples using the measurement parameters from a specified calibration curve.
Calibration curve text field
Enter the desired calibration curve or select the curve using
the Browse button.
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4.4 Sample Table Editor
4.4.5 Insert Menu
Sample Group Wizard (Page 2) Sample Parameter
The Sample Parameter window is used to enter basic information about the sample group.
Figure 4.139 Sample Group Wizard (Page 2) Sample Parameter
182
Setting Item
Description
No. of Samples
Enter the number of samples in the group. Enter an integer
ranging from 1 to 200. The default value is 1.
Start Vial
Enter the starting vial position for the sample group. Enter an
integer ranging from 0 to 9 or 1 to 100, depending on the
sample tray size. The default value is 1. This field is disabled
if an autosampler is not a component of the configured system.
Sample Name/Sample ID
The default designations for these fields are obtained from
the method or calibration curve identified in Page 1 of the
Sample Group Wizard. Enter other names if desired.
Index Start
Select this option to start the counting index. Each sample
added receives an increased counting index number.
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4.4
Sample Table Editor
4.4.5 Insert Menu
Sample Group Wizard (Page 3) Calibration Curves
The Calibration Curves window is used to identify the calibration standards in the sample
group and to specify their placement in the group. The window is also used to revise the list
of calibration curves that will be used to quantitate samples in the group.
Figure 4.140 Sample Group Wizard (Page 3) Calibration Curves
Setting Item
Description
Perform Calibration
Select one of the available options for when calibration
should be performed: At the beginning of the sample group or
Always, after (a selected number of) Samples have been analyzed.
Add button
Use this button to add a calibration curve.
Delete button
Highlight a calibration curve listed in the window and click
the Delete button to remove the curve from the sample group.
Calibration Curves
No.: Displays the number of the calibration point.
File name: Displays the name of the calibration curve.
Analysis: Displays the analysis type.
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4.4 Sample Table Editor
4.4.5 Insert Menu
Sample Group Wizard (Page 4) Controls
The Controls window is used to identify the control samples in a sample group and to
specify their placement in the sample group.
Figure 4.141 Sample Group Wizard (Page 4) Controls
Insert Control Samples
Use the options listed below to insert individual control samples in the sample group.
Setting Items
Description
At the beginning of the sample group
Select this option to add control samples at the beginning of
the sample group.
Always, after (number of)
samples
Select this option to add control samples at defined intervals
between unknown samples.
At the end of the sample
group
Select this option to add control samples at the end of the
sample group.
Control Templates
The Control Templates table displays a list of the control sample templates currently
assigned to the sample group. The templates specify measurement parameters, evaluation
criteria, and failure actions for the control samples. This table is empty by default. Use the
options listed below to revise the list of control sample templates associated with the
sample group.
Option
Description
Add
Select this option to add a control template to the sample
group.
Delete
Select this option to delete a highlighted control template
from the list.
After all four pages of the Sample Group Wizard are complete, click the Finish button to
save changes and add the sample group to the Sample Table. If invalid parameter values
were entered, an error message will be displayed and the sample group will not be inserted
into the Sample Table until after the error is corrected.
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4.4
Sample Table Editor
4.4.5 Insert Menu
4.4.5.2 Sample
The Sample command opens the Sample Wizard, which is used to insert sample
measurement parameters into an existing Sample Table. The Sample Wizard is not
accessible during an analysis.
Sample Wizard (Page 1) Parameter Source
The Parameter Source window is used to specify the source of the sample measurement
parameters. The source can either be a method file or a calibration file. When one of these
sources is selected, the sample will be analyzed using the same measurement parameters as
those in the specified method or calibration file. Some of the source parameters can be
edited in subsequent pages of the Sample Wizard. Note that a sample can also be added to
the Sample Table without specifying a source, an option that is desirable when a sample is
to be analyzed using different parameters than those specified in the method or calibration
files. In this case, unique measurement parameters for the sample will be entered on
subsequent pages of the Sample Wizard.
Figure 4.142 Sample Wizard (Page 1) Parameter Source
Parameter
Description
Method radio button
Select this option to use the sample measurement parameters from a specified
method. This is the default option. Enter the method name in the text field, or
use the Browse button to select the file using the File>Open dialog box
Calibration Curve radio
button
Select this option to use the measurement parameters from a specified calibration curve. Enter the calibration curve name in the text field, or use the
Browse button to select the file using the File>Open dialog box.
Edit parameters manually
radio button
Select this option to insert a sample without defining a source. Sample measurement parameters will be entered in subsequent pages (1-12) of the Sample Wizard.
Skip remaining Wizard
pages and use measurement parameters from the
source
Select this option to accept all measurement parameters from the source file.
The Next button will become a Finish button, and subsequent pages of the
Sample Wizard will not be displayed. This option is disabled if Edit parameters manually is selected.
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4.4 Sample Table Editor
4.4.5 Insert Menu
Sample Wizard (Page 2) Analysis Information
Figure 4.143 Sample Wizard (Page 2) Analysis Information
Parameter
Description
Analysis
Select the analysis type from the drop-down list.
Default Sample Name
Enter the sample name.
Default Sample ID
Enter the sample identification.
Dilution
Enter the preparation dilution factor.
No. of Determinations
Use the spin controls to enter the number of times the sample
is to be measured. Note that determinations and injections are
different; each determination is made up of one or more
injections. Enter an integer from 1 to 10.
Note:
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For combined analyses such as TC/TN or POC+NPOC, subsequent Sample Wizard windows may appear more than once so that parameter modifications specific to each analysis type can be made. The analysis type that is associated with
each Sample Wizard window can be found in the Analysis box at the top of the
window.
4.4
Sample Table Editor
4.4.5 Insert Menu
Sample Wizard (Page 3) Calibration Curve
The Calibration Curve window is used to identify the calibration curve(s) that will be used
to calculate the sample concentration. If more than one curve is identified, the software
automatically selects the curve to be used in calculating sample concentration. Refer to
Section 6.2.5 "Automatic Selection of Optimum Calibration Curve".
Figure 4.144 Sample Wizard (Page 3) Calibration Curve
Parameter
Description
Analysis
Displays the analysis type. This field cannot be changed.
Calibration Curve 1/2/3
Enter the name of the calibration curve or click the Browse
button to select a file using the File>Open dialog box.
Skip the injection parameter
pages of the wizard
Select this item to skip the Measurement Parameters window
of the Sample Wizard. Use this option when the sample measurement parameters will be the same as those used for calibration curve measurements.
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4.4 Sample Table Editor
4.4.5 Insert Menu
Sample Wizard (Page 4) Injection Parameters
Figure 4.145 Sample Wizard (Page 4) Injection Parameters
188
Parameter
Description
Analysis
Displays the analysis type. This field cannot be changed.
Units
Enter the concentration units.
Injection Volume
Enter the injection volume.
Expected Conc. Range
Enter the maximum expected sample concentration.
No. of Injections
Enter the minimum and maximum number of injections for
the sample.
SD Max
Enter the maximum standard deviation. If this value is met,
no additional injections are required. However, if both this
value and the CV Max value are exceeded, the sample is
automatically reinjected up to the maximum number of times
specified in the No. of Injections field. The SD Max field is
disabled if the No. of Injections is 1 or if the minimum is
equal to the maximum.
CV Max
Enter the maximum coefficient of variation. If this value is
met, no additional injections are required. However, if both
this value and the SD Max value are exceeded, the sample is
automatically reinjected up to the maximum number of times
specified in the No. of Injections field. The CV Max field is
disabled if the No. of Injections is 1 or if the minimum is
equal to the maximum.
No. of Washes
Enter the number of times the syringe is to be washed with
sample prior to the first injection. Note that if the Auto Dilution option was selected, the sample will be diluted and the
syringe will then be washed with the diluted sample.
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Sample Table Editor
4.4.5 Insert Menu
Parameter
Description
Auto Dilution
Enter a dilution factor for the sample. The instrument will
automatically dilute the sample by this factor, and the result
will be multiplied by the factor to obtain the final concentration. The default Auto Dilution value is 1.
Sparge Time
Enter the sparge time.
Acid Addition
Enter the desired quantity of acid to be added. This value is
expressed as a percent of the sample volume and is available
only for NPOC or related analyses.
Multiple Injections
Select this option to enable the syringe to draw up a single
sample aliquot with a volume equal to that required for all
injections of the sample. When this option is not selected, the
syringe will draw up a separate sample aliquot for each injection. Selecting this option reduces analysis time.
Use blank check area
Select this option to subtract the blank check area from the
measured area of the sample. This option is only available for
TC and NPOC analyses that use the high sensitivity catalyst.
Auto. correction of inj. vol.
and dilution
Select this option to enable the instrument to automatically
adjust the injection volume and dilution factor when the peak
height for the initial injection exceeds full scale. After the
adjustment, measurement will be repeated.
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4.4 Sample Table Editor
4.4.5 Insert Menu
Sample Wizard (Page 5) Peak Time Parameters
Figure 4.146 Sample Wizard (Page 5) Peak Time Parameters
190
Parameter
Description
Analysis
Displays the analysis type. This field cannot be changed.
Use default settings
Select this option to use the default integration parameters.
When this option is selected, all other options in this window
are disabled.
Allowed peak start delay
The allowed peak start delay is the amount of time (in minutes) that can elapse before the analysis is stopped because a
peak is not detected. Enter a number between 0 and 20:00.
Total integration time
The total integration time is the amount of time (in minutes)
that analysis continues after the end of the peak is detected.
Enter a number between 4:50 and 20:00.
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Sample Table Editor
4.4.5 Insert Menu
Sample Wizard (Page 6) Calibration Curve
A second Calibration Curve window is only displayed when more than one analysis type
has been specified. This window is the same as Page 3 of the Sample Wizard, which is
described above. Verify the analysis type in the Analysis text box at the top of the page and
make the appropriate selections.
Figure 4.147 Sample Wizard (Page 6) Calibration Curve Window (Second Analysis)
Sample Wizard (Page 7) Injection Parameters
A second Injection Parameters window is only displayed when more than one analysis type
has been specified. This window is the same as Page 4 of the Sample Wizard, which is
described above. Verify the analysis type in the Analysis text box at the top of the page and
make the appropriate selections.
Figure 4.148 Sample Wizard (Page 7) Injection Parameters Window (Second Analysis)
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4.4 Sample Table Editor
4.4.5 Insert Menu
Sample Wizard (Page 8) Peak Time Parameters
A second Peak Time Parameters window is only displayed when more than one analysis
type has been specified. This window is the same as Page 5 of the Sample Wizard, which is
described above. Verify the analysis type in the Analysis text box at the top of the page and
make the appropriate selections.
Figure 4.149 Sample Wizard (Page 8) Peak Time Parameters Window (Second Analysis)
Sample Wizard (Page 9) USP/EP
The USP/EP window is displayed only for TC or NPOC methods, and is used to enable
samples to be checked in accordance with USP/EP standards. This window is the same as
Page 6 of the Sample Wizard, which is described above. Select the check box to enable this
function.
Figure 4.150 Sample Wizard (Page 9) USP/EP
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Sample Table Editor
4.4.5 Insert Menu
4.4.5.3 Control
The Control command is used to insert a control sample into an existing Sample Table.
Note:
A control sample template must be created before a control sample can be
inserted into a Sample Table. A control sample template has a file extension of
*.tpl and specifies measurement parameters for the Control Sample.
The following subsections describe the procedures for creating a control sample template
and for inserting a control sample into a Sample Table.
¬Creating a Control Sample Template
Control sample templates are created using the Control Sample Wizard. To access the
Control Sample Wizard select New>Control Sample Template from the File menu. The
Control Sample Wizard consists of several windows, each of which defines specific
parameters for the control sample template, as described below.
Control Sample Wizard (Page 1) System Information
Figure 4.151 Control Sample Wizard (Page 1) System Information
Parameter
Description
System
Select the instrument.
Operator
Displays the current operator name. This field cannot be
changed.
Date of Creation
Displays the current date and time. This field cannot be
changed.
Comment
Enter a comment (512 characters maximum).
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4.4 Sample Table Editor
4.4.5 Insert Menu
Control Sample Wizard (Page 2) Control Sample Type
The Control Sample Type window is used to identify the type of control sample.
Figure 4.152 Control Sample Wizard (Page 2) Control Sample Type
194
Parameter
Description
Control Sample
Select this option to define individual sample parameters.
This is the default option.
Control Chart Sample
Select this option to add the control sample to a defined control chart. Enter the file name or use the Browse button to
select the control chart file from the File>Open dialog box.
System Suitability Test for
USP/EP
Select this option to check the control sample using USP/EP
criteria.
Save the data in a control
sample template
Enter a file name for the control sample template.
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4.4
Sample Table Editor
4.4.5 Insert Menu
Control Sample Wizard (Page 3) Parameter Source
The Parameter Source window is used to specify the source of the control sample
measurement parameters. The source can either be a method file or a calibration file. When
one of these sources is selected, the control sample will be analyzed using the same
measurement parameters as those in the specified method or calibration file. Some of the
source parameters can be edited in subsequent pages of the Control Sample Wizard. Note
that a control sample can also be added to the Sample Table without specifying a source, an
option that is desirable when a control sample is to be analyzed using different parameters
than those specified in the method or calibration files. In this case, unique measurement
parameters for the sample will be entered on subsequent pages of the Control Sample
Wizard.
Figure 4.153 Control Sample Wizard (Page 3) Parameter Source
Parameter
Description
Method radio button
Select this option to use the measurement parameters from a
specified method. Enter the method name in the text field, or
use the Browse button to select the file using the File>Open
dialog box. This is the default option.
Calibration Curve radio button
Select this option to use the measurement parameters from a
specified calibration curve. Enter the calibration curve name
in the text field, or use the Browse button to select the file
using the File>Open dialog box.
Edit parameters manually
radio button
Select this option to insert a control sample without defining
a source. Control sample measurement parameters will be
entered in subsequent pages of the Control Sample Wizard.
Skip remaining Wizard pages Select this option to accept all measurement parameters from
and use measurement param- the source file. The Next button will become a Finish button,
eters from the source
and subsequent pages of the Control Sample Wizard will not
be displayed. This option is disabled if Edit parameters manually is selected.
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4.4 Sample Table Editor
4.4.5 Insert Menu
Control Sample Wizard (Page 4) Analysis Parameters
Figure 4.154 Control Sample Wizard (Page 4) Analysis Parameters
196
Parameter
Description
Analysis
Select the analysis type from the drop-down list. If a source
method or calibration file was specified on Page 3 of the
Control Sample Wizard, this field is disabled and the applicable analysis type is displayed.
Default Sample Name
Enter the sample name. If a source method or calibration file
was specified on Page 3 of the Control Sample Wizard, the
default sample name from the source is displayed.
Default Sample ID
Enter the sample identification. If a source method or calibration file was specified on Page 3 of the Control Sample Wizard, the default sample identification from the source is
displayed.
Dilution
Enter the dilution factor. If a source method or calibration file
was specified on Page 3 of the Control Sample Wizard, the
default dilution factor is displayed.
Calibration Curve
Enter the calibration file name that is to be used to calculate
control sample concentration. If a source method or calibration file was specified on Page 3 of the Control Sample Wizard, the default calibration curve name from the source is
displayed.
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Sample Table Editor
4.4.5 Insert Menu
Control Sample Wizard (Page 5) Injection Parameters
Figure 4.155 Control Sample Wizard (Page 5) Injection Parameters
Parameter
Description
Analysis
Displays the analysis type. This field cannot be changed.
Units
Select the concentration units.
Injection Volume
Enter the injection volume.
Expected Conc. Range
Enter the maximum expected concentration.
No. of Injections
Enter the minimum/maximum number of injections for the control sample.
The setting range is from 1-20.
SD Max
Enter the maximum standard deviation that is acceptable for the injections. If
this value is met, no additional injections are required. However, if both this
value and the CV Max value are exceeded, the control sample is automatically
reinjected up to the maximum number of times specified in the No. of Injections field. The SD Max field is disabled if the No. of Injections is 1 or if the
minimum is equal to the maximum.
CV Max
Enter the maximum coefficient of variation that is acceptable for the injections. If this value is met, no additional injections are required. However, if
both this value and the SD Max value are exceeded, the control sample is
automatically reinjected up to the maximum number of times specified in the
No. of Injections field. The CV Max field is disabled if the No. of Injections is
1 or if the minimum is equal to the maximum.
No. of Washes
Enter the number of times the syringe is to be washed with sample prior to the
first injection. Note that if the Auto Dilution option was selected, the sample
will be diluted and the syringe will then be washed with the diluted sample.
Auto Dilution
Enter a dilution factor for the samples. The instrument will automatically
dilute the control sample by this factor, and the result will be multiplied by the
factor to obtain the final concentration. The default Auto Dilution value is 1.
Acid Addition
Enter the desired quantity of acid to be added. This option is available only for
NPOC and related analyses.
Sparge Time
Enter the sparge time.
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4.4 Sample Table Editor
4.4.5 Insert Menu
Parameter
Description
Multiple Injections
Select to enable the syringe to draw up a single sample aliquot with a volume
equal to that required for all injections of the sample. When this option is not
selected, the syringe will draw up a separate sample aliquot for each injection;
as a result, selecting this option reduces analysis time.
Use area retrieved from
the blank check
Select this option to subtract the blank check area from the measured area of
the control sample. This option is only available for TC and NPOC analyses
that use the high sensitivity catalyst.
Control Sample Wizard (Page 6) Peak Time Parameters
The Peak Time Parameters window is used to set peak detection parameters for the control
samples.
Figure 4.156 Control Sample Wizard (Page 6) Peak Time Parameters
198
Setting Item
Description
Use default settings
Select this option to use the default integration parameters.
When this option is selected, all other options in this window
are disabled.
Allowed peak start delay
The allowed peak start delay is the amount of time (in minutes) that can elapse before the analysis is stopped because a
peak is not detected. Enter a number between 0 and 20:00.
Total integration time
The total integration time is the amount of time (in minutes)
peak detection continues. Enter a number between 4:50 and
20:00.
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Sample Table Editor
4.4.5 Insert Menu
Control Sample Wizard (Page 7) History
The History window is used to enable the History Log. The History Log records all
modifications to the control sample template properties. The History Log can be set to
require users to enter comments for each modification.
Note:
Once the History Log is enabled, it cannot be disabled. All modifications to the
control sample template will be tracked. If the mandatory comment option is
selected, the user will be required to enter a comment each time any parameter in
the control sample template is modified.
Figure 4.157 Control Sample Wizard (Page 7) History
Setting Item
Description
Enable history log
Select this option to enable the software to monitor all modifications to the control sample template. Once the History
Log is enabled, it cannot be disabled. If the History Log is not
required, it need not be enabled, as the software operates
properly without it.
User has to comment all
modifications
Select this option to require comments or approval for all
modifications.
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4.4 Sample Table Editor
4.4.5 Insert Menu
Control Sample Wizard (Page 8) Control Checking
The Control Checking window is used to select options for control checks and control
limits. This window is not displayed if the USP/EP system suitability criteria are used
because the control limits are already defined.
Figure 4.158 Control Sample Wizard (Page 8) Control Checking
200
Setting Option
Description
Recovery
Select this option to check recovery amounts in control samples.
Spiked
Select this option to use an original and a spiked sample to
calculate the recovery amount. This option is enabled only
when the Recovery option is selected.
Original Concentration
Enter the original concentration of the spiked sample. This
field is enabled only when the Recovery option is selected.
Spiked Concentration
Enter the concentration of the spiked sample. This field is
enabled only when the Recovery and Spiked options are
selected.
Mean Value (Concentration)
Select this option to check the mean value of the measured
concentrations.
Blind Value (Area)
Select this option to check the mean value of the measured
area values.
Spanwidth (Concentration)
Select this option to check the deviation of the measured concentrations.
Max. Dev.
Enter the maximum acceptable deviation. This field is
enabled only when the Spanwidth option is selected.
Low
Enter the lower limit of the valid control range, if the Blind
Value option is selected.
Up
Enter the upper limit of the valid control range, if the Blind
Value option is selected.
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Sample Table Editor
4.4.5 Insert Menu
Control Sample Wizard (Page 9) Failure Action
The Failure Action window is used to specify the actions taken when a control sample
exceeds the specified control limits.
Figure 4.159 Control Sample Wizard (Page 9) Failure Action
Setting Item
Description
Action when the failure event Select the action to be taken the first time a control sample
occurs the first time
exceeds the control limits. Options available from the dropdown list are:
Continue (notify): Select this option to allow the analysis
sequence to continue normally and display a failure message
in the Notification Bar.
Stop (Whole Sample Run): Select this option to stop the sample run and display a failure message in the Notification Bar.
Repeat (From last control or calibration): Select this option
to automatically reanalyze all samples analyzed after the previous valid control sample or calibration curve (whichever
occurred most recently) and display a failure message in the
Notification Bar.
Action when the failure event Select the action to be taken the second time a control sample
occurs the second time
exceeds the control limits. The options available from the
drop-down list are Continue and Stop. The Repeat option is
not available.
Save the control sample template and close the Control Sample Wizard by clicking the
Finish button.
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4.4 Sample Table Editor
4.4.5 Insert Menu
¬Inserting a Control Sample into the Sample Table
Once the control sample template has been created, a control sample can be entered into the
Sample Table by following the procedure below.
Procedure
202
1.
Open the Sample Table and place the cursor in the row where the control sample will
be inserted.
2.
From the Insert menu, select Control.
The Open dialog box displays the available control sample template files.
3.
Select the appropriate control sample template and click the Open button.
The Open dialog box closes and the Sparging/Acid Addition window is displayed.
4.
Enter the ASI vial position for the control sample into the appropriate cell in the
Sparging/Acid Addition window.
5.
Click the OK button.
The Sparging/Acid Addition window closes.
6.
Scroll through the Sample Table to verify that the control sample has been inserted at
the correct location.
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4.4 Sample Table Editor
4.4.6 Instrument Menu
4.4.6 Instrument Menu
The Instrument menu contains commands for connecting, starting, and stopping the
instrument, and for instrument maintenance functions.
Figure 4.160 Instrument Menu
4.4.6.1 Background Monitor
The Background Monitor command is used to open the Background Monitor window,
which displays the status of the autosampler and all installed instrument detectors. The real
time signal and ready status for various detectors can be viewed by toggling between the
individual instrument tabs. The command is available only when an instrument is
connected to the software. Instrument and communication errors are displayed in the
Notification Bar. The Background Monitor window cannot be open during measurement.
TOC Tab
Figure 4.161 Background Monitor Window: TOC Tab
Parameter
Description
Furnace
Displays the temperature of the TC furnace.
Dehumidifier
Displays the temperature of the dehumidifier.
NDIR
Baseline Pos.: Displays the status of the NDIR detector baseline position.
Baseline Fluc.: Displays the status of the NDIR detector baseline fluctuation.
Baseline Noise: Displays the status of the NDIR detector baseline noise.
The bottom portion of the TOC tab window displays a graph of the selected items.
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4.4 Sample Table Editor
4.4.6 Instrument Menu
TN Tab
Figure 4.162 Background Monitor Window: TN Tab
Parameter
Description
TN Reactor
Displays the temperature of the TN reactor.
Chemiluminescence
Baseline Pos.: Displays the status of the chemiluminescence detector baseline
position.
Baseline Fluc.: Displays the status of the chemiluminescence detector baseline
fluctuation.
Baseline Noise: Displays the status of the chemiluminescence detector baseline
noise.
The bottom portion of the TN tab window displays a graph of the selected items.
ASI Tab
The ASI tab is available only if the ASI is connected to the instrument. The ASI Power
indicator displays the power status of the ASI. The ASI Cover indicator displays the status
of the ASI cover.
Figure 4.163 Background Monitor Window: ASI Tab
204
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4.4 Sample Table Editor
4.4.6 Instrument Menu
4.4.6.2 Connect
The Connect command is used to connect or disconnect the instrument and the software. If
the instrument is not connected, selecting the Connect command opens the communication
port, initializes the instrument, and downloads and checks the instrument parameters.
During this process, the Sequence window displays the progress of the connection. To abort
the Connect operation while it is in progress, click the Cancel button.
Figure 4.164 Sequence Window
The bottom portion of the Sequence window displays a list of tasks that are performed
during the Connect process. The progress of each task and the result after completing the
task are shown in columns to the right of the task list. The Sequence window closes when
the connection process is complete. If an error occurs during the Connect process, an error
message is displayed in the Notification Bar and the result column, and the Sequence
window remains open.
If the instrument is already connected to the software, the Connect command is used to
disconnect the instrument. A confirmation request dialog box is displayed when the
command is selected, as shown below.
Figure 4.165 Disconnect Confirmation Request Dialog Box
Click the OK button to disconnect the instrument, or the Cancel button to abort the
operation.
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4.4 Sample Table Editor
4.4.6 Instrument Menu
4.4.6.3 Standby
The Standby function is used to shut down the instrument. To access the Standby function,
open a Sample Table, then select Standby from the Instrument menu. The Standby window,
which lists options for the shut down operation, is displayed. Select the desired options and
click the Standby button. Click the Escape button to abort the Standby operation and
maintain the instrument in Ready mode.
Reference: To end measurement, refer to Section 4.3.3 "Ending Measurement".
CAUTION
Do not turn off the TOC-V main instrument switch for at least 30 minutes after
initiating the shut down procedure.
Figure 4.166 Standby Window
206
Setting Item
Description
Shut down instrument
Select this option to begin a 30-minute countdown to instrument shutdown. During the shutdown process, the carrier gas
is turned off and the furnace cools down. The power to the
instrument is automatically turned off when the countdown is
complete.
Auto restart
Select this option to shut down the instrument but automatically restart it at a specified time. Set the restart time using
the spin controls for Auto start time. The default settings are
the current system date and time.
Keep TC furnace heating
Select this option to keep the TC furnace on during the
Standby mode. This option is available only when the Auto
restart option is selected.
Keep carrier gas flowing
Select this option to keep the carrier gas flowing during the
Standby mode. This option is available only when the Auto
restart option is selected.
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4.4 Sample Table Editor
4.4.6 Instrument Menu
4.4.6.4 Measurement Start
Click the Measurement Start command to open the Standby dialog box if the ASI is
included in the system configuration. If the ASI is not included, the Measurement Mode
dialog box is displayed. To start measurement, open the Sample Table, define a new
sample, and connect to the instrument.
Figure 4.167 Measurement Mode Dialog Box
Item
Setting Description
Normal Mode
Select this option to conduct analysis sample-by-sample.
Between samples, the instrument waits for the user command
before starting the next measurement.
Multiple Row Continuous
Mode
Select this option to perform continuous, uninterrupted measurement of multiple rows until the user stops the measurement sequence.
Continuous Mode
Select this to perform measurement using multiple measurement modes, without stopping measurement between modes.
Select OK to continue on to the measurement, or select Cancel to cancel the start of
measurement.
4.4.6.5 Stop>Peak Stop
The Stop>Peak Stop command is used to interrupt the current measurement. The peak
measured up to the stopping point is considered a complete peak. After the Stop>Peak Stop
command is executed, the next injection listed in the Sample Table is made and analysis
continues normally.
4.4.6.6 Stop>Finish Current Sample
The Stop>Finish Current Sample command is used to interrupt measurement after all
injections of the current sample are complete. After the Stop>Finish Current command is
executed, the instrument remains in Ready mode.
4.4.6.7 Stop>Halt
The Stop>Halt command is used to immediately interrupt the current measurement, discard
data from the current injection, and return the instrument to Ready mode.
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4.4 Sample Table Editor
4.4.7 Maintenance Menu
4.4.7 Maintenance Menu
Instrument maintenance procedures are described in Section 5.6 "Software-Controlled
Maintenance Functions". All maintenance functions can be initiated using the options
displayed in the Instrument>Maintenance menu.
4.4.8 Tools Menu
Figure 4.168 Tools Menu
4.4.8.1 Control Charts
The Control Charts function is used to create control charts. Refer to Appendix B for a
detailed description of the function.
4.4.8.2 Method Validation
The Method Validation function is used to validate analytical methods. Refer to Appendix
A for a detailed description of the function.
4.4.8.3 Administration
The Administration function is used to access the Administration program of the TOCControl V software. Refer to Section 3.1 "Introduction to System Administration
Functions" for a detailed description of the Administration program.
208
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4.4
Sample Table Editor
4.4.8 Tools Menu
4.4.8.4 Screen Lock
If the user must temporarily leave the PC he/she is logged into, the screen can be locked by
using the password function to prevent another individual from performing operations in
TOC-Control V. This function can be used only if the User ID / Password item is checked
in the Security dialog box.
To lock the screen, select Screen Lock in the Tools menu. The screen will then be locked
and the Re-enter Password dialog box is displayed. To release the screen lock, enter the
user ID and password into the designated fields. If the user ID and password entered are not
the same as those used up to that point, the screen lock will not be released.
Figure 4.169 Re-enter Password Dialog Box
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4.4 Sample Table Editor
4.4.9 Options Menu
4.4.9 Options Menu
The Options menu contains commands for viewing and displaying system information and
for setting default measurement parameters.
Figure 4.170 Options Menu
4.4.9.1 General Information
The General Information command is used to view information about the system. The
General Information window contains two tabs, one that displays System parameters and
one that displays History information. Most of the fields in the General Information
window are disabled because they were set previously. After changing an active field, click
the OK button to close the window and save the changes or click the Apply button to save
the changes without closing the window. Click the Cancel button to close the window
without saving changes.
Figure 4.171 General Information Window: System Tab
System Tab
The System tab displays general parameters.
210
Parameter
Description
System
Displays the instrument identification.
File Version
Displays the instrument file version.
User
Displays the name of the user who set up the system.
Date of Creation
Displays the date the system was set up.
Comment
Enter a comment (512 characters maximum), if desired.
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4.4
Sample Table Editor
4.4.9 Options Menu
History Tab
Figure 4.172 General Information Window: History Tab
The History tab is used to view the system’s History Log or to enable the log if it was not
previously selected.
Note:
Once the History Log is enabled, it cannot be disabled.
Setting Item
Description
Enable history log
Select this option to enable the software to monitor all modifications to the system. Once the History Log is enabled, it
cannot be disabled. If the History Log is not required, it need
not be enabled, as the software works properly without it.
User has to comment all
modifications
Select this option to require comments or approval for all
modifications.
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4.4 Sample Table Editor
4.4.9 Options Menu
4.4.9.2 Default Measurement Parameters
The Default Measurement Parameters command is used to enter the default values for
samples, methods, and calibration curves. The Default Measurement Parameters window
contains a separate tab for each analysis type, into which the default values are entered. The
SSM-TC and SSM-IC tabs are items associated with the installation of SSM-5000A. For
details, refer to the SM-5000A User's Manual
Figure 4.173 Default Measurement Parameters: TC Tab
Figure 4.174 Default Measurement Parameters: TN Tab
The parameters shown on each of the tabs are similar and are described below.
212
Parameter
Description
Units
Select the default concentration units.
No. of Injections
Enter the default minimum/maximum number of injections.
No. of Washes
Enter the default number of times the syringe is to be washed
with sample prior to the first injection. Note that if the Auto
Dilution option was selected, the sample will be diluted and
the syringe will then be washed with the diluted sample.
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4.4
Sample Table Editor
4.4.9 Options Menu
Parameter
Description
Max SD
Enter the default maximum standard deviation that is acceptable for the injections. If this value is met, no additional
injections are required. However, if both this value and the
Max CV value are exceeded, the samples are automatically
reinjected up to the maximum number of times specified in
the No. of Injections field. The SD Max field is disabled if
the No. of Injections is 1 or if the minimum is equal to the
maximum.
Max CV
Enter the default maximum coefficient of variation that is
acceptable for the injections. If this value is met, no additional injections are required. However, if both this value and
the Max SD value are exceeded, the samples are automatically reinjected up to the maximum number of times specified in the No. of Injections field. The CV Max field is
disabled if the No. of Injections is 1 or if the minimum is
equal to the maximum.
4.4.9.3 Display Settings>Display Font
The Display Settings>Display Font function is used to select font options for both the
general screen display (such as in the Sample Table and Print Preview screens) and printed
reports. Select a font type, style, size, and color from the lists in the Font dialog box. A
preview of the font appearance is displayed in the Sample field.
Figure 4.175 Font Dialog Box
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4.4 Sample Table Editor
4.4.9 Options Menu
4.4.9.4 Display Settings>Table Settings
The Display Settings>Table Settings function is used to select the parameters that will be
displayed in the Sample Table window. The Table Options window contains two tabs, one
that lists Sample Table parameters and one that lists Injection Table parameters. Note that
on each tab, certain options are selected by default. Individual options can be selected or
deselected by clicking in the check box. Use the All and None buttons to quickly select and
deselect all options on a tab. Use the Default button to select the default options.
Sample Table Tab
Select the parameters that will be displayed in the Sample Table.
Figure 4.176 Table Options Window: Sample Table Tab
Samples Tab
Select the parameters that will be displayed in the Injection Table.
Figure 4.177 Table Options Window: Samples Tab
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4.4
Sample Table Editor
4.4.9 Options Menu
4.4.9.5 Display Settings>Notification Bar Settings
The Display Settings>Notification Bar Settings function is used to set options for the
Notification Bar, where error messages and other notices are displayed. The Notification
Bar is located at the bottom of the Sample Table Editor window.
Four folders can be displayed in the Notification Bar: Notifications, System Folders,
Errors, and Events. When a folder is selected for display, a tab appears for that folder in the
Notification Bar. When more than one folder is selected for display, the contents of a
specific folder can be displayed by clicking the appropriate tab.
Figure 4.178 Notification Bar Settings Window
Setting Item
Description
Folder List
Lists the folders that can be displayed in the Notification Bar.
Display Folder
Place a check in this box to display the folder.
Max. Number of Displayed
Lines
Enter the maximum number of lines to be displayed in the
Notification Bar. Acceptable values range from 0 to 200.
Font
Displays the selected font. Modify the font by selecting the
Browse button to open the Font dialog box.
To select a folder for display in the Notification Bar, click the folder in the Folder List, then
select the Display Folder option. Set the Max. Number of Displayed Lines field to a value
greater than 0. To change the color or appearance of the text displayed in the folder, use the
Font option. Note that the Display Folder check box, Max. Number of Displayed Lines
field, and Font option apply only to the selected folder; as a result, these options must be set
separately for each folder.
Note:
A folder will not be displayed in the Notification Bar unless the Display Folder
option is selected and the Max. Number of Displayed Lines field is set to a value
greater than 0.
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4.4 Sample Table Editor
4.4.9 Options Menu
4.4.9.6 Display Settings>Floating Point Number Formats
The Display Settings>Floating Point Number Formats command is used to select display
options for numeric results in the Sample Table. Note that these options apply only to the
manner in which numbers are displayed; internal data retain their original values.
Figure 4.179 Floating Point Format Window
Select settings for both common numbers and percent values, as described below.
Common Floating Point Numbers
Setting Item
Description
Number of significant digits
Select this option to display common floating point numbers
using a specified number of significant digits. Use the spin
control to set the number of significant digits. The default
value is 4.
Number of digits after the
decimal point
Select this option to display common floating point numbers
using a specified number of digits after the decimal point.
Use the spin control to set the number of digits after the decimal point. The default value is 2.
Percent Values
216
Setting Item
Description
Number of significant digits
Select this option to display percent values using a specified
number of significant digits. Use the spin control to set the
number of significant digits. The default value is 4.
Number of digits after the
decimal point
Select this option to display percent values using a specified
number of digits after the decimal point. Use the spin control
to set the number of digits after the decimal point. The default
value is 2.
TOC-VCPH/CPN
4.4
Sample Table Editor
4.4.9 Options Menu
4.4.9.7 Directories
The Directories function is used to modify system directories. Select Options>Directories
to display the Folder window.
Figure 4.180 Folder Window
Show all directories for
Use the drop-down list to access various directories. Available directories are listed in the
Folder text field.
Add
Click the Add button to add a new directory to the list for a specified topic, and the Folder
dialog box is displayed. Highlight the desired directory from the drop-down Drive and
Directory lists, then select it by clicking the OK button. Click the Network button to access
at network drive.
Figure 4.181 Folder Dialog Box
Delete
Click the Delete button to delete a selected directory from the list.
Up
Click the Up button to move the selected directory up one line in the list. The order of the
directories in the list is the order in which the directories will be searched during instrument
operation.
Down
Click the Down button to move the selected directory down one line in the list. The order of
the directories in the list is the order in which the directories will be searched during
instrument operation.
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4.4 Sample Table Editor
4.4.10 Window Menu
4.4.10 Window Menu
Figure 4.182 Window Menu
4.4.10.1 Cascade
The Cascade command is used to stack all open windows so that the title bars are visible.
4.4.10.2 Tile
The Tile command is used to size all open windows so that each window occupies an equal
portion of the screen.
4.4.10.3 Arrange Icons
The Arrange Icons command is used to neatly organize windows that have been minimized
or reduced to icons.
4.4.11 Help Menu
Figure 4.183 Help Menu
About
The About command is used to view copyright, software registration, and software version
information.
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4.5 Application Operations
4.5.1 Manual Injection Analysis
4.5
Application Operations
4.5.1 Manual Injection Analysis
Samples can be injected manually to perform analysis without the sample injector syringe,
when the optional manual injection kit is installed.
4.5.1.1 Analysis Preparation
Installing the Manual Injection Kit
1.
Remove the knurled thumbscrew that secures the slider then remove the TC/TN
injector slider.
Knurled Thumbscrew
Figure 4.184 Removing the Slider
2.
Install the TC/TN block provided in the kit.
TC/TN Block
Figure 4.185 Installing the TC/TN Block
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4.5 Application Operations
4.5.1 Manual Injection Analysis
3.
If the IC reactor kit is being used, remove the IC injector slider, and install the IC
block provided in the manual injection kit.
IC Block
Figure 4.186 Installing the IC Block
Note:
When installing the block, be sure that it is aligned with the
injection port.
Software Settings
Select the Manual Injection Kit option in the Instrument Setup Wizard Options window
during System Setup. Refer to Section 3.2.2 "Options Window".
Note:
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TOC-VCPH/CPN
Selecting the Manual Injection Kit option disables operation of the TOC-V injector syringe.
4.5 Application Operations
4.5.1 Manual Injection Analysis
4.5.1.2 Measurement
Measurement procedures using the manual injection kit are similar to those described in
Section 4.3 "Measurement Procedures and Tutorial".
¬Calibration Curve Measurement
Procedure
1.
From the File menu, select New. The New dialog box is displayed.
Figure 4.187 New Dialog Box
2.
Double-click the Calibration Curve icon. The Calibration Curve Wizard opens. The
System Information window of the wizard is displayed.
Figure 4.188 Calibration Curve Wizard (Page 1) System Information
3.
From the System drop-down list, select the system that was configured with the
Manual Injection Kit during setup.
4.
Select the desired options on pages 2 and 3 of the Calibration Curve Wizard, which
list calibration curve type and analysis information settings, respectively. Enter the
name of the new calibration curve in the text box at the bottom of page 3 of the
wizard.
Note: Select the settings described in Section 4.2 "Setting General Measurement Parameters".
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4.5 Application Operations
4.5.1 Manual Injection Analysis
5.
Enter the desired number of injections on page 4 of the Calibration Curve Wizard
(Calibration Measurement Parameters).
6.
Enter the injection volume on page 5 of the Calibration Curve Wizard (Calibration
Points List).
Note: An injection volume is displayed automatically. The displayed
value is based on the volume of the last injection that was performed using the sample injector. This value can be changed by the
user as appropriate.
7.
Select the desired options on pages 6 and 7 of the Calibration Curve Wizard, which
list peak time parameter and history settings, respectively. Click the Finish button to
create the new calibration curve.
Note: Select the settings described in Section 4.2 "Setting General Measurement Parameters".
8.
Create a Sample Table for the calibration curve. From the Insert menu, select
Calibration Curve. Select the newly created calibration curve from the list of files in
the Open dialog box.
9.
Connect the instrument by selecting Connect from the Instrument menu. Then select
Start from the Instrument menu. The Manual Injection Parameter dialog box is
displayed.
10. Draw an appropriate amount of sample into the syringe.
Note:
Draw in and discharge the sample 3 or 4 times before filling the
syringe for measurement.
11. Enter the injection volume in the Manual Injection Parameter dialog box, and click
the Set button.
12. Verify that the instrument is ready for measurement, and click the Start button.
13. For TC or TN measurement, open the injection port valve and insert the syringe
needle into the injection port. For IC measurement, insert the syringe needle into the
injection port septum.
Note: • Insert the syringe needle as far as possible into the injection port.
• To obtain reproducible results, perform all injections at the same
speed.
14. Withdraw the syringe from the injection port. For TC or TN measurement, close the
injection port valve.
The results are displayed when measurement is complete.
15. Click Additional Measurements to perform repeat measurements. Repeat the
procedure. Click the Finish button when all measurements are complete.
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4.5 Application Operations
4.5.1 Manual Injection Analysis
¬Sample Measurement
Procedure
1.
From the File menu, select New. The New dialog box is displayed.
Figure 4.189 New Dialog Box
2.
Double-click the Method icon. The Method Wizard opens. The System Information
window of the wizard (page 1) is displayed.
Figure 4.190 Method Wizard (Page 1) System Information
3.
Select the system that was configured with the Manual Injection Kit and used to
create the calibration curve. Advance to page 2 of the Method Wizard (Analysis
Information) and enter the new method name in the text box at the bottom of the
window.
4.
Advance to page 3 of the Method Wizard (Calibration Curves). Select the appropriate
calibration curve file.
5.
Enter “1” in the No. of Injections field on page 4 of the Method Wizard (Injection
Parameters).
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4.5 Application Operations
4.5.1 Manual Injection Analysis
6.
Select the desired options on pages 5, 6, and 7 of the Method Wizard, which list peak
time parameter, USP/EP check, and history settings, respectively. Click the Finish
button to create the new method.
Note: Select the settings described in Section 4.2 "Setting General Measurement Parameters".
7.
From the Insert menu, select Sample to open the Sample Wizard. Select the newly
created method from the list of files in the Open dialog box. Complete the remaining
wizard pages.
8.
From the Instrument menu, select Start. The Manual Injection Parameter dialog box is
displayed.
9. Draw an appropriate amount of sample into the syringe.
10. Draw in and discharge the sample 3 or 4 times before filling the syringe for
measurement.
11. Enter the injection volume in the Manual Injection Parameter dialog box, and click
the Set button.
12. Verify that the instrument is ready for measurement, and click the Start button.
13. For TC or TN measurement, open the injection port valve and insert the syringe
needle into the injection port. For IC measurement, insert the syringe needle into the
injection port septum.
Note: • Insert the syringe needle as far as possible into the injection port.
• To obtain reproducible results, perform all injections at the same
speed.
14. Remove the syringe from the injection port. For TC or TN measurement, close the
injection port valve.
15. Click Additional Measurements to perform repeat measurements. Repeat the
procedure. Click the Finish button when all measurements are complete.
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4.5 Application Operations
4.5.1 Manual Injection Analysis
4.5.1.3 Measurement Precautions for Low Concentration Samples
In manual injections of sample concentrations lower than 1µg/mL, it is necessary to take
the following precautions to prevent contamination of the sample and the measurement
process.
Injecting Sample into the Injection Port
Use a separate micro syringe (500µL) for high sensitivity measurement. Any
contamination on the sample injection port may affect the result for high sensitivity
measurement.The inside of the injection port can be contaminated by sample solution that
adheres to the tip of the micro syringe needle. When inserting the micro syringe into the
injection port, use extreme care to avoid touching the tapered portion of the inside of the
sample injection port. After filling the syringe, wipe the excess solution from the needle
surface with soft tissue paper. Prevent excess drops of solution from forming on the tip of
the needle by gently pulling back on the plunger.
Cleaning the Sample Injection Port
Under normal operating conditions, fill a 500µL micro syringe with pure water and insert it
into the injection port. Keep the bottom of the syringe barrel 8-10mm above the injection
port. Under normal operation, the bottom of the syringe barrel is inserted until it comes into
contact with the injection port allowing the needle tip to protrude from the needle guide
pipe by about 5-6mm. With the needle 8-10mm higher than normal operation, the tip of the
needle inside the needle guide pipe. Slowly dispense the pure water. The pure water does
not flow into the combustion tube. It is driven out of the injection port by the carrier gas
flowing through the needle guide pipe. Wipe off the water coming out of the injection tube
with soft tissue paper. The internal injection port and inside of the needle guide pipe are
now clean.
Measurement of service water or contamination free environmental water, such as river
water, often reveals that IC is the major part of TC when the TOC content is around 1ppm.
For these types of samples it is preferable to remove the IC content before measuring TOC
through the TC channel.
Errors for TC and IC analyses are additive. For samples that have a comparatively high IC
content relative to the TOC content, the TOC analysis error will be large if it is determined
by the difference between TC and IC results.
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4.5 Application Operations
4.5.1 Manual Injection Analysis
4.5.1.4 Maintenance
Replacing the IC Injection Port Septum (Cushion O-Ring)
The septum used with the IC injection port is a consumable item. The septum typically can
be used for 200 or more injections; however, it should be replaced if there is deterioration
in reproducibility or peak shapes.
Part number for replacement cushion O-ring (20 pcs.): P/N 630-01559-01
Replacement Procedure
1.
2.
3.
Loosen and remove the injection port bushing.
Remove the old septum, and insert a new one.
Replace the bushing and tighten it.
CAUTION
IC reaction solution may spatter close to the injection port septum and injection
port; however, this poses no problem during analysis. When replacing the
septum, wipe away any liquid, taking care to avoid contact.
Gas-tight Syringe
For analysis, use a needle length of 50mm, or a 2 inch gas-tight syringe. The following gastight syringes are available from Shimadzu. Order replacement syringes as necessary.
Table 4.7 • Gas-Tight Syringes (Option)
Part Name
P/N
Capacity
Gas-tight syringe set 25uL
638-60733-02
Gas-tight syringe set 50uL
-03
50uL*
Gas-tight syringe set 100uL
-04
100uL*
Gas-tight syringe set 250uL
-05
250uL*
Gas-tight syringe set 500uL
-06
500uL*
Gas-tight syringe 1mL
25uL
046-00026-02
1mL
Gas-tight syringe set 5mL
-03
5mL
Gas-tight syringe set 10mL
-04
10mL
* Set comprises one replacement gas-tight syringe needle and one plunger.
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4.5 Application Operations
4.5.2 Gas Sample Analysis
4.5.2 Gas Sample Analysis
If the optional manual injection kit is installed, analysis of TC and IC in gaseous samples
can be performed by using gas-tight syringes or other applicable injectors to inject the
gaseous samples.
¬Precautions for Gas Sample Analysis
CAUTION
•
•
•
Do not inject a large quantity of sample at one time when measuring combustible
or explosive gases. The combustion tube could break. The injection volume
should not exceed 10mL.
Use caution when measuring combustible or explosive gases.
Do not analyze samples that can release toxic substances during combustion. The
exhaust gas released during analysis passes through the CO2 detector to the CO2
absorber, after which it is used as NDIR purge gas, and then is vented inside the
instrument. Take appropriate countermeasures if there is a possibility that toxic
substances could be included in the exhaust gas. If appropriate countermeasures
cannot be taken, do not perform such analyses.
• The sample analysis results are displayed according to the gas concentration used in calibration. For example, if CO2 is used to generate the calibration curve, the sample analysis result is displayed based on a conversion using the CO2 gas concentration.
• Gaseous samples have certain properties such as adsorption, condensation and reactivity, and some gaseous samples are partially liquid or contain a solid component.
Depending on the properties, certain conditions may occur that cannot be ignored. Some
of these conditions are residual substances and contamination in the flow line, which
may result in peak tailing, carryover, baseline fluctuation, or other analytical problems.
• High concentrations of NOx or SOx in the sample or in the post combustion-oxidized
sample can interfere with the NDIR activity. To evaluate the degree of the interference,
combine the analysis of the base gas without the TOC component together with the
sample analysis.
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4.5 Application Operations
4.5.2 Gas Sample Analysis
4.5.2.1 Analysis Preparation
¬Installation of the Manual Injection Kit
Installation Procedure
1.
Remove the knurled thumbscrew that secures the slider then remove the TC/TN
injector slider, and install the TC/TN block provided in the kit.
2.
If the IC reactor kit is being used, remove the IC injector slider, and install the IC
block provided in the manual injection kit.
Note: When installing the block, be sure that it is aligned with the
injection port.
Software Settings
Select the Manual Injection Kit option in the Instrument Setup Wizard Options window
during System Setup. Refer to Section 3.2.2 "Options Window".
Note:
Selecting the Manual Injection Kit option disables operation of the
TOC-V injector syringe.
Reference: Refer to 4.5.1.1 "Analysis Preparation".
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4.5 Application Operations
4.5.2 Gas Sample Analysis
4.5.2.2 Measurement
The procedure for setting the various parameters is the same as described in Section 4.2
"Setting General Measurement Parameters", Section 4.3 "Measurement Procedures and
Tutorial" and Section 4.4.2.2 "Calibration Curve".
¬Calibration Curve Measurement
Procedure
1.
Prepare standard gas containing a known concentration of carbon.
Note: For IC (carbon dioxide) analysis, prepare a standard gas with a
known carbon dioxide concentration. For TC analysis, another
organic gas (for example, methane) of known concentration can be
used.
2.
From the File menu, select New. The New dialog box is displayed.
Figure 4.191 New Dialog Box
3.
Double-click the Calibration Curve icon. The Calibration Curve Wizard opens. The
System Information window of the wizard (page 1) is displayed.
Figure 4.192 Calibration Curve Wizard (Page 1) System Information
4.
From the System drop-down list, select the system that was configured with the
Manual Injection Kit during setup.
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4.5 Application Operations
4.5.2 Gas Sample Analysis
5.
Select the desired options on pages 2 and 3 of the Calibration Curve Wizard, which
list calibration curve type and analysis information settings, respectively. Enter the
name of the new calibration curve in the text box at the bottom of page 3 of the
wizard.
Note: Select the settings described in Section 4.2 "Setting General Measurement Parameters".
6.
Enter the desired number of injections on page 4 of the Calibration Curve Wizard
(Calibration Measurement Parameters).
7.
Enter the injection volume on page 5 of the Calibration Curve Wizard (Calibration
Points List).
Note: An injection volume is displayed automatically. The displayed
value is based on the volume of the last injection that was performed using the sample injector. This value can be changed by the
user as appropriate.
8.
Select the desired options on pages 6 and 7 of the Calibration Curve Wizard, which
list peak time parameter and history settings, respectively. Click the Finish button to
create the new calibration curve.
Note: Select the settings described in Section 4.2 "Setting General Measurement Parameters".
9.
Create a Sample Table for the calibration curve. From the Insert menu, select
Calibration Curve. Select the newly created calibration curve from the list of files in
the Open dialog box.
10. Connect the instrument by selecting Connect from the Instrument menu. Then select
Start from the Instrument menu. The Manual Injection Parameter dialog box is
displayed.
11. Draw an appropriate amount of sample into the syringe.
Note:
Draw in and discharge the sample 3 or 4 times before filling the
syringe for measurement.
12. Enter the injection volume in the Manual Injection Parameter dialog box, and click
the Set button.
13. Verify that the instrument is ready for measurement, and click the Start button.
14. For TC or TN measurement, open the injection port valve and insert the syringe
needle into the injection port. For IC measurement, insert the syringe needle into the
injection port septum.
Note: • Insert the syringe needle as far as possible into the injection port.
• To obtain reproducible results, perform all injections at the same
speed.
15. Withdraw the syringe from the injection port. For TC or TN measurement, close the
injection port valve.
The results are displayed when measurement is complete.
16. Click Additional Measurements to perform repeat measurements. Repeat the
procedure. Click the Finish button when all measurements are complete.
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4.5 Application Operations
4.5.2 Gas Sample Analysis
¬Sample Measurement
Procedure
1.
From the File menu, select New. The New dialog box is displayed.
Figure 4.193 New Dialog Box
2.
Double-click the Method icon. The Method Wizard opens. The System Information
window of the wizard (page 1) is displayed.
Figure 4.194 Method Wizard (Page 1) System Information
3.
Select the system that was configured with the Manual Injection Kit and used to
create the calibration curve. Advance to page 2 of the Method Wizard (Analysis
Information) and enter the new method name in the text box at the bottom of the
window.
4.
Advance to page 3 of the Method Wizard (Calibration Curves). Select the appropriate
calibration curve file.
5.
Enter “1” in the No. of Injections field on page 4 of the Method Wizard (Injection
Parameters).
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4.5 Application Operations
4.5.2 Gas Sample Analysis
6.
Select the desired options on pages 5, 6, and 7 of the Method Wizard, which list peak
time parameter, USP/EP check, and history settings, respectively. Click the Finish
button to create the new method.
Note: Select the settings described in Section 4.2 "Setting General Measurement Parameters".
7.
From the Insert menu, select Sample. Select the newly created method from the list of
files in the Open dialog box. Complete the remaining pages of the Sample Wizard.
8.
From the Instrument menu, select Start. The Manual Injection Parameter dialog box is
displayed.
9.
Draw an appropriate amount of sample into the syringe.
Note: Draw in and discharge the sample 3 or 4 times before filling the
syringe for measurement.
10. Enter the injection volume in the Manual Injection Parameter dialog box, and click
the Set button.
11. Verify that the instrument is ready for measurement, and click the Start button.
12. For TC or TN measurement, open the injection port valve and insert the syringe
needle into the injection port. For IC measurement, insert the syringe needle into the
injection port septum.
Note: • Insert the syringe needle as far as possible into the injection port.
• To obtain reproducible results, perform all injections at the same
speed.
13. Withdraw the syringe from the injection port. For TC or TN measurement, close the
injection port valve.
14. Click Additional Measurements to perform repeat measurements. Repeat the
procedure. Click the Finish button when all measurements are complete.
¬Maintenance
Replacing the IC Injection Port Septum (Cushion O-Ring)
The septum used with the IC injection port is a consumable item. The septum typically can
be used for 200 or more injections; however, it should be replaced if there is deterioration
in reproducibility or peak shapes.
Part number for replacement cushion O-ring (20 pcs.): P/N 630-01559-01
Replacement Procedure
1.
2.
3.
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Loosen and remove the injection port bushing.
Remove the old septum, and insert a new one.
Replace the bushing and tighten it.
4.5 Application Operations
4.5.2 Gas Sample Analysis
CAUTION
IC reaction solution may spatter close to the injection port septum and injection
port; however, this poses no problem during analysis. When replacing the
septum, wipe away any liquid, taking care to avoid contact.
Gas-tight Syringe
For analysis, use a needle length of 50mm., or a 2-inch gas-tight syringe. The following
gas-tight syringes are available from Shimadzu. Order replacement syringes as necessary.
Table 4.8 • Gas-Tight Syringes (Option)
Part Name
P/N
Capacity
Gas-tight syringe set 25uL
638-60733-02
25uL*
Gas-tight syringe set 50uL
-03
50uL*
Gas-tight syringe set 100uL
-04
100uL*
Gas-tight syringe set 250uL
-05
250uL*
Gas-tight syringe set 500uL
-06
500uL*
Gas-tight syringe 1mL
046-00026-02
1mL
Gas-tight syringe set 5mL
-03
5mL
Gas-tight syringe set 10mL
-04
10mL
* Set comprises one replacement gas-tight syringe needle and one plunger.
Table 4.9 • Relationship Between Appropriate Peak Height and (CO2) Gas
Concentration / Injection Volume *
Gas Concentration (CO2)
TC
IC
Gas Injection Volume
100ppm
10mL
1000ppm
1mL
1%
500uL
10%
300uL
100%
30uL
100ppm
6uL
1000ppm
600uL
1%
300uL
10%
200uL
100%
20uL
*The values indicated in this table are reference values only. Data will vary slightly among
instruments.
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4.5.2 Gas Sample Analysis
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5
5
Maintenance
Inspection and maintenance of the TOC-V instrument are required to ensure normal
operation and reliable and accurate data acquisition.
5.1
Daily Inspection
Describes the daily inspection procedures that should be performed before
instrument startup.
5.2
Periodic Inspections
Describes periodic inspection procedures for the TOC-V.
5.3
Autosampler (ASI-V) Maintenance
Describes periodic inspection procedures for the autosampler.
5.4
8-Port Sampler (OCT-1) Maintenance
Describes periodic inspection procedures for the 8-Port Sampler.
5.5
TN Unit (TNM-1) Maintenance
Describes periodic inspection procedures for the TN unit.
5.6
Software-Controlled Maintenance Functions
Describes maintenance functions controlled by the TOC-Control V software.
5.7
Troubleshooting
Describes the error messages and troubleshooting procedures.
5.1 Daily Inspection
5.1.1 Checking Dilution Water
5.1
Daily Inspection
Check the levels of dilution water, acid, drain vessel water, and humidifier water each day
before starting the instrument.
5.1.1 Checking Dilution Water
Verify that the dilution water volume is sufficient for analysis. If necessary, replenish the
dilution water as described in Section 4.1.6 "Preparation of Dilution Water".
5.1.2 Checking Acid
Verify that the acid volume is adequate for analysis. If necessary, replenish the acid as
described in Section 4.1.7 "Acid Preparation". Any container such as a small-mouth glass 1
liter bottle can be used.
5.1.3 Checking Drain Vessel Water Level
Overflow Tube
Drain
Vessel
Pure Water
Figure 5.1 Drain Vessel Water Level
Verify that the water level in the drain vessel inside the instrument is within 10mm of the
overflow tube on the side of the drain vessel. Replenish as necessary with purified water
(ion-exchange water).
Reference: Refer toSection 4.1.4 "Water Supply to the Cooler Drain Container", for details on adding
purified water,.
Confirm that the carrier gas does not leak from the tip of the drain tubing when the flow
rate is 150mL/min.
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5.1.4
5.1 Daily Inspection
Checking Humidifier Water Level
5.1.4 Checking Humidifier Water Level
Supply Port
Pure Water
“Lo” Mark
Figure 5.2 Humidifier Water Level
Verify that the water level in the humidifier is above the “Lo” mark. If the level is below the
“Lo” mark, replenish by adding purified water through the water supply port on top of the
vessel. Add water until the level reaches the “Hi” mark.
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5.2 Periodic Inspections
5.2.1 Catalyst Regeneration
5.2
Periodic Inspections
Periodically inspect the items listed in this section to maintain instrument performance
quality.
5.2.1 Catalyst Regeneration
Inorganic substances contained in the samples accumulate in the catalyst as salts and
oxides. Buildup of these residues decreases the sensitivity and reproducibility of analyses.
(Catalyst performance can be checked by measuring a standard solution.) This type of
catalyst contamination occurs when measuring alkaline samples and samples that contain
high concentrations of IC compounds. When catalyst contamination occurs, performance
can be restored by regenerating the catalyst. Catalyst regeneration is also an effective
means of reducing the system blank peaks that are present when using new catalyst or
catalyst that has not been used for a long time. The catalyst regeneration procedure has little
effect on TN analysis.
Catalyst is regenerated by injecting dilute hydrochloric acid onto the catalyst. The acid used
in the procedure is 2M hydrochloric acid obtained from the instrument reservoir (acid used
during IC and NPOC analysis). The catalyst regeneration process is the same for both TOC
standard catalyst and TOC high sensitivity catalyst. If performance is not restored after the
regeneration process has been conducted, replace the catalyst. Refer to Section 5.2.2
"Washing or Replacing Catalyst".
Regeneration Procedure
The procedure for regenerating the TC catalyst is controlled by the TOC-Control V
software, as described below.
1.
From the Instrument menu in the Sample Table Editor, select
Maintenance>Regeneration of the TC Catalyst.
The Regeneration of TC-Catalyst dialog box is displayed.
Figure 5.3 Regeneration of TC-Catalyst Dialog Box
238
2.
Click the Start button to begin the procedure. A progress bar is active until the TC
catalyst has been regenerated.
3.
Click the Close button.
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5.2.2
5.2 Periodic Inspections
Washing or Replacing Catalyst
CAUTION
Dilute hydrochloric acid is the only type of acid that can be used to regenerate
TC catalyst. Other acids, particularly phosphoric acid, cause abnormally high
peaks and scattered peak values to occur. If this happens, the catalyst must be
replaced.
5.2.2 Washing or Replacing Catalyst
Large quantities of salts accumulate in the catalyst when measuring samples with high salt
concentrations. If sensitivity and reproducibility do not improve after catalyst regeneration,
wash or replace the catalyst. Refer to Section 5.2.1 "Catalyst Regeneration".
5.2.2.1 Washing Catalyst
Standard catalyst can be washed and reused several times using the following procedure.
High sensitivity catalyst cannot be washed and reused.
WARNING
Due to the danger of burn injury, allow the oven temperature to cool to room
temperature before starting any maintenance procedure involving the
combustion tube or catalyst.
Procedure
1.
2.
3.
4.
Thoroughly wash the catalyst with tap water to remove any accumulated salts.
Neutralize the alkalis with dilute hydrochloric acid (5:1).
Thoroughly wash the catalyst with tap water to remove the hydrochloric acid.
Rinse with pure water (ion exchange water acceptable) and then dry.
CAUTION
•
•
Dry the catalyst at a temperature lower than 700°C to avoid the degradation of
catalyst activity that occurs at higher temperatures.
A large quantity of steam is produced when the regenerated catalyst is placed in
the oven and heated. Due to the danger of burn injury, leave the outlet of the
combustion tube open until no more steam is released.
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5.2 Periodic Inspections
5.2.2 Washing or Replacing Catalyst
5.2.2.2 Replacing Catalyst
If performance is not restored after washing the catalyst, it must be replaced. Replace the
catalyst with new platinum catalyst (alumina spherical support). Keep extra platinum
catalyst on hand for such a contingency. One bottle of platinum catalyst is enough for one
replacement.
Use the following procedure to replace the platinum catalyst.
Procedure
1.
Wash the platinum mesh and the inside of the combustion tube with (1:2)
hydrochloric acid (1 part concentrated HCl and 2 parts water).
2.
3.
4.
Rinse with water.
Dry, and reuse these items.
Fill the combustion tube as described in Section 4.1.1 "Catalyst Filling".
TOC High Sensitivity Catalyst
TOC high sensitivity catalyst cannot be washed and reused like standard catalyst. If
analysis sensitivity and reproducibility are not restored after catalyst regeneration, replace
the deteriorated high sensitivity catalyst with new high sensitivity catalyst. The platinum
mesh and combustion tube can be washed with hydrochloric acid and reused.
Disposal of Catalyst
Used catalyst should be disposed of according to local industrial waste disposal regulations.
It must be clearly disclosed using an industrial waste manifest that the used catalyst
contains platinum.
5.2.2.3 Replacing the Carrier Gas Purification Tube and Catalyst
The carrier gas purification tube burns the carrier gas and oxidizes carbon-based impurities,
converting them to carbon dioxide. The carbon dioxide is absorbed and eliminated by the
CO2 absorber. The carrier gas purification tube is filled with oxidation catalyst (same as
TOC standard catalyst).
The procedure for replacing the purification tube and catalyst is as follows.
Removal of Carrier Gas Purification Tube
WARNING
Before attempting to remove the carrier gas purification tube, be sure to allow
the oven temperature to cool to room temperature. There is a danger of burn
injury if this procedure is performed while the oven is hot.
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5.2.2
5.2 Periodic Inspections
Washing or Replacing Catalyst
Removal Procedure
1.
Remove the compression fitting joints at the top and bottom of the carrier gas
purification tube.
2.
Detach the TC/TN sample injection block from the combustion tube. Refer toSection
4.1.2 "Connecting the Combustion Tube".
3.
Extract the carrier gas purification tube from the electric oven by pulling upward.
Replacing Catalyst
CAUTION
The top nut of the compression fitting joint is hand-tightened. Do not use tools to
tighten or loosen this nut. Because the tube is constructed of quartz glass,
over-tightening or aggressive handling may result in damage.
Procedure
1.
Remove the catalyst from the carrier gas purification tube through the opening at the
top.
2.
3.
Remove the quartz wool using a thin tube or other instrument.
4.
Pack a small amount of quartz wool into the tube from the bottom.
Insert a small amount of new TOC standard catalyst into the combustion tube from
the bottom (straight end).
Note:
The quartz wool is inserted to prevent the catalyst from falling out
of the bottom. Packing too much quartz wool into the tube will
greatly impede airflow, so do not use too much quartz wool. To
prevent contamination of the catalyst or the inclusion of foreign
particles, use the same precautions used when filling the
combustion tube with TOC platinum catalyst.
5.
Insert the straight end of the carrier gas purification tube down into the front 8mm
diameter hole in the oven.
6.
Using the compression fitting joints, restore the tubing connections to their original
condition.
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5.2 Periodic Inspections
5.2.3 Washing/Replacing the Combustion and Carrier Gas Purification Tubes
5.2.3 Washing/Replacing the Combustion and Carrier Gas Purification Tubes
The inner surface of the combustion tube devitrifies (becomes crystalline in texture and
turns white) when it reacts with salts contained in the samples. The tube can continue to be
used in this condition until it breaks or cracks.
During the catalyst washing or replacing process, wash the interior of the combustion tube
and carrier gas purification tube with (1:2) hydrochloric acid (1 part concentrated HCl and
2 parts water) to remove the contaminants and accumulated salts. Rinse with water, dry,
and then reuse the tube(s).
5.2.4 Replacing the High-Purity Air Cylinder
A 47-liter cylinder of high-purity air used as the carrier gas will last for approximately three
months using the H Type instrument, and two months using the N Type.
• Replace the cylinder when the residual pressure diminishes to a few hundredkPa. Do
not wait until it is completely empty.
• When connecting a new cylinder, clean the connections thoroughly. After connecting
the cylinder, do not allow dust or other matter to enter the instrument.
• Keep a spare cylinder available at all times.
5.2.5 Replacing the CO2 Absorber
Once a year, replace each of the CO2 absorbers (P/N 630-00999), which are located in the
holder behind the instrument.
CO2 Absorber Disposal Procedure
Used CO2 absorbers should be disposed of according to local industrial waste disposal
regulations. It must be clearly disclosed using an industrial waste manifest that the used
CO2 absorber contains soda lime.
Reference: For details on replacing the CO2 absorbers, refer to Section 4.1.8 "Installation of the CO2
Absorber".
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5.2.6
5.2 Periodic Inspections
Replacing the Halogen Scrubber
5.2.6 Replacing the Halogen Scrubber
The absorbent inside the halogen scrubber turns black as it absorbs chlorine. The
discoloration band advances toward the outlet as the amount of chlorine absorbed
increases. Replace the scrubber with a new halogen scrubber when the front of the
discoloration band reaches the position shown in Figure 5.4 "Halogen Scrubber".
Replacement Procedure
1.
2.
3.
Unclip the upper and lower clips that secure the halogen scrubber.
Remove the upper and lower connection clamps.
Disconnect the Viton connectors and remove the halogen scrubber.
Gas Flow Direction
Replace Scrubber When
Discoloration Band Reaches
this Point
Dehumidifier
To Sample
Cell Inlet
Halogen Reactant-filled Cylinder
Figure 5.4 Halogen Scrubber
The baseline may fluctuate immediately after replacement. Allow the instrument to run for
a short time until the baseline stabilizes. Stabilization normally occurs within one hour.
Used halogen scrubbers should be disposed of according to local industrial waste disposal
regulations. It must be clearly disclosed using an industrial waste manifest that the halogen
scrubber contains copper.
Clamps
Clips
Viton Connectors
Figure 5.5 Halogen Scrubber Replacement
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5.2 Periodic Inspections
5.2.7 Replacing the Syringe Plunger Tip
5.2.7 Replacing the Syringe Plunger Tip
The syringe plunger tip is constructed of fluororesin and wears with use. Gaps will
eventually form between the plunger and the inner wall of the syringe barrel (glass tube),
causing leaks. When leaks occurs, bubbles are produced near the syringe tip when sample
is drawn into the syringe or sample may leak from the bottom of the barrel when the sample
is discharged. When these problems are observed, replace the plunger tip.
Replacement Procedure
1.
2.
Remove the syringe referring to Section 4.1.3 "Installing the Syringe".
3.
Grasp the plunger tip with a pair of pliers and remove it from the plunger. The O-ring
that is held in place by the plunger tip also comes off. DO NOT reuse this O-ring.
Use a sharp knife to make two or three incisions at the bottom of the plunger tip, as
shown in Figure 5.6 "Removing the Old Plunger Tip".
Figure 5.6 Removing the Old Plunger Tip
4.
Pushing down on the plunger, press the leading edge of the new plunger tip straight
into the plunger tip seat, as shown in Figure 5.7 "Installing the New Plunger Tip
(cross-section)". Save the syringe for future use since the plunger tip seat is enclosed
inside the syringe.
Plunger Tip
Plunger Tip Seat
Figure 5.7 Installing the New Plunger Tip (cross-section)
Note:
• Do not scratch the perimeter of the plunger tip. This could cause leaks.
• Use only Shimadzu-specified plunger tips. Use of unspecified parts may
result in malfunction and/or diminished performance.
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5.2 Periodic Inspections
Replacing Ferrules at the Combustion Tube Outlet Connection
5.2.8
5.2.8 Replacing Ferrules at the Combustion Tube Outlet Connection
For High Sensitivity Analysis Kit
The front and rear Teflon ferrules used in the compression fitting connections at the
combustion tube outlet gradually become deformed and scratched with repeated use, and
may cause gas leakage. When this occurs, replace them with new ferrules. Keep a 6F-T
Sleeve set on hand as replacement parts.
Reference: For details on the replacement procedure, refer to Section 4.1.2 "Connecting the
Combustion Tube".
5.2.9 Replacing the Sliding Sample Injector O-rings
Two types of O-rings are stacked between the injection block and the slider of the sample
injector. If a gas leak develops in this area, replace both O-rings.
•
•
White Upper O-ring: O-ring, Teflon P10 (P/N 036-11408-84)
Black Lower O-ring: O-ring, 4DP10A (P/N 0936-11209-84)
White O-ring
Black O-ring
Figure 5.8 Replacing the Sliding Sample Injector O-rings
If a gas leak develops between the injector block and the combustion tube, replace the
O-ring there as well.
CAUTION
Do not scratch the O-rings or the O-ring seat when replacing the O-rings.
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5.2 Periodic Inspections
5.2.10 Replacing the Syringe Pump 8-port Valve Rotor
5.2.10 Replacing the Syringe Pump 8-port Valve Rotor
The fluororesin rotor of the syringe pump 8-port valve gradually becomes worn and
scratched after prolonged use due to suspended particles in the samples. This wear
eventually causes leaks from the 8-port valve.
The following symptoms are associated with leaks from the 8-port valve and indicate that
rotor replacement is necessary.
• Droplets of liquid around the 8-port valve (especially around the upper shaft)
• Decreased analysis reproducibility
• Presence of bubbles in the syringe
If the leakage is great, sample remaining in the tubing after it is drawn into the syringe may
flow back into the sample container. This is most likely due to a sampling tubing flange or
connection problem.
CAUTION
Switch OFF the instrument before replacing the 8-port valve rotor.
Procedure
1.
2.
Shut down the instrument and turn OFF the power.
Verify that the O mark on the 8-port valve interrupt plate is directed toward the No. 1
port. If not, the instrument was not shut down using the appropriate procedure. In this
case, switch the instrument back ON, and follow the correct shutdown procedure.
Reference: For the correct shutdown procedure, refer to Section 4.3.3 "Ending Measurement".
3.
Remove the nut using the provided wrench.
Nut
Figure 5.9 Removing the Nut
4.
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TOC-VCPH/CPN
Pull up to remove the rotor drive component. Hang it on the screw on the right side of
the plunger.
5.2.10
5.
5.2 Periodic Inspections
Replacing the Syringe Pump 8-port Valve Rotor
Loosen the retaining nut using the provided wrench.
Spring-equipped Rod
Retaining Nut
Figure 5.10 Removing the Retaining Nut
6.
Note the orientation (toward port No. 1) of the flat surface of the spring-equipped rod.
Remove the spring-equipped rod and retaining nut.
7.
Note the orientation of the rotor hole position. Grasp the rotor with forceps and
remove by pulling up.
Rotor
Figure 5.11 Removing the Rotor
8.
9.
Insert a new rotor, taking care that the rotor hole matches original orientation.
Reinsert the retaining nut and spring-equipped rod, with the flat surface directed
toward port No. 1. Tighten the retaining nut.
10. Replace the rotor drive component, and tighten the nut.
11. Switch the instrument ON.
Note:
Perform the syringe pump zero detection procedure before analysis.
Refer to Section 4.1.3.1 "Syringe Pump Zero Point Detection".
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5.2 Periodic Inspections
5.2.11 Replacing the CO2 Absorber for the Optional Carrier Gas Purifier
5.2.11 Replacing the CO2 Absorber for the Optional Carrier Gas Purifier
The NDIR baseline becomes unstable with a decrease in the carbon dioxide absorption in
the carrier gas purifier CO2 absorber. The baseline position rises and reproducibility
diminishes, making analysis impossible. The soda lime must be replaced when this occurs.
The frequency with which soda lime must be replaced depends on the frequency of
analysis, quantity of organic impurities in the carrier gas, and the TOC content of the
samples. It is recommended that soda lime be replaced once every four months.
Soda Lime Replacement Procedure
CAUTION
The carrier gas pressure applied to the carrier gas purifier CO2 absorber is
approximately 200kPa. It is dangerous to perform this maintenance procedure
under these conditions. Before replacing the soda lime, lower the carrier gas
pressure in the instrument to normal as follows:
•
Turn the supply valve of carrier gas source OFF.
•
Switch OFF the instrument.
Procedure
1.
Remove the elbow joints of the carrier gas purifier CO2 absorber, which are behind
the instrument.
2.
3.
4.
Invert the CO2 absorber and remove the screw cap.
Remove the used soda lime.
Refill the absorber container with about 500g of new soda lime until it reaches about
5mm from the interior screw threads.
CAUTION
Do not allow any soda lime to enter the tube in the center of the container when
refilling the CO2 absorber.
5.
Fill the hollow in the screw cap with quartz wool and screw the cap back on the
container.
CAUTION
To maintain an airtight seal, a rubber O-ring is placed between the container and
the screw cap. Inspect the O-ring to verify that it is not scratched or twisted, then
attach the cap.
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5.2.12
6.
5.2 Periodic Inspections
Replenishing IC Reaction Solution
Using the elbow joints, connect the carrier gas purifier CO2 absorber to the two tubes
exiting the back of the instrument as follows:
• Tubing labeled “L”: Affixed to the connection port of the CO2 absorber container
labeled “L”
• Tubing labeled “S”: Affixed to the connection port of the CO2 absorber container
labeled “S”
CAUTION
Tighten the nut by hand only. Do not use tools.
7.
Place the carrier gas purifier CO2 absorber container on the stand behind the
instrument.
Used soda lime should be disposed of according to local industrial waste disposal regulations. It must be clearly disclosed using an industrial waste manifest that the material contains soda lime.
CAUTION
Soda lime is a corrosive chemical substance. Be careful not to touch it with bare
hands. For details, refer to Section 6.9 "Material Safety Data Sheets".
5.2.12 Replenishing IC Reaction Solution
For the H Type, verify that there is sufficient IC reaction solution in the IC reaction solution
vessel before performing IC analysis. If not, replenish the IC reaction solution referring to
Section 4.1.11 "IC Analysis Preparations".
CAUTION
The IC reaction solution is acidic. Use care not to spill or touch the fluid when
handling it. For details, refer to Section 6.9 "Material Safety Data Sheets".
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5.2 Periodic Inspections
5.2.13 Replacing the Pump Head of the IC Reaction Solution Pump
5.2.13 Replacing the Pump Head of the IC Reaction Solution Pump
The IC reaction solution pump is a roller type pump that uses a rotating roller to flatten the
rubber tube carrying the IC reaction solution, thereby feeding solution into the system. This
rubber tubing gradually deteriorates, requiring periodic replacement of the pump head.
The life of the rubber tubing is generally about 300 hours of pump operation. It is
recommended that 300 hours be entered as the warning value in the Maintenance History
dialog box. Refer to Section 4.2.4 "Maintenance History Settings".
CAUTION
The pump head and rubber tubing inside the IC reagent pump are filled with IC
reagent solution. This solution is acidic. Use care to avoid touching or spilling
the solution when changing the pump heads. For details refer to Section 6.9
"Material Safety Data Sheets".
Replacement Procedure
Use the following procedure to replace the rubber tubing of the pump head.
1.
Grasp the front and rear stops of the pump head by hand. Pull the white pump head
from the black pump body.
2.
Disconnect both of the yellow rubber tubes on the left side of the pump head from the
Teflon tubes.
3.
4.
Connect the new rubber tubing to the Teflon tubes of the pump head.
Replace the pump head by following the above procedure in reverse.
Figure 5.12 Replacing the Pump Head of the IC Reaction Solution Pump
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5.2.14
5.2 Periodic Inspections
Replacing the Filler of the Optional POC Analysis CO2 Absorber
5.2.14 Replacing the Filler of the Optional POC Analysis CO2 Absorber
The CO2 absorber for POC analysis is filled with about 6 grams of lithium hydroxide,
which is sufficient to absorb carbon dioxide gas for several hundred analyses under normal
conditions. Airflow resistance gradually increases with use and may become excessive
irrespective of adequate carbon dioxide absorbency.
Replace the lithium hydroxide in the CO2 absorber with a new batch if analysis values
become unstable or carrier gas flow is impeded. For the procedure on filling the CO2
absorber with lithium hydroxide, refer to Section 4.1.12 "Preparation for POC analysis".
CAUTION
•
•
•
•
Lithium hydroxide is a corrosive (strongly alkali) powder. Be carefuel not to spill
or touch it during handling. For details, refer to Section 6.9 "Material Safety
Data Sheets".
Used lithium hydroxide should be disposed of by a certified industrial waste
handler according to local industrial waste disposal regulations. It must be clearly
disclosed using an industrial waste manifest that the waste is lithium hydroxide.
Lithium hydroxide crystal is found in both anhydrous and hydrated forms.
Because the carbon dioxide gas absorbance properties of the hydrated form are
slightly inferior to those of the anhydrous form, use anhydrous lithium hydroxide
to fill the CO2 absorber.
The life of the CO2 absorber will be shortened by performing POC analysis on
samples with high concentrations of IC.
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251
5.3 Autosampler (ASI-V) Maintenance
5.3.1 Rinse Bottle Inspection
5.3
Autosampler (ASI-V) Maintenance
Maintenance of the autosampler includes periodic inspection of the rinse bottle, sample
catcher and rinse pump.
5.3.1 Rinse Bottle Inspection
Perform the following inspections before conducting analysis with the autosampler. If the
following inspections are not properly conducted, air will be drawn into the autosampler
injection pump, preventing the delivery of rinse water.
• Check the rinse water level
Verify that the water in the rinse bottle is above the 2-liter level mark. Add water if necessary.
• Check the rinse tubing
Verify that the tip of the rinse tubing reaches nearly to the bottom of the rinse bottle.
Adjust the tubing position if necessary.
Rinse Tubing
Rinse Bottle
Figure 5.13 Rinse Bottle Inspection
5.3.2 Sample Catcher Inspection
Examine the turntable (black plate) and the sample catcher tray below the turntable when
installing or removing the autosampler vial rack. If they are wet or dirty, wipe them clean.
CAUTION
Corrosion of the instrument may occur if spilled sample is allowed to remain in
the sample catcher. Keep the sample catcher clean.
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5.3.3
5.3 Autosampler (ASI-V) Maintenance
Replacing the Pump Head of the Rinse Pump
5.3.3 Replacing the Pump Head of the Rinse Pump
The rinse pump is located inside the autosampler and supplies rinse water to the rinse port.
The rinse pump is a roller type pump that uses a rotating roller to flatten the rubber tubing
carrying the rinse water, thereby feeding rinse water into the system. This rubber tubing
gradually deteriorates, requiring periodic replacement.
The life of the rubber tubing is generally about 300 hours of pump operation. It is
recommended that 300 hours be entered as the warning value in the Maintenance History
dialog box. For details, refer to Section 4.2.4 "Maintenance History Settings".
Replacement Procedure
Use the following procedure to replace the pump head.
1.
2.
Remove the rectangular pump access cover on the back left side of the autosampler.
3.
On the left side of the pump head, disconnect both of the yellow rubber tubes from the
Teflon tubes.
4.
5.
Connect the new rubber pump head tubing to the Teflon tubes.
Grasp the latch on the pump head by hand and pull the white pump head from the
black pump body.
Replace the pump head by following the above procedure in reverse and then replace
the pump access cover.
Pump
Head
Figure 5.14 Replacing the Pump Head of the Rinse Pump
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253
5.4 8-Port Sampler (OCT-1) Maintenance
5.3.3 Replacing the Pump Head of the Rinse Pump
5.4
5.4.1
8-Port Sampler (OCT-1) Maintenance
Replacing the 8-Port Valve Rotor
The OCT-1 uses a fluororesin 8-port valve rotor. The valve rotor may become worn or
scratched after prolonged use due to the suspended particles in the samples. This wear
eventually causes leaks from the 8-port valve.
The following symptoms are associated with leaks from the 8-port valve and indicate
that it is necessary to replace the rotor.
•
Droplets of liquid around the 8-port valve (especially, around the upper shaft)
•
Decreased analysis reproducibility.
•
Presence of bubbles in the TOC-V syringe.
If the leak is large, sample remaining in the tubing after the syringe has been filled may
flow back into the sample container. This is most likely due to a sample tubing or
flange connection problem.
CAUTION
Switch OFF the power before replacing to the 8-port valve rotor.
Replacement Procedure
1.
Shut down the TOC-V unit and switch OFF the power.
Reference: Refer to Section 4.3.3 "Ending Measurement" for details on shutting down the TOC-V unit.
2.
3.
Remove the 4 screws at the top of the 8-Port Sampler, and take OFF the cover.
Verify that the O mark on the 8-port valve cover is directed toward port No.1.
Note: If the O mark is not directed toward port No.1, the instrument was not
shut down properly. If this is the case, turn the TOC-V on again, and
shut it down properly.
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5.3.3
4.
5.4 8-Port Sampler (OCT-1) Maintenance
Replacing the Pump Head of the Rinse Pump
Remove the nut using the wrench supplied with the TOC-V.
Nut
Figure 5.15 Removing the Nut
5.
6.
Remove the 8-port valve by pulling it downward.
Loosen the retaining nut using the provided wrench.
Retaining Nut
Figure 5.16 Removing the Retaining Bracket
7.
Note the orientation (toward port No. 1) of the flat surface of the spring-equipped rod.
Remove the spring-equipped rod and retaining nut.
8.
Note the orientation of the rotor hole position. Grasp the rotor with forceps, and
remove by pulling upwards.
Rotor
Figure 5.17 Removing the Rotor
9. Insert a new rotor, positioning the rotor hole to the original position.
10. Reinsert the spring-equipped rod and retaining nut with the flat surface directed
toward port No. 1. Tighten the retaining nut.
11. Replace the 8-port valve in its original position, and secure it using the nut.
12. Replace the cover of the 8-Port Sampler and secure it with four screws.
13. Switch on the TOC-V unit.
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5.5 TN Unit (TNM-1) Maintenance
5.5.1 Replacing the Catalyst in the Ozone Treatment Unit
5.5
TN Unit (TNM-1) Maintenance
Maintenance of the TN unit includes periodic inspection of the ozone treatment unit
catalyst, chemiluminescence detector and ozone generator.
5.5.1 Replacing the Catalyst in the Ozone Treatment Unit
The ozone treatment unit breaks down ozone gas produced by the ozone generator. The
catalyst inside the ozone treatment unit must periodically be replaced. Replace the catalyst
once a year for an instrument that runs 8 hours a day and 5 days a week.
Perform maintenance to the ozone treatment unit only after stopping the instrument as
described inSection 4.3.3 "Ending Measurement".
CAUTION
The interior of the ozone treatment unit is heated to 50°C. Perform maintenance
only after cooling for at least two hours.
Replacement Procedure
Use the following procedure to replace the catalyst in the ozone treatment unit.
1.
Remove the knurled screw at the bottom of the unit, and remove the installation
bracket.
Ozone
Treatment Unit
Knurled Screw
Installation Bracket
Figure 5.18 Removing the Ozone Treatment Unit Screw and Bracket
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TOC-VCPH/CPN
5.5.1
2.
5.5 TN Unit (TNM-1) Maintenance
Replacing the Catalyst in the Ozone Treatment Unit
Remove the hose clamp at the bottom of the ozone treatment unit and pull off the
Viton tubing.
Hose Clamp
Viton Tubing
Figure 5.19 Removing the Viton tube
3.
Remove the hose clamp at the top of the unit and remove it from the Viton coupling.
Hose Clamp
Viton Coupling
Figure 5.20 Removing the Ozone Treatment Unit
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5.5 TN Unit (TNM-1) Maintenance
5.5.1 Replacing the Catalyst in the Ozone Treatment Unit
4.
Remove the cap from the ozone treatment unit and take out the used catalyst and
polypropylene packing material.
Figure 5.21 Emptying and Removing the Ozone Treatment Catalyst
5.
Pack a small amount of new polypropylene packing material into the bottom of the
ozone treatment unit, then fill with approximately 60 grams of catalyst.
6.
7.
8.
Insert a small amount of new polypropylene packing material on top of the catalyst.
Place the cap back on the container.
Remove the Viton coupling connecting the detector exhaust opening to the inlet of the
ozone treatment unit.
Replace this Viton coupling with a new one whenever the catalyst is replaced. Inspect
the Viton tubing at the outlet of the ozone treatment unit and replace it if cracked or
damaged.
9.
Reconnect the Viton tubing and Viton coupling, and reinstall the ozone treatment unit.
CAUTION
Used catalyst should be disposed of according to local industrial waste disposal
regulations. It must be clearly disclosed using an industrial waste manifest that
the catalyst contains manganese dioxide.
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5.5
5.5.2
TN Unit (TNM-1) Maintenance
Chemiluminescence Detector
5.5.2 Chemiluminescence Detector
The light receiving window of the chemiluminescence detector may become soiled by
components in the samples. Inspect and clean the window and gasket at least once a year.
Maintenance Procedure
Perform maintenance on the detector only after shutting down the instrument.
1.
After removing the tubing from the reactor, as shown in the figure below, loosen the 4
mounting screws, and detach the reactor.
Detector
Reactor
Mounting
Screws
Gasket
Figure 5.22 Removing the Reactor
2.
3.
Remove the gasket and confirm that it is not dirty or cracked. Replace it if necessary.
4.
Place the flat side of the gasket facing the detector window, sandwiching it between
the window and the reactor.
5.
6.
Secure the gasket in place with the 4 mounting screws, tightening them uniformly.
Confirm that the detector window is not dirty. If necessary, gently wipe the window
clean with a cloth.
Reconnect the tubing.
CAUTION
Recheck the tubing after completing the maintenance work to make absolutely
certain that there are no mistakes in the line connections and that everything has
been properly tightened.
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5.5 TN Unit (TNM-1) Maintenance
5.5.3 Ozone Generator Replacement
5.5.3 Ozone Generator Replacement
Replace the ozone generator with a new one after 8000 hours of operation. Set a warning
generation value of 8000 hours in the Maintenance History dialog box. For details, refer to
Section 4.2.4 "Maintenance History Settings".
Ozone generator replacement must be carried out by an authorized Shimadzu service
engineer, or someone who has been properly trained in the procedure. Contact your
Shimadzu representative to request replacement at the appropriate time.
Confirming Operation Time
The ozone generator operating time is displayed in the Maintenance History window,
which is accessed through the Sample Table Editor. From the Instrument menu, select
Maintenance>Maintenance History.
CAUTION
If the ozone generator is used after 8000 hours of operation, ozone generation
may not be sufficient for analysis, or ozone may leak from inside the generator.
Replace the ozone generator without fail.
5.5.4 Replacing the NOx Absorber
The NOx absorber absorbs NOx gas generated in the TN unit. A CO2 absorber is used for
the NOx absorber. The CO2 absorber was previously used for purging the NDIR detector
optical system Section 5.2.5 "Replacing the CO2 Absorber" and is still effective for this
application.
During the annual replacement of the CO2 absorber used to purge the optical system of the
NDIR detector, replace the NOx absorber for the TN unit with the used CO2 absorber from
the TOC-V.
Discarding the NOx Absorber (CO2 Absorber)
Place a request to an authorized industrial waste contractor to process the used NOx
absorber (CO2 absorber). Clearly indicate in the industrial waste material manifest that the
absorber contains soda lime.
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5.6
5.6
Software-Controlled Maintenance Functions
5.6.1 Zero Point Detection
Software-Controlled Maintenance Functions
Maintenance functions that can be performed using the TOC-Control V software are
described below. These functions can be accessed through the Instrument>Maintenance
menu.
Figure 5.23 Instrument>Maintenance Menu
To access the menu, select Instrument>Maintenance in the Sample Table Editor.
5.6.1 Zero Point Detection
Use this function to determine the zero point of the syringe. Click the Start button to begin
the procedure, during which a progress bar is active. The progress bar becomes inactive
after the syringe zero point is determined. Click the Close button.
Figure 5.24 Zero Point Detection Dialog Box
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5.6 Software-Controlled Maintenance Functions
5.6.2 Regeneration of the TC Catalyst
5.6.2 Regeneration of the TC Catalyst
Use this function to restore the sensitivity and efficiency of the TC catalyst, which decrease
over time as inorganic substances are deposited on the catalyst surface. During the
procedure, dilute hydrochloric acid is injected onto the catalyst. Be sure to verify that
sufficient hydrochloric acid is in the instrument acid reservoir before starting the procedure.
Figure 5.25 Regeneration of TC Catalyst Dialog Box
Click the Start button to begin the procedure. A progress bar is active until the TC catalyst
is regenerated. Click the Close button.
5.6.3 Regeneration of the IC Solution
Use this function to restore the acidity of the IC solution, which decreases over time as the
acid reacts with IC sample constituents. During the procedure, IC reagent is automatically
pumped to the IC reaction vessel. This option is available only if an IC unit is connected to
the system.
Figure 5.26 Regeneration of IC Solution Dialog Box
Click the Start button to begin the procedure. A progress bar is active until the IC solution
is regenerated. Click the Close button.
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5.6
Software-Controlled Maintenance Functions
5.6.4 Residue Removal
5.6.4 Residue Removal
Use this function to remove residue from the flow lines and syringe.
Figure 5.27 Residue Removal Dialog Box
Click the Start button to begin the procedure. A progress bar is active until the residue
removal procedure is complete. Click the Close button.
5.6.5 Replace Flowline Content
Select this command to replace the contents of the flow lines connected to the 8-port valve
from the dilution solution bottle and the hydrochloric acid bottle.
Figure 5.28 Replace Flow Line Content Dialog Box
Click the Start button to begin the procedure. A progress bar is active until the flow line
content has been replaced. Click the Close button.
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5.6 Software-Controlled Maintenance Functions
5.6.6 Flowline Washing
5.6.6 Flowline Washing
Use this function to wash the selected flow lines.
Figure 5.29 Washing Dialog Box
To perform flow line washing, click the Select Flow Lines button to open the Wash Flow
Lines dialog box. Select the flow lines to be washed, and click the Washing button. The
ports for the 8-Port Sampler 1 (2) can be selected if the 8-Port Sampler 1 (2) is being used.
Figure 5.30 Wash Flow Lines Dialog Box
While this process is being executed, the buttons in the Washing dialog box are disabled,
and progress bar activity is displayed.
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5.6
Software-Controlled Maintenance Functions
5.6.7 Mechanical Check
5.6.7 Mechanical Check
Select this function to check mechanical components of the instrument or to make
adjustments. The Mechanical Check window consists of several tabs, one for each
connected instrument.
¬TOC Tab
Figure 5.31 Mechanical Check Window: TOC Tab
Syringe Pump
Use the buttons to move the syringe pump to the Zero, Home, or Sparge positions. Click the Reset button to move the plunger to the highest position.
Solenoid Valves
Use the buttons to open or close the various solenoid valves. Different options
are available depending on the instrument configuration and oxidation method.
Port Select
Open the line between the syringe and an injection port by clicking the button for
the desired port.
TC Inj. Port
Specify whether the port should be set to drain or measure by clicking the appropriate button.
IC Inj. Port
Specify whether the port should be set to drain or measure by clicking the appropriate button.
Acid Pump
Use the buttons to open or close the IC acid pump lines.
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5.6 Software-Controlled Maintenance Functions
5.6.7 Mechanical Check
¬ASI / 8-Port Sampler Tab
Figure 5.32 ASI / 8-Port Sampler Tab of Operation Verification Dialog Box
Rinse
Use the On and Off buttons to start and stop the ASI flow line rinsing option.
Move Tray
Use the directional arrows to move the ASI tray to the desired position. Click the
Reset button to return the tray to its home position.
Arm
Use the directional arrows to move the arm vertically. Use the drop-down list to
move the arm horizontally.
Vial Position
Use the spin controls to enter a vial position, then click the Move button to verify
that the arm moves to the specified vial position. This is the only option that is
enabled for systems using the OCT-1 8-port sampler.
Magnetic Stirrer
Use the On and Off buttons to start and stop the magnetic stirrer.
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5.6
Software-Controlled Maintenance Functions
5.6.8 ASI / 8-Port Sampler Initialization
5.6.8 ASI / 8-Port Sampler Initialization
Use this function when first connecting the instrument to establish communication between
the TOC-Control V software and the ASI or 8-Port Sampler. This option is disabled if an
ASI or 8-Port Sampler is not connected to the system.
Figure 5.33 Initialize ASI / 8-Port Sampler Window
Click the Start button to begin the procedure, during which a progress bar is active. The
progress bar becomes inactive after the ASI or 8-Port Sampler is initialized. Click the Close
button.
5.6.9 ASI Rack Change
Use this function to change the ASI rack. This option is disabled if an ASI is not connected
to the system.
Figure 5.34 ASI Rack Change Window
Click the Preparation Start button to begin the procedure. A progress bar is active while the
rack moves to the position where it can be replaced. When the progress bar begins blinking,
replace the rack. Click the Finish Replacement button to initialize the ASI and complete the
rack change process. Click the Close button.
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5.6 Software-Controlled Maintenance Functions
5.6.10 ASI Needle Change
5.6.10 ASI Needle Change
Use this function to change the ASI needle. This option is disabled if an ASI is not
connected to the system.
Figure 5.35 ASI Needle Change Window
Click the Preparation Start button to begin the procedure. A progress bar is active while the
needle moves to the position where it can be replaced. When the progress bar begins
blinking, replace the needle. Click the Finish Replacement button to initialize the ASI and
complete the needle change process. Click the Close button.
5.6.11 Change Syringe
Use this function to replace the syringe.
Figure 5.36 Syringe Change Window
Click the Preparation Start button to begin the procedure. A progress bar is active while the
syringe moves to the position where it can be replaced. When the progress bar begins
blinking, replace the syringe. Verify that the syringe moves smoothly between the upper
and lower positions by clicking the directional arrows. Click the Finish Replacement button
to move the syringe to its initialization position, then click the Close button.
Note:
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Perform the zero point detection procedure whenever a new syringe is installed
or the syringe is replaced. Refer to Section 4.1.3.1 "Syringe Pump Zero Point
Detection".
5.6
Software-Controlled Maintenance Functions
5.6.12 Blank Check
5.6.12 Blank Check
Use this function to automatically determine the background TC level of the instrument.
Conducting the Blank Check procedure is recommended prior to performing high
sensitivity measurements and after loading high sensitivity catalyst. Open a blank Sample
Table, connect the instrument, and select the Blank Check option from the Instrument
menu. Refer to Section 4.1.15.2 "TC Blank Check Analysis" for details. Set the injection
volume using the spin controls, then click the Start button to begin the procedure.
Figure 5.37 Blank Check Parameters Window
Note:
Do not insert a sample into the Sample Table. The Blank Check procedure only
works in a blank Sample Table.
5.6.13 Maintenance Log
Refer to Section 4.2.4 "Maintenance History Settings" for more details.
5.6.14 History
Use this option to view the operational history of various instrument components and to set
limits for various parameters of the components. When a limit is exceeded for an
instrument component, a warning message will be generated on the PC screen to remind the
user to perform maintenance on the component. Refer to Section 4.2.4 "Maintenance
History Settings" for a detailed description of this function.
5.6.15 Sparge Gas Valve
Select this option to start and stop the flow of sparge gas when the external sparge kit is
used.
5.6.16 Adjust Sparging Flow Rate (Wet Chem.)
Use this function to adjust the sparge gas flow rate. This option is available only when the
wet chemical oxidation method is used.
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5.7 Troubleshooting
5.7.1 Error Messages
5.7
Troubleshooting
This section describes the error messages displayed by the TOC-Control V software and
the actions recommended to resolve the underlying causes.
5.7.1 Error Messages
The following error messages are displayed on the PC screen when setting or operation
errors are made, or when problems with instrument operation occur. Take the corrective
actions indicated in the table below.
Table 5.1• Error Message List 1
Error Message
270
Description
Corrective Action
WARNING: Dilution water
depleted
Actual amount of dilution water used
exceeds value set in the Maintenance
History Settings.
Replenish the water in the dilution water container. Then, reset the Dilution Water amount in
the Maintenance History Settings.
WARNING: Acid depleted
Actual amount of hydrochloric acid
used exceeds value set in the Maintenance History Settings.
Replenish the hydrochloric acid in the acid container. Then, reset the Total Acid Volume in the
Maintenance History Settings.
ERROR: Combustion tube
sample injections exceeded.
Actual volume of sample injected into
combustion tube exceeds value set in
the Maintenance History Settings.
Either regenerate the catalyst or replace the catalyst and combustion tube. Then, reset the Total
TC Injection Volume in the Maintenance History
Settings.
ERROR: Syringe stroke number exceeded
Actual number of syringe strokes perReplace the plunger tip. Then, reset the Syringe
formed exceeds value set in the Mainte- Stroke value in the Maintenance History Setnance History Settings.
tings.
WARNING: IC pump tube
operating hours exceeded.
Actual IC pump tubing operation time
exceeds value set in the Maintenance
History Settings.
Replace the IC pump tubing. Then, reset the IC
Unit Pump time in the Maintenance History Settings.
WARNING: ASI pump tube
operating hours exceeded.
Actual ASI pump tubing operation time
exceeds value set in the Maintenance
History Settings.
Replace the ASI pump tubing. Then, reset the
ASI Rinse Pump time in the Maintenance History Settings.
TOC-VCPH/CPN
5.7 Troubleshooting
5.7.1 Error Messages
Table 5.2• Error Message List 2
Error Message
Description
Corrective Action
Information entered is incorrect.
Re-enter user name and password.
The user name and password entered are not
valid.
Enter the correct user name and
password. These fields are
case-sensitive. If the user account
has not been set up, contact the
system administrator.
Database path not found.
The specified file does not exist in the specified
path.
Check the file name and path.
Check if the specified file has been
deleted or moved, or if the system
used for the file has been deleted.
Opening of communication port
has timed out. Check instrument
connection and transmission settings.
The process of opening the communication port
has timed out.
Verify that the instrument is
switched on, and that the instrument connection and communication port settings are correct.
Closing of communication port has
timed out. Transmission will be
ended.
The process of closing the communication port
has timed out.
Verify that the instrument is
switched on, and that the instrument connection and communication port settings are correct.
Communication is automatically
closed in that condition.
Instrument initialization has timed
out.
The process of initializing the instrument has
timed out.
Check if there is a problem with
the instrument operation, or if there
is a problem with communication
between the PC and the instrument.
The selected communication port
is already open. Verify that it is not
used with another connection.
An attempt was made to open a communication
port that has already been opened.
Check if the selected port is being
used with another connection.
Cannot open communication port.
Check instrument status and transmission settings.
The communication port failed to open.
Verify that the instrument is
switched on, and that the instrument connection and communication port settings are correct.
Mode error: Check instrument con- The operation was not accepted due to the instru- Verify the instrument operation. If
dition. If necessary, restart instrument condition.
necessary, restart the instrument.
ment.
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5.7 Troubleshooting
5.7.1 Error Messages
Table 5.3• Error Message List 3
Error Message
Description
ERROR: Syringe Zero Point
Detection.
Syringe zero point detection could
not be performed. Syringe is not
properly installed.
Corrective Action
Properly mount the syringe. Then select Zero
Point Detection from the Maintenance menu.
WARNING: TC furnace temper- TC furnace temperature is too low to
ature is too low to regenerate cat- perform the catalyst regeneration
alyst.
procedure.
Wait for the furnace temperature to rise before
executing the catalyst regeneration procedure.
ERROR: Vial rack not present.
Operation cannot continue because
there is no vial rack in the turntable.
Mount a vial rack, and then execute the operation
again.
ERROR: Vial rack has been
exchanged.
Measurement cannot be performed
because the vial rack specified in the
settings differs from the type actually detected.
Verify the type of vial rack mounted in the
ASI-V, and then set the vial rack type in the software.
ERROR: Vial rack type not set.
The measurement parameters cannot
be validated because the vial rack
type is not specified in the software.
Set the vial rack type in the software.
ERROR: ASI Cover is open.
The ASI-V cover is open. The
ASI-V operation has stopped as a
safety measure.
Close the ASI-V cover.
The following messages indicate that an error has occurred that prevents measurement
from continuing. Take the appropriate corrective actions as indicated in the following table.
If the cause of the problem cannot be discovered, or if the same error message appears after
taking the indicated corrective actions, contact your Shimadzu representative.
Note:
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When the following errors are generated, power to the instrument oven is automatically stopped. When power to the oven is switched on again, wait until the
temperature rises before starting measurement.
5.7 Troubleshooting
5.7.1 Error Messages
Table 5.4• Error Message List 4
Error Message
Description
Corrective Action
ERROR: ROM Write
Error
An error occurred while writing to
memory.
Switch off power to the instrument. Contact your Shimadzu representative.
ERROR: Electric Furnace Overheating
The electric furnace overheated.
With the power ON, wait approximately 20 minutes for
the oven temperature to decrease then switch OFF the
instrument. After switching on the power and running
the instrument again, see if the same error is generated.
ERROR: Electric Furnace Sensor
The oven temperature does not rise.
ERROR: Syringe Position Detection
The syringe is not operating normally.
Switch off power to the instrument. After switching on
the power and running the instrument again, see if the
same error is generated.
ERROR: Syringe Opera- The syringe is not operating normally
Switch off the instrument, and remove any foreign partition
due to clogging of the tubing connected cles from the line. After switching on the power and
to the 8-port valve.
running the instrument again, see if the same error is
generated.
ERROR: Syringe Zero
Point Detection
The syringe is not operating normally.
ERROR: 8-Port Valve
Position Detection
The 8-port valve is not operating norSwitch off the instrument, and remove the rotor from the
mally due to clogging inside of the sam- 8-port valve. Remove any particles found in the 8-port
ple injector 8-port valve.
valve and wash valve.
ERROR: TC Slider
The TC slider is not operating normally Switch off the instrument, inspect the slider and remove
due to particles wedged between the
any foreign particles from the slider mechanism. Then
moving parts.
switch on the power again.
ERROR: IC Slider
The IC slider is not operating normally
due to particles wedged between the
moving parts.
ERROR: ASI Arm Verti- The ASI-V arm is not operating norcal Position Detection
mally in the vertical direction.
ERROR: ASI Arm Verti- The ASI-V arm is not operating norcal Movement
mally in the vertical direction.
ERROR: ASI Arm Hori- The ASI-V arm is not operating norzontal Position Detection mally in the horizontal direction.
ERROR: ASI Arm Hori- The ASI-V arm is not operating norzontal Movement
mally in the horizontal direction.
Switch off the instrument. After switching on the power
and running the instrument again, see if the same error
is generated.
Switch off power to the TOC-V main instrument. After
switching on the power and running the instrument
again, see if the same error is generated.
Since the problem is unrelated to the TOC-V main unit,
disconnect the ASI-V from the main unit, and perform
operations using the TOC-V main unit alone until normal operation of the ASI-V is restored.
ERROR: ASI Turntable
Position Detection
The ASI-V turntable position could not
be detected. Either the rack is not properly seated in the turntable, or some
object may be blocking a position detection notch on the periphery of the rack.
Switch off power to the TOC-V main unit. Make sure
the rack is properly seated, and remove any objects that
may be blocking the position detection notch on the
periphery of the rack. After eliminating the cause of the
problem, place the cover on the ASI-V, and switch on
the power to the instrument again.
ERROR: TN Reactor
Temperature
The TNM-1 reactor temperature does
not rise.
Switch off power to the TOC-V main unit. After switching on the power and running the instrument again, see
if the same error is generated.
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5.7 Troubleshooting
5.7.2 Troubleshooting
Table 5.4• Error Message List 4
Error Message
8-Port Sampler 1 position detection
8-Port Sampler 1 operation
8-Port Sampler 2 position detection
8-Port Sampler 2
operation
Description
Corrective Action
8-Port Sampler 1 operation error
occurred due to foreign matter infiltration into 8-port valve, etc.
Switch off instrument. Remove 8-port valve rotor from
8-Port Sampler 1, remove debris, etc., and wash valve.
8-Port Sampler 2 operation error
occurred due to foreign matter infiltration into 8-port valve, etc.
Switch off instrument. Remove 8-port valve rotor from
8-Port Sampler 2, remove debris, etc., and wash valve.
5.7.2 Troubleshooting
5.7.2.1 TOC-V
(1) An error message is displayed.
→Refer to error message.
(2) The Ready lamp will not light.
→ Access the Background Monitor screen by selecting Background Monitor from the
Instrument menu. Refer to the screen to see which parameters are not satisfied.
(3) The baseline stays over the auto zero range. Baseline position never reaches the ready
state.
Does carrier
gas flow normally
to the analysis
cell?
NO
Carrier gas leak.
Repair the leak.
YES
Is dehumidifier
within the specified
temperature?
NO
The dehumidifier temperature
setting is bad.
YES
The infrared gas
analyzer is bad.
Contact your Shimadzu
representative.
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Contact your Shimadzu
representative.
5.7
5.7.2
Troubleshooting
Troubleshooting
(4) The baseline is unstable.
Is carrier gas
flowing normally?
NO
Carrier gas leak.
YES
Was
the catalyst
replaced?
Repair the leak.
NO
Accumulated obstructing
substance.
YES
Is the
dehumidifier
operating
normally?
Replace the catalyst.
NO
The dehumidifier is bad.
YES
Are
external
conditions (vibration,
temperature, power
voltage)
normal?
YES
The infrared gas analyzer
is bad.
Contact your Shimadzu
representative.
NO
External conditions are
adverse.
Eliminate the adverse
condition.
Contact your Shimadzu
representative.
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5.7 Troubleshooting
5.7.2 Troubleshooting
(5) Poor reproducibility with standard solution.
Is the
standard solution
normal?
NO
Bad standard solution.
Prepare new standard
solution.
YES
Is the
sample injected
normally from injection
tube?
NO
Poor injection condition.
YES
Do
bubbles remain
in syringe? (especially
in dilution
analysis)
Adjust injector.
YES
Poor injection volume
repeatability.
Eliminate bubbles.
NO
Was plunger tip
replaced recently?
NO
Backlash of plunger tip.
YES
Does
carrier gas
sometimes leak from
the drain
bottle?
Replace plunger tip.
YES
Low water level.
NO
Does the
poor reproducibility
occur in the
TC or IC
Replenish the water.
IC
IC reaction solution has
deteriorated.
circuit?
Regenerate the IC reaction
solution.
TC
Was the
TC catalyst
regenerated?
NO
Insufficient regeneration of
theTC catalyst .
YES
TC catalyst deteriorated.
Replace the TC catalyst.
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Regenerate the TC catalyst.
5.7
5.7.2
Troubleshooting
Troubleshooting
(6) No peaks appear after sample injection.
Is
sample
injected into TC
combustion tube or IC
reaction vessel?
NO
(confirm
Poor injection.
visually)
Correct the injection
condition.
YES
Is carrier gas
always flowing from
the drain
bottle?
YES
Is the
level of the water
normal in the
drain bottle?
NO
Low water level.
YES
Was membrane filter
replaced?
Replenish water.
NO
Clogged membrane filter.
YES
Bad infrared gas analyzer.
Contact your Shimadzu
representative.
Replace the membrane filter.
Large resistance downstream
of dehumidifier.
Contact your Shimadzu
representative.
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5.7 Troubleshooting
5.7.2 Troubleshooting
5.7.2.2 ASI-V
(1) The ASI-V does not operate.
Is
connection
cable and power cable
properly connected?
NO
Improperly connected cable.
Properly connect the cables.
YES
Bad electrical system.
Contact your Shimadzu
representative.
(2) Rinse water is not delivered from the rinse port.
Is there
sufficient
rinse water in rinse
NO
water bottle?
Insufficient rinse water.
YES
Is the
rinse tubing
properly inserted into
the rinse water
bottle?
YES
The rinse pump is bad.
Contact your Shimadzu
representative.
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Replenish the rinse water.
NO
The rinse tubing is not properly
inserted into rinse water bottle.
Properly insert the tubing into
the rinse water bottle.
5.7
5.7.2
Troubleshooting
Troubleshooting
(3) Reproducibility is poor.
Is there
any material
adhering to the
sample
needle?
YES
Poor reproducibility due to
foreign matter.
Remove the obstruction from
the opening at the tip of the
sample needle.
NO
Is there
a leak at the
connection of sample
needle and ASI
sample
tubing?
YES
Air is drawn in at the
connection.
NO
Properly reconnect the tubing.
Poor reproducibility due to
a problem with the TOC-V.
Refer to Troubleshooting #1.
TOC-V item (5)
5.7.2.3
8-Port Sampler OCT-1
(1) 8-Port Sampler does not operate.
Are the signal and
power cables properly
connected?
YES
NO
Cables are not properly
connected.
Connect the cables properly.
Electrical system is defective.
Contact your Shimadzu
representative.
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5.7 Troubleshooting
5.7.2 Troubleshooting
(2) Reproducibility is poor.
Is any foreign material
adhering to the sample
tubing?
YES
Reduced reproducibility due to
foreign material.
Eliminate blockage at the tip of the
sample tubing.
NO
Is the leakage
present at the 8-port valve
and sample tubing
connection?
YES
Connection is leaking.
Connect the tubing properly.
NO
Poor reproducibility is due to the
TOC-V unit.
Refer to the TOC-V User Manual.
5.7.2.4 Corrective Actions for Poor Reproducibility
Corrective Action for Poor Sample Injection
The manner in which sample is discharged from the TC or IC sample injection tubing has a
large influence on reproducibility. The sample should be injected as vertically as possible
onto the TC catalyst or into the IC reaction vessel. If the sample is scattered or injected
obliquely, detach the sample injection tubing from the slider, and remove any obstruction
that may be adhering to the opening at the tip of the sample tubing.
Appropriate
Unacceptable
(oblique spray)
Unacceptable
(scattered spray)
Figure 5.38 Sample Injection Patterns from Sample Tubing
Ensure that the tip of the tubing does not protrude beyond the bottom surface of the slider.
The O-ring or other seal parts will be scratched if the tubing protrudes, resulting in gas
leaks. The sample is not properly injected unless the tip of the tubing extends into the
depression in the bottom of the slider.
Check the state of the injection for TC analysis by looking through the TC combustion tube
while it is attached to the instrument. The sample injection tubing can be detached from the
slider, and water can be injected for inspection using the functions available in the
Instrument>Maintenance>Mechanical Check screen.
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5.7
5.7.2
Troubleshooting
Troubleshooting
Salt or other substances adhering to the tip of the tubing after rinsing can allow large
droplets of sample to remain on the tip of the tubing after injection. A deformed tip on the
sample injection tubing (a beard-like protrusion, for example) may cause the sample to be
injected obliquely. In either case, reproducibility is adversely affected and the sample
injection tubing should be replaced. Another option available only if there is sufficient
length of tubing remaining is to use a sharp cutting tool at a 90° angle to cut off 2 - 3mm
from the tip of the currently used sample injection tubing.
Tube
Bushing
Packing (spacer,
washer, gasket)
Approximately
2 - 2.5mm
Figure 5.39 Slider Assembly
Corrective Action to Eliminate Bubbles Inside the Syringe
Small bubbles that adhere to the inside of the syringe by the plunger tip will have little
effect on analysis values. Larger bubbles inside the syringe will affect values and result in
poor reproducibility. Large bubbles form easily inside a dirty syringe. This is evident when
sample is mixed with dilution water in the syringe and when sparging with carrier gas
inside the syringe for IC removal pretreatment for NPOC analysis. In this case, detach the
syringe from the syringe pump. Repeatedly draw in and discharge laboratory glassware
detergent to wash the inside of the syringe. Then draw in a full-stroke volume of the
cleaning agent and let it sit for about 20 minutes, or overnight if the syringe is extremely
dirty. Thoroughly rinse away all of the detergent and reattach the syringe to the syringe
pump.
Decreased Reproducibility Due to Plunger Tip Backlash
The plunger tip is a consumable item and, as it is used, wears in the following ways:
(1) The surface of the plunger tip becomes worn and the seal between the plunger tip and
the inside of the glass syringe barrel deteriorates, allowing slight amounts of water to
leak out with vertical movements of the plunger.
(2) The contact site of the plunger tip and plunger becomes loose, causing a slight
backlash with vertical movement of the plunger.
As the above conditions start to occur, repeatability of sample injection volume decreases,
resulting in diminished analysis reproducibility. Item (2) above rapidly leads to decreased
reproducibility. Since it is very difficult to determine backlash by inspecting movement of
the plunger tip, inspect as follows.
Before sample injection, observe the wash injection used to replace the previous sample in
the syringe and flow line with the new sample. After injection, if a droplet forms at the tip
of the injection tubing and increases in size, there is a strong possibility that backlash has
increased. The corrective action in this case is to replace the plunger tip.
Note:
The effect of backlash increases with smaller sample injection volumes. Poor
results might be obtained with a sample injection volume of 10µL, while the
effect might be negligible with a 100µL sample injection volume.
TOC-VCPH/CPN
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5.7 Troubleshooting
5.7.2 Troubleshooting
282
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6
6
Reference Information
This chapter describes the principles of analysis and lists instrument specifications,
accessories, and parts. This chapter also includes installation procedures, for use in the
event that the instrument is relocated.
6.1
Principles of Analysis
The principles for TC, IC, POC, NPOC, TOC and TN analysis are described in
this section.
6.2
Analysis-Related Technical Information
This section summarizes technical information related to analysis, including
peak area analysis and calibration curve selection.
6.3
Specifications
This section lists specifications for the TOC-VCPH/CPN main unit, autosampler,
TN unit and the various optional kits.
6.4
Standard Accessories
The standard accessories are listed in this section.
6.5
Special Accessories
The optional accessories are listed in this section.
6.6
Consumable Parts List
The consumable parts are listed in this section.
6.7
Maintenance Parts List
The maintenance parts are listed in this section.
6.8
Installation
The installation site requirements and installation procedures for future
relocation of the instrument are described here.
6.9
Material Safety Data Sheets
Material Safety Data Sheets are provided in this section.
6.1 Principles of Analysis
6.1.1 Principles of TC (Total Carbon) Analysis
6.1
Principles of Analysis
Two types of carbon are present in water: organic carbon and inorganic carbon. Organic
carbon (TOC) bonds with hydrogen or oxygen to form organic compounds. Inorganic
carbon (IC or TIC) is the structural basis for inorganic compounds such as gas carbonates
and carbonate ions. Collectively the two forms of carbon are referred to as total carbon
(TC) and the relationship between them is expressed TOC=TC-IC.
Nitrogen is also present in water in two types: organic and inorganic. The sum of these is
referred to as total nitrogen (TN).
The principles underlying TC and TN analysis are explained in the following sections.
6.1.1 Principles of TC (Total Carbon) Analysis
Sample is introduced into the TC combustion tube, which is filled with an oxidation
catalyst and heated to 680°C. The sample is burned in the combustion tube and, as a result,
the TC components in the sample are converted to carbon dioxide. Carrier gas, which flows
at a rate of 150mL/min to the combustion tube, carries the sample combustion products
from the combustion tube to an electronic dehumidifier, where the gas is cooled and
dehydrated. The gas then carries the sample combustion products through a halogen
scrubber to remove chlorine and other halogens. Finally, the carrier gas delivers the sample
combustion products to the cell of a non-dispersive infrared (NDIR) gas analyzer, where
the carbon dioxide is detected. The NDIR outputs an analog detection signal that forms a
peak; the peak area is measured by the TOC-Control V software.
The peak area is proportional to the TC concentration of the sample. A calibration curve
equation that mathematically expresses the relationship between peak area and TC
concentration can be generated by analyzing various concentrations of a TC standard
solution. The TC concentration in a sample can be determined by analyzing the sample to
obtain the peak area and then using the peak area in the calibration curve equation.
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6.1.2
6.1 Principles of Analysis
Principles of IC (Inorganic Carbon) Analysis
6.1.2 Principles of IC (Inorganic Carbon) Analysis
Two methods for measuring IC using the TOC-V are available: analysis within the injection
syringe and analysis using the optional IC reactor. In both methods, the measured IC
consists of carbon derived from carbonates, hydrogen carbonates and dissolved carbon
dioxide.
Defining IC
The IC measured by TOC analysis consists of the carbon contained in carbonates and in
carbon dioxide dissolved in water. By acidifying the sample with a small amount of
hydrochloric acid to obtain a pH less than 3, all carbonates are converted to carbon dioxide
(CO2) by the following reactions:
Me2CO3 + 2HCl --> CO2 + 2MeCl + H2O
MeHCO3 + HCl --> CO2 + MeCl + H2O
Carbon dioxide and dissolved carbon dioxide in the sample are volatilized by bubbling
(sparging) air or nitrogen gas that does not contain carbon dioxide through the sample.
Analysis Using the IC Reaction Vessel (H Type Instrument)
The TOC-V IC reactor kit is used to sparge the IC reaction solution (acidified reaction
liquid) with carrier gas. Sample is injected into the IC reaction vessel and the IC in the
sample is converted to carbon dioxide, which is volatilized by the sparging process and
detected by the NDIR.
Analysis Within the Syringe (N Type Instrument)
The sample is acidified to pH 3 or lower in the syringe, using hydrochloric acid. The
sample is sparged with carrier gas and the IC in the sample is converted to carbon dioxide
and detected by the NDIR.
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285
6.1 Principles of Analysis
6.1.3 Principles of NPOC (Non-Purgeable Organic Carbon) Analysis
6.1.3 Principles of NPOC (Non-Purgeable Organic Carbon) Analysis
After acidifying the sample to pH 2 to 3, sparge gas is bubbled through the sample to
eliminate the IC component. The remaining TC is measured to determine total organic
carbon, and the result is generally referred to as TOC. However, in the TOC-V, this analysis
value is referred to NPOC to distinguish it from the TOC value obtained by calculating the
difference between TC and IC. NPOC stands for non-purgeable organic carbon and refers
to organic carbon that is present in a sample in a non-volatile form.
NPOC and TOC (obtained by IC elimination) described in the TOC-related standard
methods and referred to in water quality-related test methods (JIS, ASTM, EPA, EN) are
identical. Purgeable organic substances in the sample can be lost during the sparging
process. Consequently, when the sample contains purgeable organic substances, TOC
should not be measured by the NPOC method. If the dissolved purgeable organic
component in the water sample is large, the amount volatilized during sparging is relatively
small. Generally, the amount of purgeable organic substances in natural environmental,
public and purified water is small; as a result, NPOC can be referred to as TOC.
Table 6.1 • Residual Rate of Volatile Organic Substances using Sparging (Nitrogen Gas)
Organic Substance
286
Pre-Sparging Conc.
Post-Sparging Conc.
(ppm)
(ppm)
Methanol
117. 5
116
98.6
Ethanol
106.5
105
98.5
Isopropyl alcohol
129
127
98.5
n-butyl alcohol
117
115
98.3
Acetone
106
101
95.3
Acetaldehyde
130
117
90.0
Ethyl acetate
102
88
86.3
Tyrosine
117
116.5
99.5
Benzene
85
2.5
2.9
Cyclohexane
79
2
2.5
TOC-VCPH/CPN
Residual Rate (%)
6.1.4
6.1 Principles of Analysis
Principles of POC (Purgeable Organic Carbon) Analysis
6.1.4 Principles of POC (Purgeable Organic Carbon) Analysis
POC analysis is used to measure the volatilized component of TOC, which is produced
during the NPOC sample sparging process. As a result, NPOC+POC is equivalent to TOC.
POC analysis is performed as follows.
Sparge gas containing the volatilized CO2 and POC components of the sample is carried to
the lithium hydroxide-filled CO2 absorber to eliminate the CO2 that was converted from the
IC in the sample. The gas, which now contains only the POC component of the sample,
then passes through the combustion tube to be oxidized. The POC component is converted
to CO2 during oxidation and the CO2 is detected by the NDIR. Data processing is
conducted in the same manner as for TC.
POC is not precisely defined. Factors that determine whether or not, or to what degree, a
volatile organic carbon component is volatilized during sparging include the type of
organic compound, the gas/liquid contact with the sparge gas, and the ambient temperature
during sparging. The target of POC analysis is the organic component present in the
aqueous phase. As a result, organic compounds that are highly soluble in water (such as
methanol or ethanol) and not easily volatilized by sparging produce almost no peaks in
POC analysis.
Organic compounds with low solubility in water (such as methylene chloride or
chloroform) produce sharp peaks in POC analysis. Over a long period of time, compounds
such as acetone and methyl isobutyl ketone generate extremely broad, tailing peaks with no
specific end time.
The lithium hydroxide-filled CO2 absorber eliminates the carbon dioxide that was
generated along with the POC substances. Therefore, POC components that are easily
caught in the CO2 absorber (such as esters) produce low values in POC analysis. POC
results obtained using this technique are not absolute. The user should take all the above
factors into consideration when measuring POC using this instrument.
TOC-VCPH/CPN
287
6.1 Principles of Analysis
6.1.5 Principles of Measuring TOC
6.1.5 Principles of Measuring TOC
TOC can be measured using the following 3 methods:
• TC-IC Method
• NPOC Method
• POC+NPOC Method
TC-IC Method
In the TC-IC method, TOC is measured as the difference between the TC and IC analysis
values. The TC-IC method is not recommended for samples that contain more IC than TOC
(samples where TC consists almost entirely of IC); the NPOC method is recommended for
such samples. The TOC value determined using the TC-IC method includes errors
associated with each of the individual TC and IC measurements, and can therefore result in
a large error in the TOC value.
Because detection accuracy decreases with increasing IC concentration, the NPOC method
is also recommended for samples containing IC concentrations exceeding 10ppm for TOC/
TN catalyst and 5ppm for high sensitivity catalyst.
NPOC Method
The NPOC method is the most widely used TOC analysis method. The NPOC method is
not recommended for samples that foam during sparging. Samples that become foamy
during sparging tend to form bubbles that flow out of the syringe, which removes the
concentrated TOC sample components and leaves a small amount of TOC in the syringe.
The TC-IC method is recommend in this situation.
POC+NPOC Method
The POC+NPOC method should be used when the amount of POC present in the sample
cannot be disregarded.
6.1.6 Principles of Measuring TN (Total Nitrogen)
When a sample is introduced into the combustion tube (furnace temperature 720°C), the
TN in the sample decomposes to nitrogen monoxide. Nitrogen gas does not become
nitrogen monoxide under these circumstances. The carrier gas, which contains the nitrogen
monoxide, is cooled and dehumidified by the electronic dehumidifier. The gas then enters a
chemiluminescence gas analyzer, where the nitrogen monoxide is detected. The detection
signal from the chemiluminescence gas analyzer generates a peak and the TN concentration
in the sample can then be measured.
Note:
TN Detection Rate
In TN analysis, the state (crystalline state) in which TN exists in the sample
greatly affects the TN detection rate. Nitrogen contained in nitrates, nitrites,
ammonia and the majority of other organic nitrogen compounds exhibit high
detection rates. Conversely, some organic nitrogen-containing compounds (such
as hydrazines, pyrazolones, and azide compounds) have detection rates ranging
from 10% to 60%, depending on the concentration.
288
TOC-VCPH/CPN
6.2
6.2
Analysis-Related Technical Information
6.2.1 Peak Area Analysis
Analysis-Related Technical Information
6.2.1 Peak Area Analysis
When a sample is analyzed, the TOC-Control V software automatically detects the
beginning and end of each peak produced, and calculates the peak areas. Detection of the
beginning and end of each peak is based on the slope of the tangent, which changes from
moment to moment. Peak detection begins when that slope exceeds a predetermined value
and ends when a negative slope falls below a specified value.
Note:
• Separated Peaks: In TC analysis, multiple peaks may occur when a large
quantity of sample is injected. Only the end of the last peak is detected. The
total area of the multiple peaks is calculated.
• Baseline Correction: Baseline correction is performed for peaks produced
with fluctuating baseline to obtain the correct peak area.
Figure 6.1 Determining Peak Area
6.2.2 Peak Shape
Multiple peaks are especially prominent when using the high sensitivity catalyst with
sample injections greater than 100µL. As sample is injected onto the catalyst, the easily
volatilized organic substances and the crystalline organic substances are combusted at
different rates. As a result, carbon dioxide is generated multiple times, resulting in the
formation of multiple peaks. Easily volatilized organic substances are organic compounds
that are volatilized with water when an aqueous solution of the compounds is heated;
ethanol is one example of such a compound. Crystalline organic compounds remain in a
solid form following the heating of an aqueous solution of the compound; glucose is one
example of such a compound.
The manner in which the sample is injected also has an effect on peak shape. If a portion of
the sample is injected into the center of the combustion tube while another portion is
injected at the periphery, combustion may occur at different times, resulting in multiple
peaks.
Peak shape does not affect the analysis results. Even if multiple peaks occur due to the type
of organic substance or injection manner described above, the TOC-Control V calculates
the total area of the peaks generated to determine the TOC (or TC) accordingly.
TOC-VCPH/CPN
289
6.2 Analysis-Related Technical Information
6.2.3 Calibration Curves
6.2.3 Calibration Curves
6.2.3.1 Types of Calibration Curves
1-Point and 2-Point Calibration Curves
The output signals of the TOC-V are linearized. As a result, there are almost no factors in
the reaction systems of the TC/TN combustion and IC reaction components that might
cause the concentration-output characteristic to deviate from linearity. Consequently,
calibration curves are commonly generated as 1-point curves consisting of 1 span point, or
2-point curves consisting of 1 span point and the zero point.
The concentration of TC and IC, or of TN, varies with standard solutions prepared with
pure water. A calibration curve generated using concentrations greater than 50 - 100mg/L
will pass very close to the zero point. In this case, it is practical to generate a 1-point
calibration curve.
Use a 2-point calibration curve when the concentration of TC and IC or TN in the pure
water used to prepare the standard solutions cannot be disregarded with respect to the
standard solution concentration. For information on handling of this type of curve, refer to
Section 6.2.3.2 "Shifting of Calibration Curves".
Multi-Point Calibration Curves
Calibration curves can be generated using up to 10 points. Calibration curves consisting of
3 or more points can be generated as a point-to-point curve or as a regression line using the
least squares method. With the least squares regression curve, a correlation coefficient is
displayed.
6.2.3.2 Shifting of Calibration Curves
Shift to Origin
The “shift to origin” function is used when the amount of TC and IC or TN in the pure
water used for standard solution preparation cannot be ignored with respect to the standard
solution concentration. A correction must be made by shifting the calibration curve in a
parallel fashion so that it passes through the origin. This corrects for the TC and IC or TN
concentration in the water used for standard solution preparation. An example of a situation
in which the “shift to origin” function is useful is described below.
When water containing 0.5mg/L TC is used to prepare a 10mg/L TC standard solution, the
actual TC concentration in the standard solution will be 10.5mg/L (0.5mg/L from the water
+ 10mg/L from the standard solution). The 2-point calibration curve generated using such a
solution is shown by the solid line in Figure 6.2 "Shifting of Calibration Curve". If this
curve is used without correction, the sample analysis values will always be 0.5mg/L less
than the true value. By shifting the calibration curve so that it passes through the origin, as
shown by the broken line in Figure 6.2 "Shifting of Calibration Curve", the calibration
curve is effectively corrected.
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TOC-VCPH/CPN
6.2
Analysis-Related Technical Information
6.2.3 Calibration Curves
A system blank is water that contains absolutely no carbon (zero water). When
measurement of a system blank produces a peak, the TC concentrations measured in
samples will be biased high by the amount of TC in the system blank. In most cases (with
the exception of high sensitivity analysis), this bias is not significant. Measurement error
resulting from the TC or TN content in the water used to prepare standard solutions is
typically much greater than measurement error resulting from the system blank value.
Correcting the calibration curve based on the TC or TN content in the standard solution
preparation water will produce satisfactory analyses. Using this correction method, the
value obtained for a system blank would be greater than zero by the amount of the blank
value.
The instrument allows shifting of calibration curves only to the extent of the system blank
value. The system blank peak height varies with such factors as the system configuration
and the type of catalyst used.
Shift to Blank Point
The “shift to blank point” procedure is performed for high sensitivity analyses when the
system blank value could have a significant effect on the measurement value.
Peak Area Value
By selecting the “shift to blank point” option, a TC blank check analysis is performed using
the same injection volume that will be used for sample measurement. The calibration curve
zero point is shifted to the TC blank check value.
0
(0.5)
TC Concentration (mg/L)
10
(10+0.5)
Figure 6.2 Shifting of Calibration Curve
TOC-VCPH/CPN
291
6.2 Analysis-Related Technical Information
6.2.4 Sparging During Standard Solution Analysis
6.2.4 Sparging During Standard Solution Analysis
Standard solutions that have TC concentrations so low as to be affected by the amount of
dissolved carbon dioxide in the solution should be sparged with carrier gas prior to
measurement. Sparging eliminates the dissolved carbon dioxide, thereby preventing it from
affecting the concentration of the standard solution.
The amount of dissolved carbon dioxide in water used for standard solution preparation is
affected by factors such as water purification method, length and condition of storage, and
the concentration of carbon dioxide in the atmosphere. Concentrations of dissolved carbon
dioxide increase when the water is exposed to the atmosphere during the standard solution
preparation process. Refer to “Table 6.2 • CO2 Content (ppm) in Distilled Water
Equilibrated with Atmosphere Temperature (°C)” for the dissolution rates of atmospheric
carbon dioxide in water.
It is important to consider both the concentration of the standard solution and the
concentration of TOC contained in the preparation water when deciding whether to use the
sparging function. Use of sparging is appropriate if the TOC contained in the water is low
enough to not substantially affect the standard solution concentration, but not low enough
to be ignored.
Note:
Do not use sparging with IC standard solutions, as sparging decreases the IC concentration.
Table 6.2 • CO2 Content (ppm) in Distilled Water Equilibrated with Atmosphere
Temperature (°C)
Atmospheric CO2
0
5
10
15
20
25
30
0.030
1.00
0.83
0.79
0.59
0.51
0.44
0.38
0.033
1.10
0.91
0.76
0.65
0.56
0.48
0.42
0.044
1.47
1.22
1.02
0.87
0.74
0.64
0.56
(vol%)
The above CO2 content can be converted to IC using the following equation.
IC (ppm) = CO2 (mg/L) x 0.27
6.2.5 Automatic Selection of Optimum Calibration Curve
Up to three different calibration curves can be selected for use in a method. The curves are
specified in the “Calibration Curve 1”, “Calibration Curve 2” and “Calibration Curve 3”
fields on page 3 of the Method Wizard when the method is being created. Refer to Section
4.4.2.3 "Method Wizard" for more information. When more than one calibration curve is
specified, the TOC-Control V software automatically selects the optimum calibration curve
to be used for calculating measurement results.
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TOC-VCPH/CPN
6.2.5
6.2 Analysis-Related Technical Information
Automatic Selection of Optimum Calibration Curve
The automatic selection process occurs on a measurement-by-measurement basis.
Measurement values are always calculated first using Calibration Curve 1. The TOCControl V software then evaluates the result, applies the optimum calibration curve, and
recalculates the value if necessary. The calibration curve with a concentration range that is
greater than and closest to the measured value is used. Examples are shown below:
(1) If the measured value is less than the concentration of Calibration Curve 1 and greater
than the concentration of Calibration Curve 2 and Calibration Curve 3, Calibration
Curve 1 is used.
Conc. of Calibration Curve 1 > Measured Value > Conc. of Calibration Curves 2 and 3 →
Calibration Curve 1 is used
(2) If the measured value is less than the concentrations of Calibration Curve 1 and
Calibration Curve 2, and if the concentration of Calibration Curve 2 is less than that of
Calibration Curve 1, Calibration Curve 2 is used.
Conc. of Calibration Curve 1 > Conc. of Calibration Curve 2 > Measured Value →
Calibration Curve 2 is used
(3) If three calibration curves are specified, the calibration curve that is greater than and
closest to the measured value is used.
Conc. of Calibration Curve 1 > Conc. of Calibration Curve 3 > Measured Value > Conc. of Calibration
Curve 2 →
Calibration Curve 3 is used
(4) If the measured value is greater than the concentration of all curves and the
concentration of Calibration Curve 1 is greater than the concentration of Calibration
Curves 2 and 3, Calibration Curve 1 is used.
Measured Value > Conc. of Calibration Curve 1 > Conc. of Calibration Curve 2 > Conc. of Calibration
Curve 3 →
Calibration Curve 1 is used
Note:
By setting the concentration ratio between calibration curves to a factor of
approximately 10, the automatic selection function can be effectively utilized for
analyses covering a wide range of concentrations. For example, use a concentration of 10ppm for Calibration Curve 1, 100ppm for Calibration Curve 2, and
1000ppm for Calibration Curve 3.
Considerations for the Automatic Selection Function
• The automatic selection process rules do not change when multi-point calibration
curves are included.
• When more than one injection is performed, the calibration curve is selected based
on the measured value of the first injection.
• Because the measured value is always calculated first using Calibration Curve 1,
specify the most commonly used calibration curve in this field.
• The priority of the second and third calibration curves is determined based on the
calibration curve concentrations and the sample concentration.
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293
6.3 Specifications
6.3.1 TOC-VCPH/CPN
6.3
Specifications
6.3.1 TOC-VCPH/CPN
Analyte
TC, IC, TOC (TC-IC), NPOC
Measurement principle
680°C catalytically-aided combustion oxidation/non-dispersive
infrared detection (NDIR)
Measuring range
TC: 0 - 25000mg/L
IC:
• TOC-VCPH: 0 - 30000mg/L
• TOC-VCPN: 0 - 3000mg/L
Detection limits
TC:
• TOC-VCPH: 4µg/L
• TOC-VCPN: TC: 50µg/L
IC: 4µg/L
Measurement time
TC: Approx. 3min
IC:
• TOC-VCPH: Approx. 3min
• TOC-VCPN: Approx. 4min
Repeatability
CV within 1.5%
Sample introduction
Auto injection using syringe pump/slider
Sample injection volume
10 - 2000µL (variable)
Sample dilution function
Dilution within syringe, dilution factor 2 - 50 times
Pretreatment for IC
Automatic acid addition and sparging
Carrier gas
High purity air (from cylinder)
Carrier gas pressure
Approx. 300 - 600kPa
Carrier gas flow rate
TOC-VCPH: 150mL/min (230mL/min when performing in-syringe
sparging)
TOC-VCPN: 230mL/min
294
Ambient temperature
5 - 35°C
Power requirements
AC 100-120V ±10% or AC 220-240V ±10%, 6 A, 50/60Hz (power
consumption: approx. 230VA)
Fuse
8A.T (100V Systems) 15A.T (200V Systems)
Approximate dimensions
(W) 440 x (D) 560 x (H) 460mm (excluding projections)
Weight
Approx. 40kg
TOC-VCPH/CPN
6.3
Specifications
6.3.2 ASI-V
6.3.2 ASI-V
Sample containers
24mL vial rack: 24mL (External diameter 23 x Height 85mm), 100
vials, 100 septum-equipped caps
40mL vial rack: 40mL (External diameter 27 x Height 9mm), 72
vials, 72 septum-equipped caps
Vial rack capacity
24mL vial rack: 93nvials
40mL vial rack: 68 vials
Sample pretreatment
•
•
•
Acid addition and sparging possible for NPOC analysis
Needle rinse possible
Stirring with magnetic stirrer (with optional magnetic stirrer)
Ambient temperature
5 - 35°C
Approximate dimensions
(W) 370 x (D) 540 x (H) 490mm (excluding projections)
Weight
Approx. 13kg
6.3.3 OCT-1 8-Port Sampler
No. of sample containers
accommodated
8 containers
Ambient temperature
5 - 35° C
External dimensions
Approx. (W) 245 x (D) 245 x (H) 440mm (excluding protruding
parts)
Weight
Approx. 3.5 kg
Analyte
TN (total nitrogen)
Measurement principle
Thermal decomposition / NO detection (chemiluminescence
method)
Measuring range
0 - 4000mg/L
Measurement time
Approx. 4min
Repeatability
CV within 3%
Ambient temperature
5 - 35°C
Power requirements
AC 100-120V ±10% or AC 220-240V ±10%, 6 A, 50/60Hz (power
consumption: approx. 230VA)
Approximate dimensions
(W) 160 x (D) 235 x (H) 400mm (excluding projections)
Weight
Approx. 8kg
16 containers (using 2 OCT-1 units)
6.3.4 TNM-1
TOC-VCPH/CPN
295
6.3 Specifications
6.3.5 POC Kit
6.3.5 POC Kit
Analyte
POC
Measurement method
Sparging / CO2 removal / combustion oxidation
CO2 removal method
Absorption via lithium hydroxide, removal
Measuring range
0 - 500mg/L
Measurement time
Approx. 4min
Repeatability
CV within 5%
6.3.6 Carrier Gas Purifier Kit
Gas purification method
Combustion oxidation / CO2 removal
Carrier gas supply
Pressurized air or oxygen (free of dust, oil mist, water droplets, etc.)
Carrier gas supply pressure
300 - 600kPa
6.3.7 Manual Injection Kit (Gas Sample Injection Kit)
Analyte
Liquid samples: TC, IC, TOC (TC-IC)
Gas samples: TC, carbon dioxide, TOC (determined by TC-carbon dioxide;
Carbon monoxide and other inorganic carbon containing gases aside from
carbon dioxide are also measured as TOC)
Measurement of IC, TOC and carbon dioxide is possible with the TOC-VCPH
Measurement principle
680°C catalytically-aided combustion oxidation/non-dispersive infrared
detection (NDIR)
Measuring range
Liquid sample:
• TC: 0 - 20000mg/L
• IC: 0 - 20000mg/L
Gas sample:
6ppm - 100% CO2
Sample injection volume Liquid sample: 1 - 150µL
Gas sample: 20µL - 10mL
Measuring time
Liquid sample:
• TC: Approx. 3min
• IC: Approx. 3min
Gas sample: 2 - 4min
Repeatability
Liquid sample: CV within 2% (CV is within 3% when sample concentration
is 8000mg/L or greater)
Gas sample: CV within 2%
Sample introduction
296
TOC-VCPH/CPN
Manual injection using microsyringe
6.3.8
6.3 Specifications
PC Hardware Requirements
6.3.8 PC Hardware Requirements
PC
IBM-PC/AT or compatible, with 9-pin RS-232C connector
CPU
233MHz or better
Memory
32 MB or greater
Hard drive
2 GB or greater
OS
Windows95, Windows98, Windows2000, WindowsNT 4.0 (SP3 or
later), WindowsXP (*For compliance with FDA 21 CFR Part 11, use
Windows2000)
The User Authentication function cannot be used with WindowsXP.
Monitor resolution
800 x 600 or better, 1024 x 768 suggested
TOC-VCPH/CPN
297
6.4 Standard Accessories
6.3.8 PC Hardware Requirements
6.4
Standard Accessories
Table 6.3 • Standard Accessories List 1 (TOC-VCPH/CPN)
Part Number
298
Part Name
TOC-VCPH
TOC-VCPN
638-41323
Combustion tube, in case
2
1
638-92069-02
TOC regular catalyst set
1
1
638-92070-01
TOC high sensitivity catalyst set
1
-
638-16023
Catalyst filling rod
1
1
630-00999
CO2 absorber
1
1
630-00315-09
Plastic tube 9mm ID x 12mm OD
2m
2m
071-60813
Adapter, ground
1
1
071-60814-01
Power cord set (100-127V)
1
1
071-60814-06
Power cord set (220-240V)
1
1
638-59213-01
Plunger tip
1
1
630-00635-01
Potassium biphthalate, 2g
1
1
630-00962-01
Sodium carbonate, 25g
1
1
638-59213
Syringe
1
1
017-30812-01
Silicone grease
1
1
072-60359-01
Wiring band
2
2
630-00963-01
Sodium bicarbonate, 25g
1
1
072-02004-25
Fuse, 218 008 (100-127V)
2
2
072-02004-27
Fuse, 218 015 (220-240V)
2
2
631-20265
Plug, 35154
1
1
631-78002
Wrench, for 8-port valve
1
1
638-52337
Rinse water bottle
1
1
638-20072
Cap
1
-
638-60074
Ceramic fibers
1
1
638-64727
CD-ROM “TOC-Control V”
1
1
638-74029
Cable, (RS-232C)
1
1
631-81214
Plate, for CO2 absorber
1
1
035-55026-02
Half union
1
1
038-00292-04
Plastic bottle
2
1
638-94241
Instruction manual
1
1
TOC-VCPH/CPN
6.4 Standard Accessories
PC Hardware Requirements
6.3.8
Table 6.4 • Standard Accessories List 2 (ASI Unit)
Part Number
Part Name
24mL
40mL
638-41462
Vials, 24mL
100
038-00165-21
Vials, 40mL (with cap, septum)
638-20074-01
Cap, 24mL
100
038-00165-48
Septum, 24mL
100
638-52337
Rinse water bottle
1
1
072-60310-03
Wiring band, TM-53M
2
2
631-51869-20
Name plate, SAMPLE
1
1
631-51869-21
Name plate, GAS
1
1
072-60301
Wiring band, Nylon TY-23M
1
1
638-74027
Cable ASSY, ASI, signal
1
1
638-41448-01
Needle, regular type 24, 40
1
1
72
TOC-VCPH/CPN
299
6.4 Standard Accessories
6.3.8 PC Hardware Requirements
Table 6.5 • Standard Accessories List 3 (OCT-1 8-Port Sampler)
Part Number
Part Name
8-Port
8-Port
Details
Sampler 1 Sampler 2
631-20265
Plug 35154
1
638-41443-03
Common Tubing C
1
638-41443-04
Additional Common
Tubing C2
638-41443-05
Common Tubing W
638-41443-06
Additional Common
Tubing W2
638-41337-03
Flanged Tubing C*
631-41660
1
Rotor (for replacement
maintenance)
Common port connection
tubing**
1
Common port connection
tubing****
Common port connection
tubing**
1
1
Common port connection
tubing****
1
1
Sample tubing for combustion
analyzers (CSH/CSN/CPH/
CPN)
Flanged Tubing W***
1
1
Sample tubing for wet
chemical analyzers (WS/WP)
638-74004-01
Power Cable
1
Cable for connection to the
main unit
638-74028-01
Power Cable
1
Cable for connection to the
main unit
638-74028-02
Power/Signal Cable
M393-E228
User Manual
1
Cable for connecting 8-Port
Sampler 1 to 8-Port Sampler 2
1
* Flanged tubing in C sets have an inner diameter of 1.0 mm. This set is provided for use
with the combustion type TOC-V.
** Connect this tubing to the common (COM) port of the 8-Port Sampler and port No. 2 on
the TOC-V unit.
*** Flanged tubing in W sets have an inner diameter of 1.5 mm. This set is provided for use
with the wet chemical type TOC-V.
**** Connect this tubing to the common (COM) port of the 8-Port Sampler and port 1on the
TOC-V unit.
300
TOC-VCPH/CPN
6.3.8
6.4 Standard Accessories
PC Hardware Requirements
Table 6.6 • Standard Accessories List 4 (TN Unit)
Part Number
Part Name
Qty
630-00999
CO2 absorber
1
638-60074
Ceramic fibers
1
017-40533-01
Potassium nitrate
1
072-02004-19
Fuse, 218 002
1
020-46547
SS screw pan head M 4 x 8
5
631-81157
Mounting plate TNM
1
072-60301
Wiring band, TY-23M
5
630-00315-05
Plastic tubing 5mm ID x 7mm OD
5m
631-41200-02
Viton tubing 5mm ID x 8mm OD
0.45
638-52353-03
Ozone treatment unit ASSY
1
035-60690-97
Tee
2
016-43284-01
Tube
0.1m
072-60338-03
Clip
2
638-42035
Capillary
1
071-60813
Adapter
1
071-60814-01
Power cord set (100-127V)
1
071-60814-06
Power cord set (220-240V)
1
Table 6.7 • Standard Accessories List 5 (Manual [Gas Sample] Injection Kit)
Part Number
Part Name
Qty
638-10194
Block, M-INJ TC ASSY
1
638-10195
Block, M-INJ IC ASSY
1
631-43291
Syringe packing
10
Table 6.8 • Standard Accessories List 6 (POC Measurement Kit)
Part Number
630-00557
Part Name
Quartz wool
Qty
1
TOC-VCPH/CPN
301
6.4 Standard Accessories
6.3.8 PC Hardware Requirements
Table 6.9 • Standard Accessories List 7 (Carrier Gas Purifier Kit)
Part No.
302
Part Name
Qty
638-42013
L-shaped combustion tube (in case)
1
638-60116
TOC regular catalyst
1
630-00557
Quartz wool
1
638-52578-01
CO2 absorber container
1
630-00556
Soda lime
1
638-40168
Compression fitting, elbow
4
016-37504
Teflon tube (3×4)
2.9m
040-82074-03
Filter
1
035-65104
Union
2
016-43284-01
Nylon tube
0.1m
TOC-VCPH/CPN
6.3.8
6.5
6.5 Special Accessories
PC Hardware Requirements
Special Accessories
Table 6.10 • Special Accessories List
Part Number
Part Name
CommentComment
638-93141-04
Autosampler ASI-V (24mL)
24mL vials
638-93141-08
Autosampler ASI-V (40mL)
40mL vials
638-93150-01
8-Port sampler OCT-1
For TOC-VCPH/CPN/CSH/CSN
638-93150-11
8-Port sampler OCT-2
unit)
638-91065-01
TN unit TNM-1
For AC 100-127V
638-91065-02
TN unit TNM-1
For AC 220-240V
638-91066
POC measurement kit
638-72596
Option wiring kit
638-41447
Carrier gas purifier kit
638-77152
External sparge kit
638-93149-03
Manual injection kit
638-41460
Suspended solids kit (when used
with TOC-V alone)
638-93151
Suspended Solids Kit (when
autosampler is used)
638-53044-01
Sample rack and vial sets for
24mL sample vials
(second
For TOC-VCPH/CPN/CSH/CSN
Required to install the POC kit or
external sparge kit for the TOC-VCPH
24mL sample rack
24mL sample vials
Vial caps
Septa
638-53044-02
Sample rack and vial sets for
40mL sample vials
40mL sample rack
40mL sample vials
Vial caps
Septa
638-67075
Stirrer (for 24mL vials)
For autosampler 24mL vials
638-67076
Stirrer (for 40mL vials)
For autosampler 40mL vials
046-00617-02
Stirrer bar (for 24mL vials)
Stirrer bar for 24mL vials, 1 required for
sample measurement
046-00617-03
Stirrer bar (for 40mL vials)
Stirrer bar for 40mL vials, 1 required for
sample measurement
630-00960
High purity air cylinder
Recommended that user provide this
item.
630-08585-05
Cylinder pressure regulator
User can provide this item.
638-41204
Air supply tubing set (with 20
meters of tubing)
User can provide this item.
630-02525-01
High speed homogenizer
638-52344
Drain bottle (for ASI)
TOC-VCPH/CPN
303
6.6 Consumable Parts List
6.3.8 PC Hardware Requirements
6.6
Consumable Parts List
Table 6.11 • Consumable Parts List 1 (TOC-VCPH)
Part Number
304
Part Name
Comment
638-41323
Combustion tube, in case
638-60116
TOC regular catalyst
630-00105-01
Platinum mesh
To support catalyst, 2
included
630-00557
Quartz wool
To support catalyst, 1g
630-00996
TOC high sensitivity catalyst
638-41308-01
Cooling coil
630-00999
CO2 absorber
630-00992
Halogen scrubber
036-11209-84
O-ring, 4D P 10A
For slider, 5pcs.
036-11408-84
O-ring, Teflon P10
For slider, 5pcs.
036-11222-84
O-ring, 4D P22
For IC reaction tube, 5pcs.
036-11219-84
O-ring, 4D P20
For TC reaction tube, 5pcs.
035-62994-03
Sleeve set 6F-T
042-00405-11
IC reaction solution supply
pump head
630-00635-01
Potassium biphthalate, 25 g
630-00962-01
Sodium carbonate, 25 g
630-00963-01
Sodium bicarbonate, 25 g
046-00044-11
Membrane filter
017-30812-01
Silicone grease, H.V.G.
630-08913-01
Chart paper
638-60074
Ceramic fibers
631-20265
8-port valve rotor
638-59213-01
Plunger tip
638-92206-01
Consumables set
TOC-VCPH/CPN
10 rolls
Refer to Table 6.13 for
contents
6.3.8
6.6 Consumable Parts List
PC Hardware Requirements
Table 6.12 • Consumable Parts List 2 (TOC-VCPN)
Part Number
Part Name
Comment
638-41323
Combustion tube, in case
638-60116
TOC regular catalyst
630-00105-01
Platinum mesh
To support catalyst, 2
included
630-00557
Quartz wool
To support catalyst, 1g
630-00999
CO2 absorber
Contains 500mL
630-00992
Halogen scrubber
036-11209-84
O-ring, 4D P 10A
For slider, 5pcs.
036-11408-84
O-ring, Teflon P10
For slider, 5pcs.
036-11219-84
O-ring, 4D P20
For TC reaction tube, 5pcs.
630-00635-01
Potassium biphthalate, 25 g
630-00962-01
Sodium carbonate, 25 g
630-00963-01
Sodium bicarbonate, 25 g
046-00044-11
Membrane filter
017-30812-01
Silicone grease, H.V.G.
638-60074
Ceramic fibers
631-20265
8-port valve rotor
638-59213-01
Plunger tip
638-92206-02
Consumables set
Refer to Table 6.13 for
contents
TOC-VCPH/CPN
305
6.6 Consumable Parts List
6.3.8 PC Hardware Requirements
Table 6.13 • Consumable Parts List 3 (TOC-VCPH/CPN)
Part No.
Description
Qty
Remark
TOC-
TOC-
VCPH
VCPN
638-41323
Combustion tube (in case)
2
2
638-60116
TOC regular catalyst
2
2
630-00996
TOC high sensitive catalyst
1
0
630-00557
Quartz wool
1
1
630-00999
CO2 absorber
1
1
630-00992
Halogen scrubber
2
2
036-11209-84
O-ring, 4D P 10A
1
1
5 pcs
036-11408-84
O-ring, Teflon P10
1
1
5 pcs
036-11219-84
O-ring, 4DP 20
1
1
5 pcs
630-00635-01
Potassium hydrogen
phthalate, 25g
1
1
630-00962-01
Sodium carbonate,25g
1
1
630-00963-01
Sodium bicarbonate, 25g
1
1
638-60074
Ceramic fiber
1
1
042-00405-11
IC reagent supply pump head 1
0
631-20265
8-port valve rotor
1
1
638-59213-01
Plunger tip
2
2
Table 6.14 • Consumable Parts List 4 (ASI-V)
Part Number
Part Name
Comment
038-00165-21
Vial set
40mL, 72 vials, septa and
caps
638-41462
Vial
24mL, 100pcs
038-00165-48
Septum
24mL, 100pcs.
038-00165-50
Septum
40mL, 100pcs.
638-20074-01
Cap
24mL, 100pcs.
038-00165-40
Cap
40mL, 200pcs.
042-00405-11
Rinse pump head
Table 6.15 • Consumable Parts List 5 (8-Port Sampler OCT-1)
Part Number
631-20265
306
TOC-VCPH/CPN
Part Name
8-Port valve rotor
Comment
6.3.8
6.6 Consumable Parts List
PC Hardware Requirements
Table 6.16 • Consumable Parts List 6 (TNM-1)
Part Number
Part Name
638-65232
Ozone treatment - catalyst
638-71162
Ozone treatment unit ASSY
631-43818
Reactor packing
631-40316
Viton joint, reactor outlet
036-19004-19
O-ring, Ozone treatment unit
017-40533-01
Potassium nitrate, 25 g
Comment
300g included
1pc.
Table 6.17 • Consumable Parts List 7 (Carrier Gas Purifier Kit)
Part Number
Part Name
638-42013
L-shaped combustion tube,
in case
630-00556
Soda lime
638-60116
TOC regular catalyst
Comment
Carrier gas purifier kit, 500g
included
TOC-VCPH/CPN
307
6.7 Maintenance Parts List
6.3.8 PC Hardware Requirements
6.7
Maintenance Parts List
Table 6.18 • Maintenance Parts List 1 (TOC-VCPH)
Part Number
Part Name
638-56135
8-port valve
638-59213
Syringe
638-41337-03
Flared tubing
631-41660
Flared tubing, for dilution
water
638-65383
Tandem cell (in case)
Comment
Table 6.19 • Maintenance Parts List 2 (TOC-VCPN)
Part Number
Part Name
638-56135
8-port valve
638-59213
Syringe
638-41337-03
Flared tubing
631-41660
Flared tubing, for dilution
water
638-65383
Tandem cell (in case)
Comment
Table 6.20 • Maintenance Parts List 3 (ASI-V)
Part Number
308
Part Name
Comment
638-41472-01
Needle, sampling
For 24mL and 40mL, 1pc.
638-41448-01
Needle, sparging
For 24mL and 40mL, 1pc.
638-41449-01
Needle, simultaneous sparge
type
For 24mL, 40mL, 1pc.
638-41450-01
Needle, suspended solids kit,
0.8mm
For 24mL, 40mL, 1pc.
638-42029-04
Tubing set (sampling)
1 sampling tube, with
retainer and tube seal
638-42029-05
Tubing set (sparge)
1 sparge tube, with retainer
and tube seal
638-42029-03
Tubing set (sampling +
sparge for simultaneous
sparge)
1 each of sampling and
sparge tube for simultaneous
sparging, with retainers and
tube seals
TOC-VCPH/CPN
6.3.8
6.7 Maintenance Parts List
PC Hardware Requirements
Table 6.21 • Maintenance Parts List 4 (OCT-1 8-Port Sampler)
Part Number
Part Name
Comment
631-20265
8-port valve rotor
Spare rotor
638-41337-03
Flared tubing C
Sampling tube; for
combustion type TOC-V
638-41443-03
Common tubing C
Main unit - OCT-1
connection tube; for
combustion TOC-V, 1 unit
638-41443-04
Common tubing C2
Main unit - OCT-1
connection tube; for
combustion TOC-V, add-on
Table 6.22 • Maintenance Parts List 5 (Manual Injection Kit)
Part Number
Part Name
Comment
630-00261
Open / Close valve, TC
injection port
638-60733-01
Microsyringe, MANU10
10µL
638-60733-02
Microsyringe, MANU25
25µL
638-60733-03
Microsyringe, MANU50
50µL
638-60733-04
Microsyringe, MANU100
100µL
638-60733-05
Microsyringe, MANU250
250µL
638-60733-06
Microsyringe, MANU500
500µL
TOC-VCPH/CPN
309
6.8 Installation
6.8.1 Before Installation
6.8
Installation
6.8.1 Before Installation
Parts Inspection
Confirm that all of the components listed in Section 6.4 "Standard Accessories" have been
included in the shipping package.
6.8.2 Installation Site
Be sure to take into account the size of the instrument, how it will be used, and the
installation conditions indicated below when selecting an installation site. Instrument
damage or measurement errors may occur based on the conditions of the installation site.
6.8.2.1 Installation Site Selection
The instrument is designed for use on a desk or bench.
TOC-V Main Unit
Autosampler
370mm
635mm
The external dimensions of the instrument are shown in Figure 6.3 "External Dimensions
of Instrument with ASI-V". A space of at least 200mm is required on either side of and
behind the instrument to enable unhindered operation and maintenance.
TOC-V Main Unit
100
mm
440mm
TN Unit
160mm
Figure 6.3 External Dimensions of Instrument with ASI-V
310
TOC-VCPH/CPN
6.8.2
6.8 Installation
Installation Site
Figure 6.4 External Dimensions of Instrument with OCT-1 8-Port Sampler
CAUTION
When lifting the instrument, lift from the bottom and at both sides of the
instrument.
Do not lift the instrument by the front access door, as this may cause damage.
6.8.2.2 Installation Site Conditions
Select an installation site with the following conditions:
• A clean environment free of corrosive gases, organic gases, and dusts.
Note: Contamination in the atmosphere will cause analysis errors, especially for high
sensitivity analyses.
• A strong, level bench, free of vibration and shock.
• A location with a stable ambient temperature.
• A location with access to a completely grounded, stable power supply.
CAUTION
Avoid locations where flames are prohibited. Some internal parts reach high
temperatures and could cause a fire hazard.
Avoid the following kinds of locations:
• Locations close to heat sources, windows in direct sunlight, or in direct contact with
drafts from air conditioning vents.
• Near equipment that generates intense magnetic fields, electrical fields, or high
frequency waves.
TOC-VCPH/CPN
311
6.8 Installation
6.8.3 Installation Procedure
6.8.3 Installation Procedure
6.8.3.1 Connecting Power Supply and Ground
¬Connecting Power Supply
Connect the instrument to a stable, AC 100-127V (100V System) or AC 220-240V (200V
System), 50Hz or 60Hz (single phase) power supply with sufficient capacity to
accommodate 6A or greater current.
CAUTION
The instrument may not operate properly if the power supply voltage exceeds
the range of AC100-127V ±10% or AC 220-240V ±10%. Unstable voltage may
cause problems during high sensitivity analysis.
Note:
The instrument is compatible with both 50 Hz and 60 Hz power supplies and can
be used with either frequency.
¬Grounding
The included power cord is a three-conductor cable including a ground wire, and a 2P plug
(with ground) at the end. If the power outlet does not have ground receptacle, use the
included 2P (no ground) adapter. Connect the external ground terminal to the ground.
The voltage terminals (AC) and ground terminal (ACC) on the power plug of this
instrument are arranged as shown in Figure 6.5 "Power Plug". Connect them so that they
match the power outlet being used.
Voltage terminal (AC)
Ground terminal (ACC)
Ground terminal (G)
(Be sure to ground completely.)
Figure 6.5 Power Plug
312
TOC-VCPH/CPN
6.8.3
6.8 Installation
Installation Procedure
CAUTION
•
In addition to the consideration of safety, complete grounding is necessary to
prevent as much as possible the occurrence of signal noise. A Type-3 ground
(ground resistance: 100W or less, see Electrical Facilities Engineering Standards
for details) is recommended.
•
Perform grounding separately and avoid contact with water supply pipes, gas
pipes, and lightning rods.
6.8.3.2 Changing the Power Supply Voltage
The instrument is set up before shipment to match the power supply voltage in the locale
where it will be used. In the event that it becomes necessary to change the power supply
voltage, please contact your Shimadzu representative. Depending on the voltage change,
an authorized Shimadzu service engineer may be required to rewire connections to the
terminal block to change the power supply voltage and/or perform changes to the main
board.
6.8.3.3 Connecting Gas
Use one of the following as the carrier gas supply for this instrument.
• Cylinders filled with high purity air
• Compressed air or instrumentation air (Requires special Carrier Gas Purifier Kit
accessory)
¬High Purity Air Cylinders
High purity air is synthetic air manufactured from pure nitrogen and pure oxygen. It must
be guaranteed to contain less than one 1ppm of each of the following impurities: carbon
dioxide, carbon monoxide, and hydrocarbons.
The cylinder must be equipped with a pressure regulator to supply it at 300kPa to the gas
connection inlet of the instrument.
Note:
If the carrier gas contains excessive impurities, analysis accuracy is diminished
and good results will not be obtained.
TOC-VCPH/CPN
313
6.8 Installation
6.8.3 Installation Procedure
Precautions for Handling Gas Cylinders
The handling and safety management of high-pressure gases is strictly regulated
by high-pressure gas control laws, general high-pressure gas safety codes, and
fire laws.
The gas used in the instrument is not dangerous, but mistakes in handling of
high-pressure gas cylinders can be extremely hazardous. Carefully read and
obey the following precautions.
• Place gas cylinders in a well-ventilated location out of direct sunlight.
• Ensure that gas cylinders never reach temperatures higher than 40°C.
• Make sure there are no open flames anywhere within 2 meters of a gas cylinder.
• Secure cylinders with bands or other fasteners to prevent tipping and falling.
• Turn OFF, immediately and completely, all valves on the cylinder, when finished
using gas.
• Inspect the operation of the pressure gauge at least once every three (3) months.
¬Compressed Air or Instrument Air Purified with the Carrier Gas Purification
Kit
Using the Carrier Gas Purification Kit enables air from a compressor or instrumentation air,
or high-impurity pressurized air in a cylinder, to be used as the carrier gas.
Since there are limits to the capabilities of the Carrier Gas Purification Kit, the following
conditions must be met when supplying compressed air.
• Provide an air filter in the supply line to remove dust, oil mist, water drops, and other
contaminants. Place an air filter in the tubing near the gas connection inlet of the
instrument when a compressor is used.
• Select the Oil-less Carrier Gas Purification Kit when a compressor is used.
• There are cases where the organic gas concentration is too high to be removed
completely by the gas purifier. Analysis accuracy is poor in atmospheres containing
high concentrations of volatile gases from exposed organic solvents and gasoline, or
high concentrations of automobile and diesel engine exhaust. If the possibility of the
presence of these kinds of gases cannot be avoided, use a filter to remove organic
particles and/or gases.
¬Gas Supply Pressure
Ensure that the gas supplied to the gas inlet of the instrument maintains a constant, stable
pressure of 300kPa. When using compressed air or instrumentation air, verify that the gas
supply pressure is greater than 300kPa and less than 600kPa.
Note:
Do not allow the carrier gas supply pressure to exceed 600kPa.
¬Gas Tubing Connections
The special accessory Air Supply Tubing Set includes nylon tubing and connectors (two [2]
half unions).
314
TOC-VCPH/CPN
6.8.3
6.8 Installation
Installation Procedure
Procedure
Connection Inlet
Half Union
Nylon Tubing
Figure 6.6 Gas Tubing Connection
1.
Connect the half unions to the carrier gas inlet on the instrument and the connection
outlet (¼” NPT) of the gas supply source.
2.
Connect the nylon tubing (4mm OD, 2.5mm ID) between the gas supply source and
the instrument.
Note: To connect the nylon tubing, firmly insert it into the half union. To
disconnect the tubing, pull the tubing off while pushing down
firmly on the blue ring of the half union with a screwdriver.
3.
Verify that there are no gas leaks.
CAUTION
•
Do not allow acute bends in the tubing.
•
Clean the tubing and connectors to remove any oils or other contaminants on
their inner surfaces.
•
Copper tubing or stainless steel tubing may also be used.
TOC-VCPH/CPN
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6.8 Installation
6.8.3 Installation Procedure
6.8.3.4 Connecting the Drain Tubing
Drain tubing is connected to provide for external discharge of measured samples and other
liquid waste. If a nearby drainage pit is not available, use a 10 to 20 liter polypropylene
container as the drain receptacle.
Figure 6.7 Connect the Drain Tubing
The drain tubing from the dehumidifier drain port is located inside the right panel. Connect
it to the external drain tubing using two of the provided wiring bands so that there are no
leaks.
CAUTION
• Drainage occurs on a gravity basis. Keep resistance to a minimum. Ensure that
the drain tubing is never higher than the drain discharge port. Do not allow the
tip of the drain tubing to come in contact with the surface of the liquid in the
container. If resistance is high, insufficient drainage could cause the drainage liquid to overflow inside the instrument.
• Corrosive substances such as acids may be present in the drainage liquid. Avoid
touching or spilling these liquids.
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TOC-VCPH/CPN
6.8.4
6.8 Installation
Installing the Autosampler
6.8.3.5 PC Cable Connections
This section describes the procedure for connecting the TOC-V to the PC using the
supplied RS-232C cable.
Procedure
1.
Insert the supplied RS-232C cable into the RS-232C-1 connector on the back of the
TOC-V, and tighten the retaining screws on both sides. Figure 2.4 "Rear View"
2.
Insert the plug at the other end of the RS-232C cable into the RS-232C connector of
the PC, and tighten the retaining screws on both sides.
6.8.4 Installing the Autosampler
This section describes procedures for installing the ASI-V autosampler.
¬Positioning the Autosampler
The autosampler is placed to the left of the TOC-V, as shown in Figure 6.8 "Installing the
Autosampler".
Figure 6.8 Installing the Autosampler
Note:
Keep the distance between the autosampler and main unit to a minimum to allow
a free range of motion of the autosampler. If the autosampler tubing becomes
stretched taut, it may impede the movement of the autosampler arm, resulting in
operation errors and damage.
¬Removing the Shipping Screw
The ASI arm is secured with a shipping screw to prevent damage during shipment. Before
connecting power to the instrument, remove the ASI cover to access the shipping screw,
which is located on the retaining bracket. Remove the shipping screw and replace the cover.
Label the shipping screw and store it for future use.
TOC-VCPH/CPN
317
6.8 Installation
6.8.4 Installing the Autosampler
CAUTION
To prevent instrument damage, verify that the ASI arm is firmly attached to the
retaining bracket with the shipping screw before shipping the instrument or
moving it to another location.
¬Connecting Cables
The TOC-V and ASI-V are connected using cables, as described below.
CAUTION
Verify that the TOC-V is switched OFF before performing the following
procedure.
Procedure
1.
Connect the ASI-V power cord at the rear of the ASI-V to the ASI-V power connector
at the rear of the TOC-V.
2.
Connect the provided signal cable to the ASI-V signal connectors at the rear of the
TOC-V and the ASI-V.
Figure 6.9 Connecting the Cables (TOC-V to ASI-V)
318
TOC-VCPH/CPN
6.8.4
6.8 Installation
Installing the Autosampler
¬Connecting the Sample Tubing and Sparge Tubing (External Sparge Kit)
The procedure for connecting the ASI-V sample tubing and sparge tubing for the External
Sparge Kit is as follows.
Procedure
1.
2.
3.
Open the TOC-Control V Sample Table Editor and connect the instrument.
4.
Remove the screw at the lower left side of the needle replacement window, and detach
the window cover by pulling downward.
5.
Install the tubing clamp.
From the Instrument menu, select Maintenance>ASI Needle Change.
Click the Preparation Start button.
The autosampler arm moves to the front of the needle replacement window, allowing
easy access.
Needle Replacement Window
Sample Catcher
Figure 6.10 Tubing Installation
6.
Install the bushing at the end of the sample tubing to the Number 2 port of the TOC-V
sample injector 8-port valve.
TOC-VCPH/CPN
319
6.8 Installation
6.8.4 Installing the Autosampler
7.
Draw the sparge tubing out through the joint and connect the sparge tubing.
Sparge Tubing
(External Sparge Kit)
External Sparge Unit
Advance Sparge
Needle
Sampling Needle
Sparge Tubing
Tubing Installation Label
(External Sparge Kit)
Sparge Tubing
(External Sparge Kit)
ASI-V Cover
Installation figure using the anvance
sparge needle and the sampling needle.
Figure 6.11 Installing the External Sparge Kit
Note:
Do not use the flow controller knob to turn off the sparge gas flow.
¬Installing the Needle
This section describes installation of the ASI-V needle. There are two types of needles, the
sample needle (same as the sparge needle) and the coaxial needle, which is a combined
sample/sparge needle.
When installing the needle, remove the needle replacement window cover. Refer to Figure
6.11 "Installing the External Sparge Kit", for the removal procedure.
320
TOC-VCPH/CPN
6.8.4
6.8 Installation
Installing the Autosampler
Installation Procedure for the Sample Needle and Sparge Needle
1.
2.
3.
Open the TOC-Control V Sample Table Editor and connect the instrument.
4.
5.
6.
Remove the screw, and then detach the needle holder from the arm.
From the Instrument menu, select Maintenance>ASI Needle Change.
Click the Preparation Start button.
The autosampler arm moves to the front of the needle replacement window, allowing
easy access.
Insert the needle into the opening in the needle holder.
Secure the needle by turning the retaining bracket and tightening the screw at the top
of the needle holder.
Note: There are two openings; the left opening is for the sample tubing
and the right opening is for the sparge tubing.
Retaining Bracket
Needle Holder
Sample Needle
Figure 6.12 Installing the Needle - 1
7.
Securely fit the sample tubing or sparge tubing onto the upper end of the needle.
Note: Verify that the bushing is in position to secure the sample tubing
onto the sample needle.
8.
Insert the lower tip of the needle into the needle guide opening, thrusting the needle
holder into the pin of the arm, and then tighten the screw.
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321
6.8 Installation
6.8.4 Installing the Autosampler
9.
Reinstall the needle replacement window cover, and tighten the screw.
Figure 6.13 Installing the Needle - 2
Installing the Coaxial Needle
1.
2.
3.
Open the TOC-Control V Sample Table Editor and connect the instrument.
4.
5.
6.
Detach the needle holder from the arm.
7.
8.
Install the provided 3-way joint on the top of the needle.
9.
Insert the tip of the needle into the needle guide opening, thrusting the needle holder
into the pin of the arm, and then tighten the screw.
From the Instrument menu, select Maintenance>ASI Needle Change.
Click the Preparation Start button.
The autosampler arm moves to the front of the needle replacement window, allowing
easy access.
Insert the needle into the opening in the needle holder.
Secure the needle by turning the retaining bracket, and tightening the screw at the top
of the needle holder.
Connect the sample tubing to the top of the 3-way joint, and the sparge tubing to the
side of the joint.
10. Reinstall the needle replacement window cover, and tighten the screw at the lower left
of the cover.
322
TOC-VCPH/CPN
6.8.4
6.8 Installation
Installing the Autosampler
¬Installing the Turntable, Vial Rack and Cover
Installing the Turntable
1.
Place the turntable on the ASI-V.
Note: There is no distinction between front and rear of the turntable, so
placement orientation is irrelevant.
2.
Place the turntable so that the 3 guides on the ASI-V pass through the 3 holes at the
center of the turntable.
Three Holes at
Center of Turntable
Turntable
Figure 6.14 Installing the Turntable
Installing the Vial Rack
1.
2.
Place the vial rack on top of the turntable.
Rotate the vial rack until the guides of the turntable fit into the vial rack. This secures
the vial rack in place.
Installing the Cover
1.
Place the cover on the ASI-V.
Note: There is a magnet at the left rear of the cover. Verify that the cover
and ASI-V are in contact at the magnet.
¬Install the Rinse Bottle and Drain Tank
Installation of the rinse bottle and drain tank is explained below.
Rinse and drain tubing are attached to the autosampler, and are respectively labeled
“RINSE” and “DRAIN.” Use the rinse water tubing as is, and cut the drain tubing to an
appropriate length.
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6.8 Installation
6.8.4 Installing the Autosampler
CAUTION
• Verify that the drain tubing remains lower than the drain port of the ASI-V, and
that the end of the drain tubing remains above the surface of the liquid in the
drain tank.
• Corrosive substances such as acids may be present in the drainage liquid. Avoid
touching or spilling these liquids.
Preparation
• The rinse bottle is provided as a standard accessory.
• The drain bottle is a special accessory (P/N 638-52344). A suitable substitute may be
used as the drain container.
Procedure
1.
2.
3.
Place the rinse bottle on the bench with the TOC-V and the autosampler.
Place the drain container on the floor.
To minimize resistance, keep the tip of the drain tubing above the surface of the drain
liquid and as close to the instrument as possible.
CAUTION
Do not allow any slack or bends in the tubing that could cause a buildup of water
pressure.
Before Starting Analysis
Check the following before starting analysis.
• The rinse water bottle is filled to above the 2 L mark.
• The tip of the rinse tubing reaches nearly to the bottom of the rinse water bottle.
CAUTION
Perform the checks described above to ensure that rinse water will be delivered
and air will not be taken into the TOC-V injection pump.
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TOC-VCPH/CPN
6.8.5
6.8 Installation
OCT-1 8-Port Sampler Installation
6.8.5 OCT-1 8-Port Sampler Installation
The OCT-1 8-port sampler is installed as described below.
6.8.5.1 Installation Procedure
This section describes the procedure for installing the OCT-1 8-Port Sampler.
The unit is set up to the left of the TOC-V main body as shown in Figure 6.15“Installation
of the 8-Port Sampler”.
TIP »
When 2 OCT-1 8-Port Samplers are to be used, place both units to the left of the TOC-V
main unit as shown in the overhead view of Figure 6.4“External Dimensions of Instrument
with OCT-1 8-Port Sampler”.
8-Port Sampler
TOC-V Main Unit
Figure 6.15 Installation of the 8-Port Sampler
Cable Connections
The cable is connected between the main unit of the TOC-V and the 8-Port Sampler.
CAUTION
Confirm that the power to the TOC-V main unit is switched OFF before
performing this procedure.
Connection Procedure
1.
2.
3.
Remove the 4 screws at the top of the 8-Port Sampler, and take off the cover.
4.
Pass the cable through the rear panel, and replace the cover of the 8-Port Sampler.
Connect the power and signal cable to the circuit board of the 8-Port Sampler.
Connect the ground wire of the power cable to the grounding terminal on the circuit
board of the OCT-1.
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325
6.8 Installation
6.8.5 OCT-1 8-Port Sampler Installation
Rear Panel
8-Port Sampler Signal Cable
8-Port Sampler Power Cable
Figure 6.16 Cable Connections (TOC-V and 8-Port Sampler)
5.
6.
Connect the power cable to the power receptacle on the back of the TOC-V.
Connect the signal cable to the 8-Port Sampler connection on the back of the TOC-V.
Installing Two 8-Port Sampler Units
When installing two 8-Port Sampler units, a signal cable (standard accessory) is connected
between 8-Port Sampler 1 and 8-Port Sampler 2.
Installation Procedure
1.
2.
Remove the covers from both 8-Port Sampler units.
Connect the signal cable exiting 8-Port Sampler 2 to the connector of 8-Port Sampler
1.
8-Port Sampler 2
Signal Cable
8-Port Sampler 1
Figure 1.17 Connecting Two 8-Port Samplers
326
TOC-VCPH/CPN
6.8.5
6.8 Installation
OCT-1 8-Port Sampler Installation
3.
Remove the port number label from the 8-Port Sampler 2 unit and replace it with the
port number label provided with the unit.
Note: The port that was originally labeled as port No. 1 should be labeled
as port No. 9.
4.
Replace the covers on the 8-Port Samplers.
Connecting the Sample Tubing
Use the following procedure to connect the sample tubing of the 8-Port Sampler.
Tubing Connection Procedure
1.
The sample tubing differs according to the TOC-V model that is used with the 8-Port
Sampler
Note: Refer to Table 6.21 •“Maintenance Parts List 4 (OCT-1 8-Port Sampler)” for the appropriate part numbers.
2.
Connect the fitting at one end of the tubing to the common (COM) port of the 8-Port
Sampler.
3.
Pass the sample tubing through the hole in the left side panel of the TOC-V main unit.
Connect the fitting at the other end of the sample tubing to port No. 2 of the 8-port
valve of the TOC-V sample injector. Connect to port No. 1 when installing 8-Port
Sampler 2.
4.
Connect the sample tubing to ports 1 - 8 (ports 9 - 16 for 8-Port Sampler 2) of the 8Port Sampler.
Sample Tubing
Figure 6.18 Tubing Connections
Note:
Connection to the TOC-V Main Unit
• 8-Port Sampler 1
Connect the COM tubing to the common (COM) port of 8-Port Sampler 1 and
port No. 2 on the TOC-V unit.
• 8-Port Sampler 2
Connect the COM tubing to the common (COM) port of 8-Port Sampler 2 and
port No. 1 on the TOC-V unit
TOC-VCPH/CPN
327
6.8 Installation
6.8.6 Installing the TN Unit
6.8.6 Installing the TN Unit
6.8.6.1 Connecting the Power and Installation
¬Connecting the Power Supply
Connect the TN unit to a stable, AC100V±10 V, 50Hz or 60Hz (single phase) power supply
with sufficient capacity to accommodate 2A or greater current. The symbol “~” on the
name plate indicates alternating current.
CAUTION
The instrument may not operate properly if the power supply voltage exceeds
the range of AC100-127V ±10% or AC 220-240V ±10%. Unstable voltage may
cause problems during high sensitivity analysis.
Note:
The instrument is compatible with both 50Hz and 60Hz power supplies and can
be used with either frequency.
¬Grounding
The included power cord is a three-conductor cable including a ground wire and a 2P plug
(with ground) at the end. If the power outlet does not have ground receptacle, use the
included 2P (no ground) adapter and ground the external ground tap terminal.
The voltage terminals (AC) and ground terminal (ACC) on the power plug of this
instrument are arranged as shown in Figure 6.19 "Power Plug". Connect them so that they
match the power outlet being used.
Voltage Terminal (AC)
Ground Terminal (ACC)
Ground Terminal (G)
(Be sure to ground completely.)
Figure 6.19 Power Plug
328
TOC-VCPH/CPN
6.8.6
6.8 Installation
Installing the TN Unit
CAUTION
•
In addition to the consideration of safety, complete grounding is necessary to
prevent as much as possible the occurrence of signal noise. A Type-3 ground
(ground resistance: 100W or less, see Electrical Facilities Engineering Standards
for details) is recommended.
•
Perform grounding separately and avoid contact with water supply pipes, gas
pipes, and lightning rods.
6.8.6.2 Connecting Ozone Source Air
The TNM-1 incorporates an internal ozone generator, requiring a source of air gas
(supplied at about 500mL/min) separate from the carrier gas supplied to the TOC-V. While
it is possible to use TOC-V high purity carrier gas by providing branch tubing, the
consumption of the combined-use carrier gas would increase to about 150 - 250mL/min.
Assuming operation at the rate of 8 hours/day, 5 days/week, the 47 L, 12MPa air cylinder
would require monthly replacement (as compared to every 3 months when used for carrier
gas alone).
Because air gas for ozone generation is not required to be the high purity air used as carrier
gas, it is recommended to use instrumentation air or compressor-supplied air for ozone
generation, separate from the carrier gas.
¬Using Compressor Air or Instrumentation Air
When using compressor air or instrumentation air for generation of ozone, be sure that the
following conditions are satisfied.
• Install an air filter in the air supply line to eliminate dust, oil mist and water droplets
from the air. If a compressor is used, install the air filter (equipped with drain separation
and discharge branch) close to the tubing connection at the instrument.
• If a compressor is used, select an oil-less type air compressor. The oil-less air compressor SLP-5D-2 SVF (P/N 638-59203-01) is available as an option.
¬Using a High Purity Air-Filled Cylinder (Via Branch Tubing from Carrier Gas)
High purity air is synthesized air using pure nitrogen and pure oxygen. Ensure that
contaminants, including carbon dioxide, carbon monoxide and total hydrocarbons, are
guaranteed not to exceed 1ppm each.
Install a pressure regulator on the gas cylinder and supply gas to the instrument so that the
pressure is 300kPa at the instrument gas connection port.
Note:
If there are excessive contaminants in the carrier gas, measurement results will be
adversely affected due to low measurement reproducibility, etc.
TOC-VCPH/CPN
329
6.8 Installation
6.8.6 Installing the TN Unit
Precautions in Handling Gas Cylinders
The handling and safety management of high-pressure gases is strictly regulated
by high-pressure gas control laws, general high-pressure gas safety codes, and
fire laws.
The gas used in this instrument itself is not dangerous, but mistakes in the
handling of high-pressure gas cylinders can be extremely hazardous. Carefully
read and obey the following precautions.
• Place gas cylinders in a well-ventilated location out of direct sunlight.
• Ensure that gas cylinders never reach temperatures higher than 40°C.
• Make sure there are no open flames anywhere within 2 meters of a gas cylinder.
• Secure cylinders with bands or other fasteners to prevent tipping and falling.
• When finished using gas, immediately and completely turn OFF all valves on the
cylinder.
• Inspect the operation of the pressure gauge at least once every three (3) months.
¬Gas Supply Pressure
Supply gas at a constant, stable pressure of 300kPa (44PSI)at the gas inlet connection of the
TNM-1.
Note:
Keep the carrier gas supply pressure to the instrument from exceeding 600kPa
(87PSI).
¬Gas Tubing Connections
The special accessory Air Supply Tubing Set includes nylon tubing and connectors (two (2)
half unions).
Connection Inlet
Half Union
Nylon Tubing
Figure 6.20 Gas Tubing Connection
330
TOC-VCPH/CPN
6.8.6
6.8 Installation
Installing the TN Unit
Procedure
1.
Connect the half unions to the carrier gas inlet on the instrument and the connection
outlet (¼” NPT) of the gas supply source.
2.
Connect the nylon tubing (4mm O.D., 2.5mm I.D.) between the gas supply source and
the instrument.
Note:
3.
The nylon tubing can be connected simply by firmly inserting it
into the half union. When disconnecting the tubing, pull off the tubing while pushing down firmly on the green-colored ring of the half
union using a screwdriver.
After connection, check to see that there are no gas leaks.
CAUTION
•
Do not allow any acute bends in the tubing.
•
When tubing and connectors are prepared by the user, be sure to use clean
components that are free of oils or other contaminants on their inner surfaces.
•
Copper tubing or stainless steel tubing may also be used.
¬Low Ozone Air Supply Pressure Safety Mechanism
To ensure safety, the TN unit is equipped with an ozone air gas pressure sensor that will
automatically cause the ozone generator to be switched off when the ozone air gas pressure
decreases below 50kPa.
If this occurs, the red lamp labeled “PRESS” at the lower right of the TNM front panel will
illuminate. Take the appropriate measures to correct the low pressure problem.
TOC-VCPH/CPN
331
6.8 Installation
6.8.6 Installing the TN Unit
6.8.6.3 Connecting Gas Exhaust Tubing
Because the unit uses a chemiluminescence system for the detection of TN components, it
is equipped with an internal ozone generator. The ozone and NOx generated are removed
by the ozone treatment unit and NOx absorber, and are then exhausted. However, in the
event that the performance of the ozone treatment catalyst and NOx absorber deteriorate,
ozone and NOx gas may be expelled in the exhaust gas. Be sure to discharge exhaust gas to
the outdoors or to an exhaust pit using a 5mm I.D. flexible vinyl hose.
CAUTION
• To minimize resistance, leave the gas exhaust tubing open to the atmosphere.
• Be sure to connect the gas exhaust tubing to the instrument and discharge the
exhaust gas to the outdoors or an exhaust pit.
• If the gas exhaust tubing is not connected, ozone and NOx gas may be exhausted
from the instrument, causing harm to the respiratory organs of individuals in the
vicinity.
332
TOC-VCPH/CPN
6.9 Material Safety Data Sheets
6.9.1 Hydrochloric Acid (HCl)
6.9
Material Safety Data Sheets
6.9.1 Hydrochloric Acid (HCl)
957006
Shimadzu Scientific Instruments, Inc.
7102 Riverwood Drive Columbia, MD 21046
Tel: 1(800) 477-1227
Control No.
November, 1995
MATERIAL SAFETY DATA SHEET
SECTION I
CAT. NO.:
630-00998-00
NAME:
Hydrochloric Acid
PRODUCT USE:
PRODUCT IDENTIFICATION
CAS NO.:
Hydrochloric Acid -7647-01-0
OTHER NAME: Muriatic Acid; Regeneration Liquid
This product is for specific use in the regeneration of the catalysts of the Shimadzu TOC. Refer to the Instruction Manual of the
unit for proper use.
SECTION II
PRECAUTIONS TO BE TAKEN IN HANDLING
Do not get in eyes, on skin or on clothing. Wear rubber or neoprene gloves and impervious boots, apron or coveralls, as needed, to prevent skin contact. Avoid
breathing mist. Use only with adequate ventilation; local and/or general exhaust is recommended to keep employee exposure below the Airborne Exposure Limits.
If TLV is exceeded, a full face piece chemical cartridge respirator may be worn, in general, up to 100 times the TLV or the maximum use concentration specified
by the respirator supplier, whichever is less. Store in tightly closed containers, in cool, dry, ventilated area. Protect from physical damage and direct sunlight. Isolate from incompatible substances. Protect from moisture. Remove and wash contaminated clothing promptly. Wash hands thoroughly after handling. This substance is classified as a POISON under the Federal Caustic Poison Act.
SECTION III
PHYSICAL DATA
Melt
Boil Point Density
Vapor
Vapor
Point
N/A
N/A
N/A
SECTION IV
Evaporation
Pressure
Density
Rate
N/A
N/A
N/A
Odor
Color
Phase
Water Solubility
Pungent
Colorless / Clear
Fuming
Liquid
Infinite / slight
evolution / heat
REACTIVITY DATA
Stable under ordinary conditions of use and storage. Containers may burst when heated. When heated to decomposition, emits toxic hydrogen chloride fumes and
will react with water or steam to produce heat and toxic and corrosive fumes. Hazardous Polymerization will not occur. Incompatibilities: A strong mineral acid;
concentrated hydrochloric acid is highly reactive with strong bases, metals, metal oxides, hydroxides, amines, carbonates and other alkaline materials. Incompatible with materials such as cyanides, sulfides, sulfites and formaldehyde.
SECTION V
FIRE:
EXPLOSION:
EXTINGUISHING MEDIA:
SECTION VI
RAT/MOUSE LD50
FIRE AND EXPLOSION HAZARD DATA
Can react with metals to release flammable hydrogen gas.
Not considered to be an explosion hazard.
If involved in a fire, use water spray. Special firefighting procedures: Use full protective clothing and NIOSH-approved selfcontained breathing apparatus with full face piece operated in the pressure demand or other positive pressure mode.
TOXICITY DATA
RTECS#
OSHA PEL
900mg/kg(hydrocloric acid concentrated)
SECTION VII
N/A
5ppm (TWA) Ceiling
ACGIH TLV-TWA
5ppm (TWA) Ceiling
HEALTH HAZARD DATA
Symptoms of overexposure: Inhalation: corrosive; can cause coughing, choking, inflammation of the nose, throat and upper respiratory tract. Inhalation of higher
concentrations may cause lung damage. Ingestion: corrosive; swallowing product can cause immediate pain and burns of the mouth, throat, esophagus and gastrointestinal tract; may cause nausea, vomiting and diarrhea. Contact with skin: corrosive; can cause redness, pain, and severe skin burns; deep ulcers and discolored skin; severe burns and eye damage. Chronic exposure: long-term exposure to concentrated vapors may cause erosion of teeth; long-term exposure seldom
occurs due to the corrosive properties of the acid. Persons with preexisting skin disorders or eye disease may be more susceptible to the effects of this substance.
SECTION VIII
FIRST AID
An antidote is a substance intended to counteract the effect of a poison. It should be administered only by a physician or trained emergency personnel. Medical
advice can be obtained from a POISON CONTROL CENTER.
In case of contact: Immediately flush eyes or skin with copious amounts of water for at least 15 minutes while removing contaminated clothing and shoes. Assure
adequate flushing of the eyes by separating eyelids with fingers. If inhaled, remove to fresh air. If not breathing, give artificial respiration. If breathing is difficult,
give oxygen. If swallowed, wash out mouth with water provided person is conscious. CALL A PHYSICIAN. DO NOT INDUCE VOMITING. If conscious, give
large quantities of milk or water. Never give anything by mouth to an unconscious or convulsing person. Get medical attention immediately.
SECTION IX
SPILL OR LEAK PROCEDURES
Cleanup personnel should wear protective clothing and respiratory equipment suitable for toxic or corrosive fluids or vapors. Isolate or enclose the area of the leak
or spill. Small spills: Flush with water and neutralize with alkaline material (soda ash, lime, etc.). Sewer neutralized material with excess water. Larger spills and
lot sizes: Neutralize with alkaline material, pick up with absorbent material (sand, earth, vermiculite). Provide forced ventilation to dissipate fumes. For disposal,
neutralize with alkaline materials (soda ash, lime, etc.). Dispose in a RCRA-approved waste facility or sewer the neutralized slurry with excess water if local ordinances allow. Reportable quantity (RQ) (CWA/CERCLA): 5000 labs. Ensure compliance with federal, state and local regulations.
SECTION X
SPECIAL PRECAUTIONS AND COMMENTS
The above information is believed to be correct but does not purport to be all inclusive and shall be used only as a guide. SHIMADZU shall not be held liable for
any damage resulting from handling or from contact with the above product. Users should make their own investigations to determine the suitability of the information for their particular purposes.
TOC-VCPH/CPN
333
6.9 Material Safety Data Sheets
6.9.2 Phosphoric Acid
6.9.2 Phosphoric Acid
957006
Shimadzu Scientific Instruments, Inc.
7102 Riverwood Drive Columbia, MD 21046
Tel: 1(800) 477-1227
MATERIAL SAFETY DATA SHEET
SECTION I
CAT NO.:
630-00710-00
NAME:
Phosphoric Acid 25% Ultrapure
SECTION II
PRODUCT IDENTIFICATION
CAS NO.:
SYNONYM:
Control No.
November, 1995
07664-38-2
Phosphoric Acid, IC Reaction Liquid
PRDUCT USE
This product is specifically for use in the IC channel of the TOC 500, TOC 5000, and TOC 4000 series of TOC analyzers. Refer to the appropriate instruction manual for directions on proper use. Keep tightly sealed in a cool, dry, well ventilated place. Store separate form flammable and combustible materials. Wear appropriate protective clothing and eye protection.
SECTION III
PHYSICAL DATA
Melt Point Boil Point Density Vapor Pressure
Color
N/A
N/A
N/A
SECTION IV
N/A
Phase Water Solubility
Colorless / Clear Liquid Completly Soluble
HAZARDS IDENTIFICATION
Corrosive, causes burns. Harmful if swallowed. Target organ(s): liver, blood. In case of contact with eyes, rinse immediately with plenty of water and seek medical
advice. Take off immediately all contaminated clothing. Wear suitable protective clothing, gloves and eye/face protection.
SECTION V
UNR-MAN LDLO:220mg/kg
TOXICITY DATA
ORL-RAT LD50:1530mg/kg
IHL-RAT LC50: >850mg/m3/1h
SECTION VI
Acute Effects:
Chronic Effects:
SECTION VII
SKN-RBT LD50:2740mg/kg
HEALTH HAZARD DATA
Harmful if swallowed. May be harmful if inhaled. May be harmful if absorbed through the skin. Material is extremely
destructive to tissue of the mucous membranes and upper respiratory tract, eyes and skin. Inhalation may result in spasm,
inflammation and edema of the larynx and bronchi, chemical pneumonitis and pulmonary edema. Symptoms of exposure may
include burning sensation, coughing, wheezing, laryngitis, shortness of breath, headache, nausea and vomiting. May cause
cyanosis.
Target organ(s): liver, blood, bone marrow. To the best of our knowledge, the chemical, physical, and toxicological properties
have not been thoroughly investigated.
FIRST-AID MEASURES
In case of contact, immediately flush eyes or skin with copious amounts of water for at least 15 minutes while removing contaminated clothing and shoes. Assure
adequate flushing of the eyes by separating the eyelids with fingers. If inhaled, remove to fresh air. If not breathing give artificial respiration. If breathing is difficult, give oxygen. If swallowed, wash out mouth with water provided person is conscious. Call a physician. Wash contaminated clothing before reuse. Discard contaminated shoes.
SECTION VIII
EXTINGUISHING MEDIA:
FIRE FIGHTING MEASURES
Carbon dioxide, dry chemical powder or appropriate foam.
SPECIAL FIREFIGHTING PROCEDURES:
Wear self-contained breathing apparatus and protective clothing to prevent contact
with skin and eyes.
UNUSUAL FIRE AND EXPLOSIONS HAZARDS:
Emits toxic fumes under fire conditions.
SECTION IX
ACCIDENTAL RELEASE MEASURES
Evacuate area. Wear self-contained breathing apparatus, rubber boots and heavy rubber gloves. Cover with dry lime or soda ash, pick up, keep in a closed container
and hold for waste disposal. Ventilate area and wash spill site after material pickup is complete.
SECTION X
INCOMPATIBILITIES:
STABILITY AND REACTIVITY
Strong bases, finely powdered metals
HAZARDOUS COMBUSTION OR DECOMPOSITION PRODUCTS:
SECTION XI
Thermal decomposition may produce toxic fumes of phosphorus
oxides and/or phosphine.
SPECIAL PRECAUTIONS AND COMMENTS
The above information is believed to be correct but does not purport to be all inclusive. It shall serve only as a guide. Shimadzu shall not be held liable for any
damage resulting from handling or contact with the above product. Users should make their own determinations regarding the suitability of this information for
their particular purposes.
334
TOC-VCPH/CPN
6.9 Material Safety Data Sheets
CO2 Absorber, CA(OH)2, KOH, NAOH: soda lime
6.9.3
6.9.3 CO2 Absorber, CA(OH)2, KOH, NAOH: soda lime
957003
Shimadzu Scientific Instruments, Inc.
7102 Riverwood Drive Columbia, MD 21046
Tel: 1(800) 477-1227
Control No.
November, 1995
MATERIAL SAFETY DATA SHEET
SECTION I
CAT. NO.
630-00556-00
NAME:
Soda Lime
PRODUCT USE:
PRODUCT IDENTIFICATION
CAS NO.
80006-28-8
OTHER NAME: Soda Lime; Soda and Lime
CO2 Scrubber in Shimadzu TOC Analyzers
SECTION II
PRECAUTIONS TO BE TAKEN IN HANDLING
Protect skin, eyes and clothing. Avoid prolonged or repeated exposure. Wash thoroughly after handling. Safety shower and eye bath. Use 8" minimum face shield.
Store as a corrosive. Keep tightly closed and store in a cool, dry, place. Air and moisture sensitive. Use as directed in the TOC-4000 Instruction Manual.
SECTION III
Melt
Boil
Point
Point
N/A
N/A
PHYSICAL DATA
Density Vapor Pressure Vapor Density
Evaporation
Odor Color
Phase
Rate
N/A
N/A
SECTION IV
N/A
N/A
Water
Solubility
N/A
White
Granules, various sizes
N/A
REACTIVITY DATA
Incompatible with strong acids. Absorbs CO2, moisture inactivates.
SECTION V
FIRE AND EXPLOSION HAZARD DATA
EXTINGUISHING MEDIA:
UNUSUAL FIRE HAZARD:
Dry chemical fire extinguisher. Wear self-contained breathing apparatus and protective clothing to prevent skin and eye
exposure.
Emits toxic fumes in a fire.
SECTION VI
TOXICITY DATA
RAT/MOUSE LD50 RTECS# OSHA PEL ACGIH TLV-TWA
N/A
SECTION VII
VX965000
N/A
N/A
HEALTH HAZARD DATA
Acute effects: Harmful if swallowed, inhaled, or absorbed through skin. Material is extremely destructive to tissue of the mucous membranes and upper respiratory
tract, eyes and skin. Inhalation may be fatal as a result of spasm, inflammation and edema of the larynx and bronchi, chemical pneumonitis and pulmonary edema.
Symptoms of exposure may include burning sensation, coughing, wheezing, laryngitis, shortness of breath, headache, nausea and vomiting. To the best of our
knowledge, the chemical, physical, and toxicological properties have not been thoroughly investigated.
SECTION VIII
FIRST AID
An antidote is a substance intended to counteract the effect of a poison. It should be administered only by a physician or trained emergency personnel. Medical
advice can be obtained from a POISON CONTROL CENTER.
In case of contact: Immediately flush eyes or skin with copious amounts of water for at least 15 minutes while removing contaminated clothing and shoes. Assure
adequate flushing of the eyes by separating eyelids with fingers. If inhaled, remove to fresh air. If not breathing, give artificial respiration. If breathing is difficult,
give oxygen. If swallowed, wash out mouth with water provided person is conscious. CALL A PHYSICIAN. Wash contaminated clothing before reuse. Discard
contaminated shoes. For complete information, see actual entry in RTECS #VX965000.
SECTION IX
SPILL OR LEAK PROCEDURES
Occupational spill: Evacuate area. Wear self-contained breathing apparatus, rubber boots and heavy rubber gloves. Absorb on sand or vermiculite and place in
closed containers for disposal. Ventilate area and wash spill site after material pickup is complete.
SECTION X
SPECIAL PRECAUTIONS AND COMMENTS
The above information is believed to be correct but does not purport to be all inclusive and shall be used only as a guide. SHIMADZU shall not be held liable for
any damage resulting from handling or from contact with the above product. Users should make their own investigations to determine the suitability of the information for their particular purposes.
TOC-VCPH/CPN
335
6.9 Material Safety Data Sheets
6.9.4 Lithium Hydroxide (monohydrate)
6.9.4 Lithium Hydroxide (monohydrate)
957002
Shimadzu Scientific Instruments, Inc.
7102 Riverwood Drive Columbia, MD 21046
Tel: 1(800) 477-1227
Control No.
November, 1995
MATERIAL SAFETY DATA SHEET
SECTION I
CAT. NO.
630-00961-00
NAME:
PRODUCT IDENTIFICATION
CAS NO.
1310-66-3
Lithium Hydroxide Anhydride, 99.95%OTHER NAME: Lithium Hydroxide Hydrate, Lithium Hydroxide Anhydride
(DOT,N2680(DOT)
TRADE NAME:
PRODUCT USE:
IC Absorbent
This product is for specific use with TOC instruments.
SECTION II
PRECAUTIONS TO BE TAKEN IN HANDLING
Wear appropriate NIOSH/MSHA-approved respirator, chemical-resistant gloves, safety goggles, other protective clothing. Safety shower and eye bath. Use only in
a chemical fume hood. Face shield, 8-inch minimum. Do not breathe dust. Do not get in eyes, on skin, or on clothing. Avoid prolonged or repeated exposure. Wash
thoroughly after handling. Corrosive, harmful solid. Keep tightly closed. Hygroscopic. Store under nitrogen, in a cool, dry, place.
SECTION III
PHYSICAL DATA
Melt
Boil
Point
Point
N/A
N/A
Density
1.510
SECTION IV
Vapor
Vapor
Evaporation
Pressure
Density
Rate
N/A
N/A
N/A
Odor
Color
Phase
Water
Solubility
N/A
White
Crystals
N/A
REACTIVITY DATA
Substance is strongly alkali. In contact with or mixed with acid, reaction is extremely strong. Aluminum and zinc are corroded by this substance and not suitable as
containers. Corrosive effect is enhanced in presence of humidity or water. Absorbs CO2 from air. Containers made of steel, stainless steel, glass, ceramic and many
synthetic compounds are relatively durable. Nature of decomposition products not known.
SECTION V
FIRE AND EXPLOSION HAZARD DATA
FIRE:
EXPLOSION:
EXTINGUISHING MEDIA:
SECTION VI
This substance is nonflammable. Use water mist, powdered extinguishing reagents, foam or carbon dioxide gas. Cool container
using water mist, and move container to safe location.
Not considered to be an explosion hazard.
Carbon dioxide, dry chemical powder, alcohol or polymer foam. Special Firefighting Procedures: Use full protective clothing
and NIOSH-approved self-contained breathing apparatus with full face piece operated in the pressure demand or other positive
pressure mode.
TOXICITY DATA
RAT/MOUSE LD50
RTECS#
N/A
0j6307080 Lithium hydroxide, Monohydrate
OSHA PEL ACGIH TLV-TWA
N/A
N/A
REVIEWS, STANDARDS, AND REGULATIONS: NOES 1983, HZD X6293000; TNF 60; NIS 6239; NOS 54; TNE 59941; TFE 6243
SECTION VII
HEALTH HAZARD DATA
Acute Effects: Harmful if swallowed, inhaled or absorbed through skin. Material is extremely destructive to tissue of the mucous membranes and upper respiratory
tract, eyes and skin. Inhalation may be fatal as a result of spasm, inflammation and edema of the larynx and bronchi, chemical pneumonitis and pulmonary edema.
Symptoms of exposure may include burning sensation, coughing, wheezing, laryngitis, shortness of breath, headache, nausea and vomiting. Uncontrolled movement, muscle spasms, and loss of consciousness may occur. To the best of our knowledge, the chemical, physical and toxicological properties have not been thoroughly investigated.
SECTION VIII
FIRST AID
An antidote is a substance intended to counteract the effect of a poison. It should be administered only by a physician or trained emergency personnel. Medical
advice can be obtained from a POISON CONTROL CENTER. In case of contact: Immediately flush eyes or skin with copious amounts of water for at least 15
minutes while removing contaminated clothing and shoes. Assure adequate flushing of the eyes by separating the eyelids with fingers. If inhaled, remove to fresh
air. If not breathing, give artificial respiration. If breathing is difficult, give oxygen. If swallowed, wash out mouth with water, provided person is conscious. CALL
A PHYSICIAN. Wash contaminated clothing before reuse, discard contaminated shoes. Additional information: Large doses of lithium ion have caused dizziness
and prostration, and can cause damage if sodium intake is limited. Dehydration, weight loss, dermatological effects and thyroid disturbances have been reported.
Central nervous system effects that include slurred speech, blurred vision, sensory loss, ataxia and convulsions may occur. Diarrhea, vomiting and neuromuscular
effects such as tremor, clonus and hyperactive reflexes may occur as a result of repeated exposure to lithium ion.
SECTION IX
SPILL OR LEAK PROCEDURES
Occupational Spill: Evacuate area. Wear protective footwear. Sweep up and place in a bag and hold for waste disposal. Waste Disposal Method: For small quantities, cautiously add to a large stirred excess of water. Adjust the pH to neutral, separate any insoluble solids or liquids and package them for hazardous-waste disposal. Flush the aqueous solution down the drain with plenty of water. The hydrolysis and neutralization reactions may generate heat and fumes which can be
controlled by the rate of addition. Observe all federal, state and local environmental regulations. Water Contamination: Harmful to marine life. Change in pH will
result in alkaline damage to marine life.
SECTION X
SPECIAL PRECAUTIONS AND COMMENTS
The above information is believed to be correct but does not purport to be all inclusive and shall be used only as a guide. SHIMADZU shall not be held liable for
any damage resulting from handling or from contact with the above product. Users should make their own investigations to determine the suitability of the information for their particular purposes.
336
TOC-VCPH/CPN
6.9
Material Safety Data Sheets
6.9.5 Halogen Scrubber
6.9.5 Halogen Scrubber
Shimadzu Scientific Instruments, Inc.
7102 Riverwood Drive Columbia, MD 21046
Tel: 1(800) 477-1227
Control No.
Date:
MATERIAL SAFETY DATA SHEET
SECTION I
CAT. NO.
630-0092-00
NAME:
Halogen Scrubber
PRODUCT USE:
PRODUCT IDENTIFICATION
CAS NO.
07740-50-8
OTHER NAME: Copper Wool
This product is for specific use with TOC instruments.
SECTION II
PRODUCT USE
For use specifically with the Shimadzu TOC 500, TOC 5,000, and TOC 4,000 instruments. Consult the appropriate instrument manual for proper use.
SECTION III
PHYSICAL DATA
Melt
Boil
Point
Point
1083°C
2595°C
Density
SECTION IV
N/A
Vapor
Vapor
Evaporation
Pressure
Density
Rate
N/A
N/A
N/A
Odor
Color
Phase
Water
Solubility
N/A
Reddish
Solid Malleable
Metal
N/A
HAZARDS IDENTIFICATION
Dust, mist or fumes may cause eye and skin irritation. Avoid contact.
SECTION V
RAT/MOUSE LD50
N/A
SECTION VI
TOXICITY DATA
RTECS#
OSHA PEL ACGIH TLV-TWA
GL5325000
N/A
N/A
HEALTH HAZARD DATA
Exposure to large amounts can cause gastrointestinal disturbances, nausea, vomiting, headaches, or dizziness.
SECTION VII
FIRST-AID MEASURES
In case of contact, immediately flush eyes with copious amounts of water for at least 15 minutes. in case of skin contact, immediately wash skin with soap and
copious amounts of water. if ingested and subject is conscious, immediately give large amounts of water. get medical attention.
SECTION VIII
EXTINGUISHING MEDIA:
SECTION IX
FIRE FIGHTING MEASURES
Appropriate to surrounding fire. Possible formation of toxic copper fumes. Use appropriate respiratory support.
ACCIDENTAL RELEASE MEASURES
N/A
SECTION X
INCOMPATIBILITIES:
SECTION XI
STABILITY AND REACTIVITY
Strong acids, active halogens such as chlorine, fluorine, iodine, and bromine. ammonia.
SPECIAL PRECAUTIONS AND COMMENTS
The above information is believed to be correct but does not purport to be all inclusive. It shall serve only as a guide. Shimadzu shall not be held liable for any
damage resulting from handling or contact with the above product. Users should make their own determinations regarding the suitability of this information for
their particular purposes.
TOC-VCPH/CPN
337
6.9 Material Safety Data Sheets
6.9.6 Quartz Wool
6.9.6 Quartz Wool
Shimadzu Scientific Instruments, Inc.
7102 Riverwood Drive Columbia, MD 21046
Tel: 1(800) 477-1227
Control No.
Date:
MATERIAL SAFETY DATA SHEET
SECTION I
CAT. NO.
630-0557-00
NAME:
Quartz Wool
SECTION II
PRODUCT IDENTIFICATION
CAS NO.
14808-60-7
OTHER NAME: N/A
PRODUCT USE
Support for catalyst in reaction tubes of TOC instruments. consult instrument manuals for proper use.
SECTION III
PHYSICAL DATA
Melt
Boil
Point
Point
N/A
N/A
Density
N/A
SECTION IV
Vapor
Vapor
Evaporation
Pressure
Density
Rate
N/A
N/A
N/A
Odor
Color
Phase
Water
Solubility
N/A
Grey
Fibrous
N/A
HAZARDS IDENTIFICATION
Possible eye and skin irritation. Avoid contact.
SECTION V
TOXICITY DATA
INERT
SECTION VI
HEALTH HAZARD DATA
INERT
SECTION VII
FIRST-AID MEASURES
In case of contact, immediately flush eyes with copious amounts of water for at least 15 minutes. In case of skin contact, immediately wash skin with soap and
copious amounts of water.
SECTION VIII
FIRE FIGHTING MEASURES
N/A
SECTION IX
ACCIDENTAL RELEASE MEASURES
N/A
SECTION X
STABILITY AND REACTIVITY
N/A
SECTION XI
SPECIAL PRECAUTIONS AND COMMENTS
The above information is believed to be correct but does not purport to be all inclusive. It shall serve only as a guide. Shimadzu shall not be held liable for any
damage resulting from handling or contact with the above product. Users should make their own determinations regarding the suitability of this information for
their particular purposes.
338
TOC-VCPH/CPN
6.9 Material Safety Data Sheets
6.9.7 High Sensitivity Catalyst
6.9.7 High Sensitivity Catalyst
Shimadzu Scientific Instruments, Inc.
7102 Riverwood Drive Columbia, MD 21046
Tel: 1(800) 477-1227
Control No.
Date:
MATERIAL SAFETY DATA SHEET
SECTION I
CAT. NO.
630-00996-00
NAME:
High Sensitivity TC Catalyst
SECTION II
PRODUCT IDENTIFICATION
CAS NO.
N/A
OTHER NAME: Platinum on Quartz Wool
PRDUCT USE
This product is specifically for use as a catalyst in the TOC 500,TOC 5000, and TOC 4000 series of TOC analyzers. Refer to the appropriate instruction manual for
directions on proper use.
SECTION III
PHYSICAL DATA
Melt
Boil
Point
Point
N/A
N/A
Density
SECTION IV
FLAMMABLE:
SECTION V
ACUTE EFFECTS:
EXPOSURE CAN CAUSE:
SECTION VI
N/A
Vapor
Vapor
Evaporation
Pressure
Density
Rate
N/A
N/A
N/A
Odor
Color
Phase
Water
Solubility
N/A
Grey
Fibrous Solid
N/A
HAZARDS IDENTIFICATION
Possible sensitizer. Keep away from sources of ignition - NO SMOKING. Take precautionary measures against static
discharges. Keep container tightly closed and in a well-ventilated place.
TOXICITY DATA
May be harmful by inhalation or ingestion. May cause eye irritation. May cause skin irritation. Material may be irritating to
mucous membranes and upper respiratory tract. Prolonged or repeated exposure may cause allergic reactions in certain
sensitive individuals.
Coughing, chest pains, difficulty in breathing. To the best of our knowledge, the chemical, physical, and toxicological
properties have not been thoroughly investigated.
HEALTH HAZARD DATA
SEE SECTION 5.
SECTION VII
FIRST-AID MEASURES
In case of contact, immediately flush eyes or skin with copious amounts of water for at least 15 minutes while removing contaminated clothing and shoes. IF
inhaled, remove to fresh air. If not breathing give artificial respiration. If breathing is difficult, give oxygen. If swallowed, wash out mouth with water provided
person is conscious. Call a physician. Remove and wash contaminated clothing promptly.
SECTION VIII
EXTINGUISHING MEDIA:
SECTION IX
FIRE FIGHTING MEASURES
CARBON dioxide, dry chemical powder or appropriate foam.
ACCIDENTAL RELEASE MEASURES
Shut off all sources of ignition. Wear self-contained breathing apparatus, rubber boots and heavy rubber gloves.
Sweep up, place in a bag and hold for waste disposal. Ventilate area and wash spill site after material pickup is complete.
SECTION X
STABILITY AND REACTIVITY
INCOMPATIBILITIES:
Strong oxidizing agents, organic materials.
HAZARDOUS COMBUSTION OR DECOMPOSITION PRODUCTS:Nature of decomposition products not known. Hazardous polymerization will not occur.
SECTION XI
SPECIAL PRECAUTIONS AND COMMENTS
The above information is believed to be correct but does not purport to be all inclusive. It shall serve only as a guide. Shimadzu shall not be held liable for any
damage resulting from handling or contact with the above product. Users should make their own determinations regarding the suitability of this information for
their particular purposes.
TOC-VCPH/CPN
339
6.9 Material Safety Data Sheets
6.9.8 Normal Sensitivity Catalyst
6.9.8 Normal Sensitivity Catalyst
Shimadzu Scientific Instruments, Inc.
7102 Riverwood Drive Columbia, MD 21046
Tel: 1(800) 477-1227
Control No.
Date:
MATERIAL SAFETY DATA SHEET
SECTION I
CAT. NO.
PRODUCT IDENTIFICATION
017-42801-00 and 017-42801-01
CAS NO.
NAME:
Regular Sensitivity Catalyst
SECTION II
7440-06-4(Platinum) and 1344-28-1(Alumina)
OTHER NAME: Platinum on 1/8" Alumina Pellets
PRDUCT USE
This product is specifically for use as a catalyst in the TOC 500,TOC 5000, and TOC 4000 series of TOC analyzers. Refer to the appropriate instruction manual for
directions on proper use.
SECTION III
PHYSICAL DATA
Melt
Boil
Point
Point
N/A
N/A
Density
N/A
SECTION IV
FLAMMABLE:
TARGET ORGAN(S):
SECTION V
ACUTE EFFECTS:
EXPOSURE CAN CAUSE:
CHRONIC EFFECTS:
TARGET ORGAN DATA:
SECTION VI
OSHA PEL:
SECTION VII
Vapor
Vapor
Evaporation
Pressure
Density
Rate
N/A
N/A
N/A
Odor
Color
Phase
Water
Solubility
N/A
Grey
Solid Pellets
N/A
HAZARDS IDENTIFICATION
Possible sensitizer. keep away from sources of ignition - no smoking. Take precautionary measures against static discharges.
Keep container tightly closed and in a well-ventilated place. Harmful by inhalation. Irritating to respiratory system.
Lungs, bones, do not breathe dust. In case of insufficient ventilation, wear suitable respiratory equipment. Wear suitable
protective clothing.
TOXICITY DATA
May be harmful by inhalation or ingestion. May cause eye irritation. may cause skin irritation. Material may be irritating to
mucous membranes and upper respiratory tract. prolonged or repeated exposure may cause allergic reactions in certain
sensitive individuals.
Coughing, chest pains, difficulty in breathing, gastrointestinal disturbances.
Prolonged exposure can cause damage to the lungs and bones. TO the best of our knowledge, the chemical, physical, and
toxicological properties have not been thoroughly investigated.
Lungs, thorax or respiration (tumors) tumorigenic (neoplastic by RTECS criteria) tumorigenic (equivocal tumorigenic agent by
RTECS criteria) tumorigenic (tumors at site of application) only selected registry of toxic effects of chemical substances
(RTECS) data is presented here. see actual entry in RTECS.
HEALTH HAZARD DATA
8H TWA 5MG/ME respirable fraction; 8h TWA 10MG/M3 total dust
FIRST-AID MEASURES
In case of contact, immediately flush eyes with copious amounts of water for at least 15 minutes while removing contaminated clothing and shoes. If inhaled,
remove to fresh air. If not breathing give artificial respiration. If breathing is difficult, give oxygen. If swallowed, wash out mouth with water provided person is
conscious. Call a physician. Remove and wash contaminated clothing promptly. In case of skin contact, immediately wash skin with soap and copious amounts of
water.
SECTION VIII
FIRE FIGHTING MEASURES
EXTINGUISHING MEDIA:
Carbon dioxide, dry chemical powder or appropriate foam.
UNUSUAL FIRE AND EXPLOSIONS HAZARDS: Material may have an exothermic reaction above 200 c with halocarbon vapors and may produce toxic
hydrochloric acid and phosgene.
SECTION IX
ACCIDENTAL RELEASE MEASURES
Shut off all sources of ignition. Wear self-contained breathing apparatus, rubber boots and heavy rubber gloves. Sweep up, place in a bag and hold for waste disposal. Ventilate area and wash spill site after material pickup is complete.
SECTION X
Stability:
Incompatibilities:
SECTION XI
STABILITY AND REACTIVITY
Stable.
Strong acids, strong bases, chlorine trifluoride, ethylene oxide, halocarbons, oxygen difluoride, sodium nitrate, vinyl acetate,
strong oxidizing agents,organic materials. Protect from moisture. Hazardous combustion or decomposition products. Nature of
decomposition products not known. Hazardous polymerization will not occur.
SPECIAL PRECAUTIONS AND COMMENTS
The above information is believed to be correct but does not purport to be all inclusive. It shall serve only as a guide. Shimadzu shall not be held liable for any
damage resulting from handling or contact with the above product. Users should make their own determinations regarding the suitability of this information for
their particular purposes.
340
TOC-VCPH/CPN
6.9
Material Safety Data Sheets
6.9.9 Potassium Nitrate
6.9.9 Potassium Nitrate
Shimadzu Scientific Instruments, Inc.
7102 Riverwood Drive Columbia, MD 21046
Tel: 1(800) 477-1227
Control No.
Date:
MATERIAL SAFETY DATA SHEET
SECTION I
CAT. NO.
PRODUCT IDENTIFICATION
CAS NO.
NAME:
Potassium Nitrate
PRODUCT USE:
This product is for specific use with TOC instruments.
SECTION II
7757-79-1
OTHER NAME: Nitric Acid, Potassium Salt, Saltpeter
PHYSICAL DATA
Melt
Boil
Specific
Vapor
Vapor
Evaporation
Point
Point
Gravity
Pressure
Density
Rate
334°C
N/A
2.11
N/A
3.0
N/A
SECTION III
Odor
Color
Phase
Water
Solubility
Odorless
White
Crystalline Powder
Appreciable
(>10%)
HAZARDS IDENTIFICATION
Possible eye and skin irritation. Avoid contact.
SECTION IV
HEALTH HAZARD DATA
TARGET ORGANS: Blood, Central Nervous System
SIGNS/SYMPTOMS OF OVEREXP: Chronic exposure can cause anemia, nephritis and methemoglobinemia.
SECTION V
INGESTION:
SKIN:
EYES:
SECTION VI
FIRST-AID MEASURES
If conscious, induce vomiting and call a physician.
Flush with water.
Flush with water for 15 minutes and call a physician.
FIRE FIGHTING MEASURES
EXTUNGUISHING MEDIA
SPECIAL.
Carbon dioxide, dry chemical, or appropriate foam.
Use NIOSH/MSHA approved SCBA & full protective equipment. Move containers from fire area if it can be done without
risk. Use water to keep fire exposed containers cool.
UNUSUAL FIRE AND EXPLOSIONS HAZARDS.Strong oxidizer. Contact with other materials may cause fire. When exposed to heat, closed containers may
explode.Emits toxic fumes under fire conditions.
SECTION VII
ACCIDENTAL RELEASE MEASURES
Absorb on sand or vermiculite and place in closed containers for disposal. Ventilate area and wash spill site after material pickup is complete. Evacuate the area.
Wear self-contained breathing apparatus, rubber boots, and heavy rubber gloves.
SECTION VIII
SPECIAL PRECAUTIONS AND COMMENTS
The above information is believed to be correct but does not purport to be all inclusive. It shall serve only as a guide. Shimadzu shall not be held liable for any
damage resulting from handling or contact with the above product. Users should make their own determinations regarding the suitability of this information for
their particular purposes.
TOC-VCPH/CPN
341
6.9 Material Safety Data Sheets
6.9.10 Sodium Bicarbonate
6.9.10 Sodium Bicarbonate
Shimadzu Scientific Instruments, Inc.
7102 Riverwood Drive Columbia, MD 21046
Tel: 1(800) 477-1227
Control No.
Date:
MATERIAL SAFETY DATA SHEET
SECTION I
CAT. NO.
630-00963-01
NAME:
Sodium Bicarbonate 100%
SECTION II
PRODUCT IDENTIFICATION
CAS NO.
144-55-8
OTHER NAME: Baking Soda
PRDUCT USE
This product is specifically for use as a catalyst in the TOC 500,TOC 5000, and TOC 4000 series of TOC analyzers. Refer to the appropriate instruction manual for
directions on proper use.
SECTION III
PHYSICAL DATA
Melt
Boil
Point
Point
50°C
N/A
Density
2.16
SECTION IV
Vapor
Vapor
Evaporation
Pressure
Density
Rate
N/A
N/A
N/A
Odor
Color
Phase
Water
Solubility
N/A
White
Solid Powders
10%
HAZARDS IDENTIFICATION
Possible eye and skin irritation. Avoid contact.
SECTION V
TOXICITY DATA
N/A
SECTION VI
HEALTH HAZARD DATA
Exposure to large amounts can cause gastrointestinal disturbances.
SECTION VII
FIRST-AID MEASURES
In case of contact, immediately flush eyes with copious amounts of water for at least 15 minutes. In case of skin contact, immediately wash skin with soap and
copious amounts of water.
SECTION VIII
FIRE FIGHTING MEASURES
N/A
SECTION IX
ACCIDENTAL RELEASE MEASURES
N/A
SECTION X
STABILITY AND REACTIVITY
N/A
SECTION XI
SPECIAL PRECAUTIONS AND COMMENTS
The above information is believed to be correct but does not purport to be all inclusive. It shall serve only as a guide. Shimadzu shall not be held liable for any
damage resulting from handling or contact with the above product. Users should make their own determinations regarding the suitability of this information for
their particular purposes.
342
TOC-VCPH/CPN
6.9
Material Safety Data Sheets
6.9.11 Sodium Carbonate
6.9.11 Sodium Carbonate
Shimadzu Scientific Instruments, Inc.
7102 Riverwood Drive Columbia, MD 21046
Tel: 1(800) 477-1227
Control No.
Date:
MATERIAL SAFETY DATA SHEET
SECTION I
CAT. NO.
630-0092-01
NAME:
Sodium Carbonate, 100%
SECTION II
PRODUCT IDENTIFICATION
CAS NO.
497-19-8
OTHER NAME: N/A
PRDUCT USE
This product is specifically for use in the IC channel of the TOC 500, TOC 5000, and TOC 4000 series of TOC analyzers. Refer to the appropriate instruction manual for directions on proper use. Keep tightly sealed in a cool, dry, well ventilated place. Store separate form flammable and combustible materials. Wear appropriate protective clothing and eye protection.
SECTION III
PHYSICAL DATA
Melt
Boil
Point
Point
N/A
N/A
SECTION IV
Density
2.16
Vapor
Vapor
Evaporation
Pressure
Density
Rate
N/A
N/A
N/A
Odor
Color
Phase
Water
Solubility
N/A
White
Solid Powder or
Crystals
Completely
Soluble
HAZARDS IDENTIFICATION
Corrosive, causes burns, harmful if swallowed. Target organ(s): liver, blood. In case of contact with eyes, rinse immediately with plenty of water and seek medical
advice. Take off all contaminated clothing. Wear suitable protective clothing, gloves and eye/face protection.
SECTION V
TOXICITY DATA
ORL-RAT LD50:4090mg/KG,IHL-RAT LC50:2300mg/M3/2H
ORL-MUS LD50:6600mg/KG,IHL-MUS LC50:1200mg/M3/2H
SCU-MUS LD50:2210mg/KG,IHL-GPG LC50:800mg/M3/2H
SECTION VI
HEALTH HAZARD DATA
Harmful if swallowed, inhaled, or absorbed through skin.causes severe irritation. High concentrations are extremely destructive to tissues of the mucous membranes and upper respiratory tract, eyes and skin. Symptoms of exposure may include burning sensation, coughing, wheezing, laryngitis, shortness of breath, headache, nausea and vomiting. To the best of our knowledge, the chemical, physical, and toxicological properties have not been thoroughly investigated.
SECTION VII
FIRST-AID MEASURES
In case of contact, immediately flush eyes or skin with copious amounts of water for at least 15 minutes while removing contaminated clothing and shoes. Assure
adequate flushing of the eyes by separating the eyelids with fingers. If inhaled, remove to fresh air. If not breathing give artificial respiration. If breathing is difficult, give oxygen. If swallowed, wash out mouth with water provided person is conscious. Call a physician. wash contaminated clothing before reuse. Discard contaminated shoes.
SECTION VIII
FIRE FIGHTING MEASURES
NONCOMBUSTIBLE.
Use extinguishing media appropriate to surrounding fire conditions.
SPECIAL.
Wear self-contained breathing apparatus and protective clothing to prevent contact with skin and eyes.
UNUSUAL FIRE AND EXPLOSIONS HAZARDS.Emits toxic fumes under fire conditions.
SECTION IX
ACCIDENTAL RELEASE MEASURES
Evacuate area. Wear self-contained breathing apparatus, rubber boots and heavy rubber gloves. Wear disposable coveralls and discard them after use. Sweep up,
place in a bag and hold for waste disposal. Avoid raising dust.Ventilate area and wash spill site after material pickup is complete.
SECTION X
STABILITY AND REACTIVITY
INCOMPATIBILITIES:
Strong acids, aluminum, protect from moisture.
HAZARDOUS COMBUSTION OR DECOMPOSITION PRODUCTS:Carbon monoxide, carbon dioxide.
SECTION XI
SPECIAL PRECAUTIONS AND COMMENTS
The above information is believed to be correct but does not purport to be all inclusive. It shall serve only as a guide. Shimadzu shall not be held liable for any
damage resulting from handling or contact with the above product. Users should make their own determinations regarding the suitability of this information for
their particular purposes.
TOC-VCPH/CPN
343
6.9 Material Safety Data Sheets
6.9.12 Potassium Hydrogen Phthalate
6.9.12 Potassium Hydrogen Phthalate
Shimadzu Scientific Instruments, Inc.
7102 Riverwood Drive Columbia, MD 21046
Tel: 1(800) 477-1227
Control No.
Date:
MATERIAL SAFETY DATA SHEET
SECTION I
CAT. NO.
630-00635-01
NAME:
Potassium Hydrogen Phthalate
SECTION II
PRODUCT IDENTIFICATION
CAS NO.
877-24-7
OTHER NAME: Phthalic Acid, Monopotassium Salt, Khp Primary Standard
PRODUCT USE
Specifically for use as an organic carbon standard in the Shimadzu TOC 500, TOC 5,000, and TOC 4,000 instruments. Consult the appropriate instrument manual
for proper use.
SECTION III
PHYSICAL DATA
Melt
Boil
Point
Point
295-300°C
N/A
Density
N/A
SECTION IV
Vapor
Vapor
Evaporation
Pressure
Density
Rate
N/A
N/A
N/A
Odor
Color
Phase
Water
Solubility
N/A
White
Crystals
N/A
HAZARDS IDENTIFICATION
Irritant, irritating to eyes, respiratory system and skin. Possible sensitizer. In case of contact with eyes, rinse immediately with plenty of water and seek medical
advice. Wear suitable protective clothing.
SECTION V
TOXICITY DATA
RTECS #: CZ4326000
1,2-BENZENEDICARBOXYLIC ACID, MONOPOTASSIUM SALT
ORL-RAT LD50:>3200mg/KG
KODAK* 21MAY1971
SKN-GPG LD50:>1 GM/KG
KODAK* 21MAY1971
Only selected registry of toxic effects of chemical substances (RTECS) data is presented here. See actual entry in RTECS for complete information.
SECTION VI
HEALTH HAZARD DATA
ACUTE EFFECTS:
May be harmful by inhalation, ingestion, or skin absorption; causes skin irritation; vapor or mist is irritating to the eyes,
mucous membranes and upper respiratory tract.
EXPOSURE CAN CAUSE ASTHMATIC SYMPTOMS: Cough, hoarseness, rhinorrhea, wheezing, and conjunctivitis, nausea, or vomiting. Prolonged or repeated
exposure may cause allergic reactions in certain sensitive individuals. To the best of our knowledge, the chemical, physical, and
toxicological properties have not been thoroughly investigated.
SECTION VII
FIRST-AID MEASURES
In case of contact, immediately flush eyes or skin with copious amounts of water for at least 15 minutes while removing contaminated clothing and shoes. If
inhaled, remove to fresh air. if not breathing give artificial respiration. If breathing is difficult, give oxygen. If swallowed, wash out mouth with water provided person is conscious. Call a physician. wash contaminated clothing before reuse.
SECTION VIII
FIRE FIGHTING MEASURES
EXTINGUISHING MEDIA:
Water spray, carbon dioxide, dry chemical powder or appropriate foam.
SPECIAL FIREFIGHTING PROCEDURES: Wear self-contained breathing apparatus and protective clothing to prevent contact with skin and eyes.
UNUSUAL FIRE AND EXPLOSIONS HAZARDS:Emits toxic fumes under fire conditions.
SECTION IX
ACCIDENTAL RELEASE MEASURES
Wear respirator, chemical safety goggles, rubber boots and heavy rubber gloves. Sweep up, place in a bag and hold for waste disposal. Avoid raising dust. Ventilate
area and wash spill site after material pickup is complete.
SECTION X
STABILITY AND REACTIVITY
STABILITY:
Stable.
INCOMPATIBILITIES:
Strong oxidizing agent
HAZARDOUS COMBUSTION OR DECOMPOSITION PRODUCTS:Toxic fumes of carbon monoxide, carbon dioxide
HAZARDOUS POLYMERIZATION:Will NOT occur.
SECTION XI
SPECIAL PRECAUTIONS AND COMMENTS
The above information is believed to be correct but does not purport to be all inclusive. It shall serve only as a guide. Shimadzu shall not be held liable for any
damage resulting from handling or contact with the above product. Users should make their own determinations regarding the suitability of this information for
their particular purposes.
344
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6.9
Material Safety Data Sheets
6.9.13 Water
6.9.13 Water
Shimadzu Scientific Instruments, Inc.
7102 Riverwood Drive Columbia, MD 21046
Tel: 1(800) 477-1227
Control No.
Date:
MATERIAL SAFETY DATA SHEET
SECTION I
CAT. NO.
PRODUCT IDENTIFICATION
CAS NO.
NAME:
Water
7732-18-5
OTHER NAME: Dihydrogen Oxide
MOLECULAR WEIGHT: 18
CHEMICAL FORMULA:H2O
SECTION I
HAZARDS IDENTIFICATION
EMERGENCY OVERVIEW:
HEALTH RATING:
REACTIVITY RATING:
LAB PROTECTIVE EQUIP:
Not applicable.
0 - None
1 - Slight
Goggles; lab coat
SECTION II
FLAMMABILITY RATING:
CONTACT RATING:
STORAGE COLOR CODE:
0 - None
0 - None
Orange (General Storage)
HEALTH EFFECTS
POTENTIAL HEALTH EFFECTS: Water is non-hazardous.
INHALATION:
Not applicable.
INGESTION:
Not applicable.
SKIN CONTACT
Not applicable.
EYE CONTACT:
Not applicable.
CHRONIC EXPOSURE:
Not applicable.
AGGRAVATION OF PRE-EXISTING CONDITIONS: Not applicable.
SECTION III
FIRST AID MEASURES
INHALATION:
SKIN CONTACT:
Not applicable.
Not applicable.
SECTION IV
INGESTION:
EYE CONTACT:
Not applicable.
Not applicable.
FIRE FIGHTING MEASURES
FIRE:
Not applicable.
EXPLOSION:
Not applicable.
FIRE EXTINGUISHING MEDIA: Use extinguishing media appropriate for surrounding fire.
SPECIAL INFORMATION:
In the event of a fire, wear full protective clothing and NIOSH-approved self-contained breathing apparatus with full facepiece
operated in the pressure demand or other positive pressure mode.
SECTION V
ACCIDENTAL RELEASE MEASURES
Non-hazardous material. Clean up of spills requires no special equipment or procedures.
SECTION VI
HANDLING AND STORAGE
Keep container tightly closed. Suitable for any general chemical storage area. Protect from freezing. Water is considered a non-regulated product, but may react
vigorously with some specific materials. Avoid contact with all materials until investigation shows substance is compatible.
SECTION VII
EXPOSURE CONTROLS/PERSONAL PROTECTION
AIRBORNE EXPOSURE LIMITS: Not applicable.
VENTILATION SYSTEM:
PERSONAL RESPIRATORS (NIOSH APPROVED): Not applicable.
SKIN PROTECTION:
None required.
EYE PROTECTION:
SECTION VIII
Not applicable.
None required.
PHYSICAL AND CHEMICAL PROPERTIES
Melt
Boil
Specific
Vapor
Vapor
Evaporation
Point
Point
Gravity
Pressure
Density
Rate
0°C
100°C
1.00
17.5 @ 20°C
N/A
N/A
SECTION IX
pH
Color
Phase
Water
Solubility
7.0
Clear,
Colorless
Liquid
Complete
STABILITY AND REACTIVITY
STABILITY:
Stable under ordinary conditions of use and storage.
HAZARDOUS DECOMPOSITION PRODUCTS: Not applicable.
HAZARDOUS POLYMERIZATION: Will not occur.
INCOMPATIBILITIES:
Strong reducing agents, acid chlorides, phosphorus trichloride, phosphorus pentachloride, phosphorus oxychloride.
SECTION X
ECOLOGICAL INFORMATION
ENVIRONMENTAL FATE:
Not applicable.
ENVIRONMENTAL TOXICITY: Not applicable.
SECTION XI
DISPOSAL CONSIDERATIONS
Whatever cannot be saved for recovery or recycling should be flushed to sewer. If material becomes contaminated during use, dispose of accordingly. Dispose
of container and unused contents in accordance with federal, state and local requirements.
SECTION XII
TRANSPORT INFORMATION
Not regulated.
SECTION XIII
NFPA RATINGS:
LABEL HAZARD WARNING:
LABEL PRECAUTIONS:
LABEL FIRST AID:
PRODUCT USE:
SECTION XIV
OTHER INFORMATION
Health: 0 Flammability: 0 Reactivity: 0
Not applicable.
Keep in tightly closed container.
Not applicable.
Laboratory Reagent.
SPECIAL PRECAUTIONS AND COMMENTS
The above information is believed to be correct but does not purport to be all inclusive. It shall serve only as a guide. Shimadzu shall not be held liable for any
damage resulting from handling or contact with the above product. Users should make their own determinations regarding the suitability of this information for
their particular purposes.
TOC-VCPH/CPN
345
6.9 Material Safety Data Sheets
6.9.13 Water
346
TOC-VCPH/CPN
Appendix A
Appendix A
Method Validation
The Method Validation function tests the variance and the linearity of the data. The
function also determines performance characteristics according to the requirements of DIN
38402-Part 51. The Method Validation function displays the data used for executing
method validation, performs the required calculations and displays the results. Data can
either be imported directly from the TOC-Control V Sample Table, or entered manually
into the data table. Data can also be exported to ASCII files, stored and printed.
Method Validation
Main Window
A.1
Main Window
The Main Window is separated into three sections. The upper left section of the window
displays the calibration curve, the upper right section displays the calculated validation
results and the lower portion displays the data table, which contains all relevant data for
performing the validation. The toolbar options (such as Open, Save, Cut, Copy, and Paste)
are similar to those described in Section 4.4.2 "File Menu" and Section 4.4.3 "Edit Menu".
Figure A.1 Method Validation Main Window
The windows can be resized by dragging the dividers between the sections.
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Method Validation
File Menu
A.2
File Menu
Figure A.2 File Menu
A.2.1 New
Use the New command to create a new, empty method validation file. A new file can also
be created by clicking the New toolbar button. If a file that contains modified and unsaved
data is open when the New command is selected, a prompt is displayed in a dialog box.
Select one of the options in the dialog box to determine if the unsaved data should be saved
before opening a new method validation file. Click the Yes button to save the document and
create a new method validation file. Click the No button to create a new document without
saving previous data.
Figure A.3 Prompt for Saving Data
TOC-VCPH/CPN
349
Method Validation
File Menu
A.2.2 Open
Use the Open command to open a saved method validation file (*.val). A file can also be
opened by clicking the Open toolbar button.
Start the method validation process by selecting a.cal file; application of DIN 38402 will
begin. The process can also be started by selecting the calibration curve row in the Sample
Table and opening the method validation function using the Tools>Method Validation
command.
Figure A.4 Open Dialog Box
When the Open command is selected, the File>Open dialog box is displayed. To open an
existing file, select the filename and choose the Open button. To create a new method
validation file, type the filename into the File name text field, then select the New button.
For further information on the standard functions of the Open dialog box, refer to Section
4.4.2.4 "Open".
Note:
350
TOC-VCPH/CPN
An error message is displayed if a file that is not in a correct, TOC-Control V format is selected.
Method Validation
File Menu
A.2.3 Save
Use the Save command to save data in the current active file. If the file has not been saved,
selecting the Save command opens the Save As dialog box. The Save command can also be
executed by clicking the Save toolbar button.
A.2.4 Save As
Figure A.5 Save As Dialog Box
The Save As command saves the active, current data to a new file name. Enter the desired
name in the File Name field. Two different file types are available: validation files (*.val)
used for storing the data in binary files and ASCII files (*.txt) used for exporting the data.
Select the desired file type from the Save As Type drop-down list. Use the Save In window
to select the location where the file should be saved. For details about the Save As
command, refer to Section 4.4.2.7 "Save As".
A.2.5 Print
Use the Print command to print data from a method validation file. Executing the Print
command opens the Print dialog box; displayed options vary based on the installed printer
driver. The Print command can also be executed by clicking the Print toolbar button.
Figure A.6 Print Dialog Box
Use the Print Range option to specify the range to be printed. The All selection prints all
pages in the file. Specific pages can be printed by selecting the Pages option and entering
the desired page numbers. Use the Number of Copies field to select the number of copies to
be printed.
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351
Method Validation
File Menu
A.2.6 Print Preview
Use the Print Preview command to view the method validation file before printing.
Figure A.7 Print Preview Window
Button
Description
Next Page and Previous Page Click the Next Page button to display the next page of the
report. Click the Previous page button to display the previous
page of the report. The Next Page button is disabled when the
last page of the report is displayed, and the Previous Page
button is disabled when the first page of the report is displayed.
352
One Page/Two Page
Click the One Page button to display one page at a time in the
Print Preview window. After selection, the button toggles to
the Two Page button. Click the Two Page button to display
two pages side by side.
Zoom In and Zoom Out
Click the Zoom In and Zoom Out buttons to change the magnification of the displayed pages. Three different zoom factors are available. Repeated selection of either option will
continue to increase or decrease the magnification, as applicable.
Close
Click the Close button to close the Print Preview window and
return to the previous window.The Print Preview window
must be closed to edit the report.
Print
Click the Print button to print the report.
TOC-VCPH/CPN
Method Validation
File Menu
A.2.7 Print Setup
Select Print Setup to open the Print Setup dialog box.
Figure A.8 Print Setup Dialog Box
The print options available vary based on the printer installed. Select the paper size and
source from the drop-down lists, and select Portrait or Landscape to change the orientation
of the printed pages. Click the OK button to save the selections, or click the Cancel button
to close the dialog box without saving changes.
A.2.8 Page Setup
Use the Page Setup command to select items to be printed and to select options for printing
format, such as margins, headers, and footers.
Figure A.9 Page Setup Window: Data Tab
The Page Setup window consists of several tabs. Use the OK button to save changes and
exit the Page Setup window. Click the Cancel button to exit the Page Setup window without
saving changes. Click the Apply button to update the parameters without closing the Page
Setup window.
Note:
On each tab in the Page Setup window, certain items are checked (selected) by
default. To deselect these options, click the item.
TOC-VCPH/CPN
353
Method Validation
File Menu
Data Tab
The Data tab displays a list of items that can be selected for printing. Select the desired
items and click the OK button.
Grid Tab
Figure A.10 Page Setup Window: Grid Tab
The Grid tab displays a list of format items for the report, as described below.
354
Option
Description
Row Headers
Prints row headers in the table.
Column Headers
Prints column headers in the table.
Print Frame
Prints a frame around the table.
Vertical Lines
Prints vertical lines in the table.
Horizontal Lines
Prints horizontal lines in the table.
Only Black and White
Prints only in 2 colors, without gray backgrounds or other
colors.
First Rows, then Columns
Prints rows first, followed by columns, when more than one
page is printed
First Columns, then Rows
Prints columns first, followed by rows, when more than one
page is printed.
Vertical
Prints the table on the vertical center of the page.
Horizontal
Prints the table on the horizontal center of the page.
TOC-VCPH/CPN
Method Validation
File Menu
Miscellaneous Tab
Figure A.11 Page Setup Window: Miscellaneous Tab
The Miscellaneous tab displays a list of format items for the report, as described below.
Setting Item
Description
Margins
Use the spin controls to enter the page margins (in mm.).
Footer, Page No.
Select this option to print the page number in the footer of
each page.
Header
Organization: Select this option and enter the name of the
organization in the text box to print the organization name in
the page header.
Logo: Select this option to print a bitmap in the page header.
Use the Browse button to select the bitmap file.
Date/Time: Select this option to print the current system date
and time in the page header.
Operator: Select this option to print the current user name in
the page header.
A.2.9 Exit
Select Exit to close the Method Validation application. If an active file contains unsaved
information, a prompt to save changes is displayed. Select Yes or No, or select Cancel to
abort the exit function.
Figure A.12 Prompt to Save Data Changes
TOC-VCPH/CPN
355
Method Validation
Edit Menu
A.3
Edit Menu
Options such as Cut, Copy, and Paste are available only if content is selected.
Figure A.13 Edit Menu
A.3.1 Undo
Use the Undo function to reverse the last change made in the data table. This function is
available only in documents that can be manually edited and when the user changes the
content of a cell in the data table.
A.3.2 Cut/Copy/Paste
Use the Cut, Copy, and Paste commands to edit highlighted table cells and rows. The Cut
command deletes information in rows or cells and stores it on the clipboard. The Copy
command copies data from rows or cells to the clipboard. The Paste command copies the
contents of the clipboard to the current row of the table. When pasting a whole row, select
the entire destination row first by clicking the row number.
Note:
TIP »
Do not select a row for pasting that currently contains data. The data will be overwritten!
The Cut, Copy and Paste commands have shortcut buttons on the toolbar.
A.3.3 Insert Row
Use the Insert Row command to add an additional row to the data table. This command is
available only for documents that can be manually edited. TOC-Control V method
validation documents have a fixed number of rows equivalent to the number of calibration
points in the calibration curve.
356
TOC-VCPH/CPN
Method Validation
Edit Menu
A.3.4 Delete Row
Use the Delete Row command to delete a row from the data table. The command is
available only for documents that can be manually edited. TOC-Control V method
validation documents have a fixed number of rows equivalent to the number of calibration
points in the calibration curve. The Delete Row function is not available if the number of
rows is 4 or less. Once a row is deleted, the format of the remaining rows is updated. A
confirmation dialog box opens asking you to confirm the deletion.
Figure A.14 Delete Row Confirmation Dialog Box
A.3.5 Insert Column
Use the Insert Column command to add an additional column to the data table. The
command is available only for documents that can be manually edited. TOC-Control V
method validation documents have a fixed number of columns equivalent to the maximum
number of injections specified for the calibration points.
A.3.6 Delete Column
Use the Delete Column function to delete a column from the data table. The command is
available only for documents that can be manually edited. TOC-Control V method
validation documents have a fixed number of columns equivalent to the maximum number
of injections specified for the calibration points. The Delete Column function is not
available if the number of columns is 3 or less. Once a column is deleted, the format of the
remaining columns is updated. A confirmation dialog box opens asking you to confirm the
deletion.
A.3.7 Recalculate
Use the Recalculate command to recalculate all method validation data. The results and
calibration curve sections of the Method Validation window are also updated when the
Recalculate command is selected. Errors that occur during the recalculation process are
displayed in message boxes. For example, an error message may be displayed if the data in
the table does not contain sufficient information, if there are not enough data points defined
in the table, if less than 3 injections are available, and if numeric data is incorrect and
results in an illegal mathematical operation (such as division by zero).
TIP »
The Recalculate command has a shortcut button on the toolbar.
TOC-VCPH/CPN
357
Method Validation
View Menu
A.4
View Menu
Figure A.15 View Menu
Toolbar
The Toolbar function displays or hides the toolbar.
Status Bar
The Status Bar function displays or hides the status bar.
358
TOC-VCPH/CPN
Method Validation
Options Menu
A.5
Options Menu
Figure A.16 Options Menu
A.5.1 General Parameter
Select the General Parameter command to display the General Information dialog box.
Figure A.17 General Information Dialog Box
The General Information dialog box is used to view and edit information about the method
validation file, such as the system used to create the file, the file version, the operator who
created the file and the date on which the file was created. Some information fields may be
disabled. Comments about the file are displayed in the Comment field.
TOC-VCPH/CPN
359
Method Validation
Options Menu
A.5.2 Method Validation Parameter
The Method Validation Parameter command displays the Method Validation Parameter
window, which contains detailed information about the method, as described below.
Figure A.18 Method Validation Parameter Window
360
Item
Description
Enable manual editing
Select to allow data tables to be edited manually. This option
is disabled for files linked to TOC-Control V calibration
curves. If this option is deselected, it is disabled and cannot
be selected again. This option is selected by default.
Unit
Displays the calibration curve units. This option is disabled if
the Enable manual editing option is not selected.
Analysis Type
Displays the analysis used to create the calibration curve.
This option is disabled if the Enable manual editing option is
not selected.
Date/Time
Displays the date and time the file was created.
Title
Displays the title of the method validation file.
Calibration curve file name
Displays the name of the TOC-Control V calibration curve.
TOC-VCPH/CPN
Method Validation
Options Menu
A.5.3 Font
Use the Font command to select fonts for printed reports and display screens. Selecting the
Font command opens the Font dialog box.
TIP »
The Font command has a shortcut button on the toolbar.
Figure A.19 Font Dialog Box
Choose a font for printed reports by selecting options from the Font, Font Style, Size, Color
and Script drop-down lists. A preview of the font appearance is visible in the Sample field
on the lower portion of the Font dialog box.
TOC-VCPH/CPN
361
Method Validation
Options Menu
A.5.4 Floating Point Numbering Format
Use the Floating Point Numbering Format command to select display options for numeric
results in the method validation tables. These options apply only to the manner in which
numbers are displayed; internal data retain their original values.
Figure A.20 Floating Point Format Window
Common Floating Point Numbers
Setting Item
Description
Number of significant digits
Select this option to display common floating point numbers
using a specified number of significant digits. Use the spin
control to set the number of significant digits. The default
value is 4.
Number of digits after the
decimal point
Select this option to display common floating point numbers
using a specified number of digits after the decimal point.
Use the spin control to set the number of digits after the decimal point. The default value is 2.
Percent Values
362
Setting Item
Description
Number of significant digits
Select this option to display percent values using a specified
number of significant digits. Use the spin control to set the
number of significant digits. The default value is 4.
Number of digits after the
decimal point
Select this option to display percent values using a specified
number of digits after the decimal point. Use the spin control
to set the number of digits after the decimal point. The default
value is 2.
TOC-VCPH/CPN
Method Validation
Options Menu
A.5.5 ASCII Export Options
Use the ASCII Export Options function to export method validation data to an ASCII file.
Figure A.21 ASCII Export Options Dialog Box
Setting Item
Description
Header
Select this option to export method validation file header.
Data
Select this option to export method validation data.
Results
Select this option to export method validation results.
Separator
Select the type of separator to be used between items in the
ASCII file.
Export strings in quotation
marks
Select this option to add quotation marks to all exported
strings.
To export a file, create or open a method validation file. Select the desired options from the
ASCII Export Options dialog box and select OK. The File>Save As dialog box is
displayed. Enter a file name for the ASCII file and select the *.txt file type.
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363
Method Validation
Options Menu
A.5.6 Validation Strictly Following DIN38402
Use the Validation Strictly Following DIN38402 option to conduct the validation
calculation by DIN 38402 requirements; that is, only the area obtained from the first
injection of every standard is used in the calibration calculation. When this option is not
selected, the mean value of the area counts from all injections of each standard is used in
the calibration calculation.
Perform method validation according to DIN regulations as follows:
Step 1
Select the estimated working range.
Step 2
Prepare 10 calibration standards, with concentrations distributed uniformly
over the complete working range.
Step 3
Create a Sample Table, with 10 injections of the highest and lowest standard
concentrations and a single injection for all other standards. If more than one
injection is made of the intermediate standards, the linearity test is calculated
with the results of the first replicates only.
Step 4
Analyze the standards. The results are saved in a.cal file.
Step 5
Select Method Validation from the Tools menu in the Sample Table Editor.
The Method Validation main window is displayed.
Step 6
Select the Validation Strictly Following DIN from the Options menu.
Step 7
Select Open from the File menu.
Step 8
Select.cal from the file type drop-down list.
Step 9
From the list of file names, select the.cal file where the measurement data was
saved. Then select OK.
Step 10
The calculations are automatically performed, and the validation data
displayed.
Step 11
Select Save from the File menu, assign a file name in the dialog box, and
select OK. The validation data is saved with a.val file name extension.
When the Validation Strictly Following DIN option is enabled, a check mark is displayed in
front of the menu item. After selecting this option, a confirmation message is displayed.
Figure A.22 Confirmation Message for Validation Strictly Following DIN 38402
Select Yes to execute recalculation. The calibration curve and result sections of the Method
Validation window are updated accordingly.
364
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Method Validation
Help Menu
A.6
Help Menu
About Meth Val...
Use the About command to view copyright and version information.
TOC-VCPH/CPN
365
Method Validation
Help Menu
366
TOC-VCPH/CPN
Appendix B
Appendix B
Control Charts
The Control Charts software monitors precision and accuracy of a defined data set. The
software supports five types of Control Charts:
•Mean Value Control Charts
•Recovery Control Charts
•Blind Value Control Charts
•Spanwidth Control Charts
•User Defined Control Charts
The Mean Value Control Chart checks the accuracy of an analytical method on an
instrument. Control value drifts may indicate a change in system performance.
The Recovery Control Chart tests an analytical method for matrix influences and provides a
restrictive control of accuracy by testing proportional system errors. Using certified
standards will test the accuracy of the system as well as the recovery rate.
The Blind Value Control Chart is a special form of the Mean Value Control Chart used for
quality assurance of the instrument and variable elements. Unlike the Mean Value Control
Chart, the control value is the information value (absorbance, peak height, peak area)
received from the analysis.
The Spanwidth Control Chart tests the precision of an analytical method and monitors the
accuracy under actual conditions (Drift Control). For this type of Control Chart, there are
several existing models for calculating the control and warning limits.
Each type of control chart can be used to create charts for different working range and
analysis methods. For each control chart, a file is created which contains general
information about the type, data structure and other global data.
Control Charts
File Menu
B.1
File Menu
Figure B.1 File Menu
B.1.1 New
The New function is used to define new control charts and displays the Control Chart
Wizard. Follow the Control Chart Wizard process to enter a new control chart. The file
extension *.cc is used for all control charts.
Note:
Control Chart parameters can be changed at a later time by selecting
Options>Control chart options from the main menu bar.
Control Chart Wizard System Information Window
The first page of the Control Chart Wizard is used to enter basic system information and is
similar to the System Information pages in the Method and Sample Wizards. Refer to
Section 4.4.5.2 "Sample" and Section 4.4.2.3 "Method Wizard".
Figure B.2 Control Chart Wizard: System Information Window
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Control Charts
File Menu
Control Chart Wizard Control Chart Type Window
Select the type of control chart to be created and select the analysis type from the drop
down list.
Figure B.3 Control Chart Wizard: Control Chart Type Window
Control Chart Wizard Control Chart Parameters Window
Enter the control chart parameter values and limits as described below.
Figure B.4 Control Chart Wizard: Control Chart Parameters Window
Setting Item
Description
Automatic calculation of the
control chart limits
Select to enable automatic calculation of the control chart
limits. The upper and lower warning and control limits are
calculated after the control samples for the preparation period
are added to the control chart.
No. of samples in the preperiod
Enter the number of samples in the preparation period. The
default value is 12. This option is disabled if the Automatic
calculation of the control chart limits option is not selected.
No. of samples in the control
period
Enter the number of samples in the control period. The
default value is 50.
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369
Control Charts
File Menu
Setting Item
Description
Working range
Enter the upper and lower limits of the working range. Match
the range with the concentration of samples used for control
tracking and the concentration range of the selected calibration curve. Use the drop-down list to select the units.
Rated Value
Enter the rated value of the working range. This option is disabled if the Automatic calculation of the control chart limits
option is not selected.
Control Limits
Enter the upper and lower control limits. This option is disabled if the Automatic calculation of the control chart limits
option is not selected.
Warning Limits
Enter the upper and lower warning limits. This option is disabled if the Automatic calculation of the control chart limits
option is not selected.
Exclusion Limits
Enter the upper and lower exclusion limits.
Control Chart Wizard Recovery Control Chart Parameter Window
This window is only displayed if the Recovery Control Chart is selected in the Control
Chart Wizard, and Automatic calculation of the control chart limits is not selected.
Figure B.5 Control Chart Wizard: Recovery Control Chart Parameter Window
370
Setting Item
Description
Use of certified standard
Select this option to use a certified sample as a control sample.
Fixed theoretical concentration
Select this option if the standard has a fixed concentration.
Enter the concentration in the text box.
Use of real sample
Select this option if the control sample is a real sample.
Fixed concentration of the
spiked component.
Select this option if the spiked component has a fixed concentration. Enter the concentration in the text box.
TOC-VCPH/CPN
Control Charts
File Menu
Control Chart Wizard Spanwidth Control Chart Options Window
This window is only displayed if the Spanwidth Control Chart is selected in the Control
Chart Wizard.
Figure B.6 Control Chart Wizard: Spanwidth Control Chart Options Window
Setting Item
Description
No. of inj. per sample
Enter the number of injections for a sample used in the control chart. The default value is 3, and the range is 3-25.
Refuse control samples with
different inj. no
Select this option to exclude from the control chart samples
whose number of injections differs from those specified in
the No. of inj. per sample field.
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371
Control Charts
File Menu
Control Chart Wizard History Window
The Control Chart Wizard History function is identical to other history functions in the
TOC-Control V system. Refer to Section 4.4.2.3 "Method Wizard" for more details about
the History function. The History window provides information on all control chart
changes when enabled.
Figure B.7 Control Chart Wizard: History Window
Setting Item
Description
Enable history log
Select this option to enable the History Log, which is used to
monitor all modifications to the control charts. Once the History Log is enabled, it cannot be turned off.
Operator has to comment on
all modifications
Select this option to require the user to enter comments or
obtain approval for modifications to the control charts.
B.1.2 Following Control Chart
Select the Following Control Chart menu item to create a Following Control Chart. It is
recommended that a new control chart be created after 50 samples have been entered in the
control period. The new control chart uses the calculated standard deviation from the
control period as the new control chart limits. Control chart options are:
Setting Item
Description
File Name
Displays the name of the currently active control chart.
Save the current control chart Enter a new file name in this field to save the currently active
as
control chart to a new location or with a new file name. A
confirmation message is displayed to confirm the operation.
372
Create
Select this option to create the Following Control Chart. The
new limits are calculated from the samples of the control
period stored in the previous control chart.
Parameter
Select this option to display the parameters of the newly created Following Control Chart. This function can also be
accessed using the Options>Control Chart Options command
in the main window.
TOC-VCPH/CPN
Control Charts
File Menu
B.1.3 Open
The Open command is used to open files. Select a *.cc file to open a control chart file.
Refer to Section 4.4.2.4 "Open" for further information on the standard File>Open dialog
box.
B.1.4 Save
The Save command saves the current control chart.
B.1.5 Save As
Use the Save As command to save files for the first time, or to save a file using a new file
name. Files can be saved as file types *.cc or *.txt (ASCII format). For more information
on the Save As function, refer to Section 4.4.2.7 "Save As".
B.1.6 Print>Data
Use the Print>Data command to print data in spreadsheet format. For more information on
the Print function, refer to Section 4.4.2.10 "Print>Table".
B.1.7 Print>Graph
Use the Print>Graph command to print data in graphical format. For more information on
the Print function, refer to Section 4.4.2.10 "Print>Table".
B.1.8 Print Preview>Data/Print Preview>Graph
Use the Print Preview>Data function to display a preview of the data to be printed. Use the
Print Preview>Graph function to display a preview of the graph to be printed. For more
information on the Print Preview function, refer to Section 4.4.2.12 "Print Preview>Table".
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373
Control Charts
File Menu
B.1.9 Print Setup
Use the Print Setup command to select the printing parameters.
Figure B.8 Print Setup Dialog Box
The print options available vary based on the printer installed. Select the paper size and
source from the drop-down lists, and select Portrait or Landscape to change the orientation
of the printed file. Select OK to save the selections, or Cancel to close the dialog box
without saving changes.
B.1.10 Page Setup
Use the Page Setup command to select items to be printed and to select options for printing
format, such as margins, headers, and footers.
Figure B.9 Page Setup Window: Data Tab
The Page Setup window consists of several tabs. Use the OK button to save changes and
exit the Page Setup window. Click the Cancel button to exit the Page Setup window without
saving changes. Click the Apply button to update the parameters without closing the Page
Setup window.
Note:
374
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On each tab in the Page Setup window, certain items are checked (selected) by
default. To deselect these options, click the item.
Control Charts
File Menu
Data Tab
The Data tab displays a list of items that can be selected for printing. Select the desired
items and click the OK button.
Grid Tab
Figure B.10 Page Setup Window: Grid Tab
The Grid tab displays a list of format items for the report.
Option
Description
Row Headers
Prints row headers in the table.
Column Headers
Prints column headers in the table.
Print Frame
Prints a frame around the table.
Vertical Lines
Prints vertical lines in the table.
Horizontal Lines
Prints horizontal lines in the table.
Only Black and White
Prints only in 2 colors, without gray backgrounds or other
colors.
First Rows, then Columns
Prints rows first, followed by columns, when more than one
page is printed
First Columns, then Rows
Prints columns first, followed by rows, when more than one
page is printed.
Vertical
Prints the table on the vertical center of the page.
Horizontal
Prints the table on the horizontal center of the page.
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375
Control Charts
File Menu
Miscellaneous Tab
Figure B.11 Page Setup Window: Miscellaneous Tab
The Miscellaneous tab displays a list of format items for the report, as described below.
Setting Item
Description
Margins
Use the spin controls to enter the page margins (in mm).
Footer, Page No.
Select this option to print the page number in the footer of
each page.
Header
Organization: Select this option and enter the name of the
organization in the text box to print the organization name in
the page header.
Logo: Select this option to print a bitmap in the page header.
Use the Browse button to select the bitmap file.
Date/Time: Select this option to print the current system date
and time in the page header.
Operator: Select this option to print the current user name in
the page header.
B.1.11 Exit
Select Exit to close the Control Chart application.
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Control Charts
Edit Menu
B.2
Edit Menu
Figure B.12 Edit Menu
Copy
Use the Copy command to copy the selected range from the data table to the clipboard.
Recalculate
Use the Recalculate command to recalculate the limits of the control chart. This function
should be performed after one or more control samples have been excluded or added to the
control chart.
Exclude
Use the Exclude command to exclude a selected range of control samples from the control
chart calculations. When Exclude is selected, the Exclude dialog box is displayed. Enter a
comment describing the reason for excluding the sample. The Exclude function is only
available when one or more control samples are selected. A dialog box displays a message
requesting confirmation that the sample be excluded. Select Yes to confirm and recalculate
the control limits, or No to abort recalculation.
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377
Control Charts
View Menu
B.3
View Menu
Figure B.13 View Menu
B.3.1 Statistics
The Statistics command displays the Statistics window.
Figure B.14 Statistics Window
378
Setting Item
Description
Type
Displays the type of control chart.
No. of samples (pre-period)
Displays the number of samples in the preparation period.
This value was entered in the Control Chart Wizard.
Total no. of samples
Displays the total number of samples in the control chart.
Excluded samples are not included in the total number.
Control limits
Displays the control limits.
Data from the control period
Displays the Average Control Value, which is the mean value
of the samples in the control period. Also displays the calculated standard deviation and coefficient of variation.
TOC-VCPH/CPN
Control Charts
View Menu
B.3.2 Comparison
After a control chart is completed, the results from the control period must be compared
with the results from the preparation period. For control charts without a preparation
period, the current values must be compared with the results of the preparation period or the
control period from the previous control chart. The View>Comparison command displays
the Comparison between control charts window.
Figure B.15 Comparison Between Control Charts Window
Setting Item
Description
Previous control chart
Displays the file name of the previous control chart, if applicable.
Mean value t-test
Displays the results of the T-test in the text box beneath the
Item and Value lists. The T-table value and the calculated test
value are also displayed in the Item and Value list. The test
value is calculated based on the mean values and variances
obtained from the control and preparation period. The T-test
result shows whether the long term deviation of the control
samples is significant.
F-test
Displays the results of the F-test in the text box beneath the
Item and Value list. The F-table value and the calculated test
value are also displayed in the Item and Value list.
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379
Control Charts
View Menu
B.3.3 Out of Control Events
The Out of Control Events window displays a list of all out of control events.
Figure B.16 Out of Control Events Window
Spl. No.
Displays the sample number for which the out of control event occurred.
Event
Describes the out of control event.
B.3.4 Toolbar/Status Bar
The View>Toolbar and View>Status Bar commands show and hide the Toolbar and Status
Bar, respectively.
380
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Control Charts
Options Menu
B.4
Options Menu
Figure B.17 Options Menu
B.4.1 Control Chart Options
Use the Control Chart Options command to view and edit the control chart parameters
entered in the various pages of the Control Chart Wizard. Refer to Section B.1.1 "New".
Note:
Some options within the Control Chart Options tabs (such as control chart type or
sample concentrations) may be disabled if the control chart contains data. The
disabled parameters are options that cannot be modified once data is entered.
B.4.2 Font
The Font command opens the standard Font dialog box. Refer to Section 4.4.9.3 "Display
Settings>Display Font" for detailed information about font options.
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381
Control Charts
Options Menu
B.4.3 Floating Point Numbering Format
The Floating Point Numbering Format command is used to select display options for
numeric results in the control charts. These options apply only to the manner in which
numbers are displayed; internal data retain their original values.
Figure B.18 Floating Point Format Window
Common Floating Point Numbers
Setting Item
Description
Number of significant digits
Select this option to display common floating point numbers
using a specified number of significant digits. Use the spin
control to set the number of significant digits. The default
value is 4.
Number of digits after the
decimal point
Select this option to display common floating point numbers
using a specified number of digits after the decimal point.
Use the spin control to set the number of digits after the decimal point. The default value is 2.
Percent Values
382
Setting Item
Description
Number of significant digits
Select this option to display percent values using a specified
number of significant digits. Use the spin control to set the
number of significant digits. The default value is 4.
Number of digits after the
decimal point
Select this option to display percent values using a specified
number of digits after the decimal point. Use the spin control
to set the number of digits after the decimal point. The default
value is 2.
TOC-VCPH/CPN
Control Charts
Options Menu
B.4.4 ASCII Export Options
The ASCII Export Options function is used to export control chart data to an ASCIIformatted file.
Figure B.19 ASCII Export Options Dialog Box
Setting Item
Description
Header
Select this option to export control chart file header.
Data
Select this option to export control chart data.
Limits
Select this option to export control chart limits.
Separator
Select the type of separator to be used between items in the
ASCII file.
Export strings in quotation
marks
Select this option to add quotation marks to all exported
strings.
To export a file, create or open a control chart. Select the desired options from the ASCII
Export Options dialog box, and select OK. The File>Save As dialog box is displayed. Enter
a file name for the ASCII file and select the *.txt file type.
B.4.5 Enable Exclusion
Use the Enable Exclusion command to exclude a selected range of control samples from
the control chart calculations. When the Enable Exclusion command is executed, the
Exclude dialog box is displayed. Enter a comment describing the reason for excluding the
sample. This option is only available when one or more control samples are selected. A
dialog box displays a message requesting confirmation that the sample be excluded. Select
Yes to confirm and recalculate the control limits, or No to abort the process.
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383
Control Charts
Help Menu
B.5
Help Menu
About ContrCharts...
Use the About command to view copyright and version information.
384
TOC-VCPH/CPN
Index
Numerics
8-Port Sampler
Analysis Using ...................................................80
Connecting Two Units .....................................326
Connection .......................................................327
Front View .........................................................15
High Sensitivity..................................................82
Initializing ........................................................267
Installation .......................................................325
Maintenance............................................ 254–255
Rear View .......................................................... 15
Sealing the Sample Containers ..........................80
8-Port Valve
Replacing Rotor (8-Port Sampler) ...................254
Replacing Rotor (Syringe Pump).....................246
A
Accessories...................................................... 298–303
Special..............................................................303
Standard ...........................................................298
Acid
Addition in NPOC..................................... 76, 189
Addition Volume..............................................139
Checking Volume ............................................236
Effect on Instrument...........................................71
Hydrochloric ....................................................333
Phosphoric........................................................334
Preparation .........................................................51
Add Event Log ...........................................................22
Administration .................................................... 19–33
Air, Low Pressure Safety .........................................331
Alkaline Samples .......................................................71
Analysis
Blank Check.......................................................66
Calibration Parameters.....................................128
Calibration Run ................................................100
Control Sample Parameters..............................196
Creating New Method......................................135
Ending ..............................................................120
Gas Sample ......................................................227
Group Of Samples............................................181
High Sensitivity..................................................75
IC........................................................................56
Individual Sample ............................................185
Manual Injection ..............................................219
Method Parameters ..........................................136
New ..................................................................125
New Catalyst ......................................................36
POC....................................................................58
Preparation .................................................. 36–82
Principles................................................. 284–288
Procedures................................................. 89–121
Sample Parameters...........................................186
Sample Run ......................................................108
Suspended Solids ...............................................69
Technical Information............................. 289–293
TN ......................................................................59
Viewing Data in Real Time .............................167
Application Operations ................................... 219–233
ASCII Export Options
Data Tab...........................................................147
Header Tab.......................................................146
Miscellaneous Tab ...........................................148
System Tab ......................................................147
ASCII File, Exporting Control Charts .....................383
ASI-V, See Autosampler
Auto Dilution ..........................................132, 139, 189
Auto Generate ..........................................................181
Auto Regeneration of IC Solution ............................. 27
Auto Restart .............................................................121
Autosampler.............................................................295
Cables, Connecting ................................. 318, 319
Cover Installation.............................................323
Drain Tank Installation .................................... 323
Front View .........................................................14
High Sensitivity Analysis ..................................75
Initializing........................................................ 267
Installation .......................................................317
Maintenance............................................ 252–253
Needle Change.................................................268
Needle Types .............................................. 28, 85
Needle, Coaxial................................................322
Needle, Sample ................................................321
NPOC Analysis..................................................76
Positioning .......................................................317
Rear View .......................................................... 14
Rinse Bottle Inspection.................................... 252
Rinse Bottle Installation...................................323
Rinse Pump Head Replacement.......................253
Sample Catcher Inspection ..............................252
Shipping Screw ................................................317
Software Settings ........................................ 28, 84
Specifications...................................................295
Tray Type...........................................................28
Troubleshooting ...................................... 278–280
Turntable Installation.......................................323
Vial Positions...................................................179
Vial Rack Change ............................................267
Vial Rack Installation ......................................323
B
Background Monitor ................................................203
Base, Effect on Instrument.........................................71
Blank Check...................................................... 68, 269
Analysis..............................................................66
Using Area in Calculations ............ 139, 189, 198
Blank, System ..........................................................291
Buzzer, Setting in Software .......................................84
Index-1
Index
C
Cable Connections ................................................... 325
Cables, Connecting ......................................... 318, 319
Calibration Curve .................................................... 290
1-Point and 2-Point .......................................... 290
Calculation Method ......................................... 171
Creating .................................................. 126, 132
Entering Calibration Standard Levels.............. 132
Gas Sample Analysis ....................................... 229
High Sensitivity Analysis .................................. 65
Inserting into Method ...................................... 137
Inserting into Sample Table............................. 126
Inserting Into Sample Wizard.......................... 187
Manual Injection Kit........................................ 221
Multi-Point....................................................... 290
Optimum .......................................................... 292
Options............................................................. 128
Points List ........................................................ 131
Points Parameters ............................................ 132
Shifting To Blank Point ................................... 291
Shifting to Origin............................129, 172, 290
Types ...................................................... 128, 290
Viewing Data ................................................... 160
Viewing Properties .......................................... 170
Calibration Curve Wizard............................... 100, 126
Analysis Information Window ........................ 128
Analysis Options.............................................. 102
Calibration Points List ..................................... 103
Calibration Points Window ............................. 131
Curve Type ...................................................... 101
Curve Type Window ....................................... 128
Default Measurement Parameters.................... 102
History ............................................................. 104
History Window .............................................. 134
Measurement Parameters Window .................. 130
Opening ........................................................... 125
Peak Integration Parameters ............................ 103
Peak Time Parameters Window ...................... 133
System Information Window........................... 127
Carrier Gas
Connecting....................................................... 313
Flow Rate........................................................... 90
Pressure.............................................................. 89
Purification Tube ............................................. 240
Purifier ............................................................. 314
Kit Specifications .................................... 296
Replacing CO2 Absorber ......................... 248
Supply Pressure ............................................... 314
Tubing Connections......................................... 314
Catalyst
Disposal ........................................................... 240
Filling................................................................. 36
Filling Rod .................................................. 37, 38
High Sensitivity ........................................ 37, 240
New.................................................................... 36
Regenerating ........................................... 238, 262
Replacing ......................................................... 239
Index-2
Setting Type ...................................................... 26
Standard............................................................. 36
TOC ................................................................... 37
TOC/TN............................................................. 39
Washing........................................................... 239
Ceramic Fiber ......................................................39, 42
Change Password ...................................................... 21
Dialog Box ........................................................ 21
Chemiluminescence Detector.................................. 259
CO2 Absorber .......................................................... 335
Disposal ........................................................... 242
Installation ...................................................52, 58
MSDS .............................................................. 335
Replacing........................................ 242, 248, 251
Used as NOx Absorber...................................... 59
Coaxial Needle ........................................... 28, 85, 320
Com Port.................................................................... 30
Combustion Tube
Connecting......................................................... 40
Filling with Catalyst ............................. 37, 38, 39
Installating H Type ............................................ 40
Installating N Type ............................................ 43
Replacing......................................................... 242
Replacing Ferrules........................................... 245
Washing........................................................... 242
Comment ................................................................... 22
Communication Settings ........................................... 30
Configured System, Deleting .................................... 33
Connecting Gas Tubing (TN Unit).......................... 330
Connection
8-Port Sampler................................................. 327
Cables .............................................................. 325
Two 8-Port Samplers....................................... 326
Consumable Parts ............................................304–307
Control Chart Wizard .............................................. 368
Control Charts ........................................ 208, 367–384
Comparing ....................................................... 379
Creating ........................................................... 368
Editing .....................................................377, 381
Excluding Samples From ........................377, 383
Exporting To ASCII File ................................. 383
Following Chart............................................... 372
Opening ........................................................... 373
Out Of Control Events..................................... 380
Printing ............................................................ 373
Recalculating Limits........................................ 377
Saving .............................................................. 373
Setting Number Format ................................... 382
Statistics........................................................... 378
Types ............................................................... 367
Control Checking .................................................... 200
Control Sample
Identifying ....................................................... 184
Inserting Into Sample Table ............................ 202
Selecting Type ................................................. 194
Template .......................................................... 193
Index
Control Sample Wizard
Analysis Parameters Window ..........................196
Control Checking Window ..............................200
Control Sample Type Window ........................194
Creating A Template........................................193
Failure Action Window....................................201
History Window...............................................199
Injection Parameters Window..........................197
Opening............................................................126
Parameter Source Window...............................195
Peak Time Parameters Window.......................198
System Information Window ...........................193
Cooler Drain Container..............................................48
Corrective Action
Eliminate Syringe Bubbles...............................281
Poor Reproducibility ........................................280
Poor Sample Injection......................................280
Corrosion Warning ......................................................x
Cover, Installation....................................................323
Creating
Calibration Curve.............................................126
Control Charts..................................................368
Control Sample Template ................................193
Method .............................................................135
Method Validation File.................................... 349
Sample Table ...................................................125
TC Calibration File ..........................................100
CV Max
Setting in Method Wizard................................138
Setting In Sample Wizard ................................188
D
Determinations, No. of............................136, 162, 186
Dialog Box
Change Password...............................................21
Dilution Water
Checking ..........................................................236
Preparing............................................................50
Display Settings
Floating Point Number Formats ......................216
Notification Bar Settings .................................215
Table Settings ..................................................214
Disposal
Catalyst ............................................................240
CO2 Absorber ..................................................242
Drain Tank, Installation ...........................................323
Drain Tubing, Connecting .......................................316
Drain Vessel Water, Checking.................................236
Data
Deleting............................................................158
Exporting to Database......................................148
Importing from ASCII .....................................159
Recalculating....................................................158
Replacing .........................................................157
Database, Exporting Data to ....................................148
Default Measurement Parameters ..................... 87, 212
Default Measurement Parameters Dialog Box...........98
Deleting
All Sample Table Data.....................................158
Configured System.............................................33
Selected Sample Table Data ............................159
Description, System .............................................. 7–18
Detector
Chemiluminescence .........................................259
Viewing Status .................................................203
E
Edit Menu, Sample Table Editor..............................156
Editing
Calibration Point Parameters ...........................132
Control Charts ......................................... 377, 381
Method Validation File ....................................356
Sample Table....................................................156
Electric Shock Warning ........................................... viii
Ending Measurement ...............................................120
Error Messages................................................ 270–274
Excluding
Data from Sample Table ..................................158
Injections from Calculations............................158
Samples From Control Charts................. 377, 383
Exporting
Control Charts..................................................383
Data to ASCII File ...........................................146
Data to Database ..............................................148
Method Validation Data...................................363
F
File Menu, Sample Table Editor ..............................125
Flow charts, Troubleshooting ..................................274
Flow Diagram
TOC-VCPH .........................................................11
TOC-VCPH+POC OPTION ..................................12
TOC-VCPH+TNM-1...........................................12
TOC-VCPN .........................................................13
TOC-VCPN+TNM-1...........................................13
Flow Diagrams.................................................... 11–13
Flow Line
Replacing Content............................................263
Replacing Parts and Slider.................................54
Residue Removal .............................................263
Setting Washes in Software ...............................86
Washing ...........................................................264
Index-3
Index
Flow Rate
Carrier Gas......................................................... 90
Ozone Source..................................................... 91
Sparge Gas ......................................................... 53
Sparge Gas, Wet Chemical .............................. 269
Front View
8-Port Sampler................................................... 15
Autosampler ...................................................... 14
TOC-V................................................................. 8
Furnace ...................................................................... 90
Power................................................................. 90
Temperature.................................................27, 84
G
Ground, Connecting ................................................ 312
Grounding........................................................312, 328
Grubb Test, See Outlier Test
General Information Window.................................. 125
General Measurement Parameters ...................... 83–88
Graph, in Sample Window ...................................... 167
H
Halogen Scrubber
MSDS .............................................................. 337
Replacing ......................................................... 243
High Purity Air Cylinder ................................ 242, 313
High Sensitivity
Analysis ............................................................. 63
Catalyst .............................................37, 240, 339
Combustion Tube .............................................. 40
Using 8-Port Sampler ........................................ 82
High Temperature Warning.......................................vii
History Log
Calibration ....................................................... 134
Control Sample................................................ 199
Instrument.......................................................... 31
Method............................................................. 142
History Settings, Maintenance .................................. 88
Humidifier
Checking Water Level..................................... 237
Filling with Water ............................................. 49
Hydrochloric acid .................................................... 333
I
IC ............................................................................. 285
Analysis Preparation.......................................... 56
Injection Port Septum ...................................... 226
Principles ......................................................... 285
Reaction Solution ..................................... 57, 249
Reaction Solution Pump .................................. 250
Reaction Solution Regeneration .........27, 84, 262
Removal Pretreatment ....................................... 68
Standard Solution .............................................. 61
Injection Parameters
Control Sample ................................................ 197
Method............................................................. 138
Sample ............................................................. 188
Injection Port Septum, Replacing ............................ 226
Injection Table, in Sample Window ........................ 168
Injection Volume, Setting............................... 138, 188
Injury Warning ........................................................... ix
Inorganic Carbon, See IC
Insert Menu, Sample Table Editor........................... 181
Inside Front View
TN ...................................................................... 17
TOC-V ............................................................... 10
Inside Top View
TOC-V ............................................................... 11
Inspection
Daily ....................................................... 236–237
Periodic ................................................... 238–251
Index-4
Installation
8-Port Sampler................................................. 325
Autosampler .................................................... 317
Cover ....................................................... 323
Drain Tank............................................... 323
Needle, Coaxial ....................................... 322
Needle, Sample........................................ 321
Positioning............................................... 317
Rinse Bottle ............................................. 323
Shipping Screw........................................ 317
Turntable ................................................. 323
Vial Rack ...........................................74, 323
CO2 Absorber ..............................................52, 58
Combustion Tube
High Sensitivity......................................... 40
N Type....................................................... 43
Manual Injection Kit ....................................... 219
Preparation....................................................... 310
Procedure......................................................... 312
Site................................................................... 310
Suspended Solids Kit......................................... 54
Syringe............................................................... 45
TN Unit............................................................ 328
TOC-V.....................................................310–332
Index
Instrument
Auto Restart .....................................................121
Background Monitor ........................................203
Connecting And Disconnecting .......................205
Detector Status .................................................203
Effects of Acid, Base, and Salt ..........................71
History Log ........................................................31
Maintenance .....................................................261
Menu, Sample Table Editor .............................203
Operation................................................... 35–233
Overview......................................................... 1–5
Power .................................................................89
Setup............................................................ 23–33
Shut Down Procedure ......................................120
Standby Window..............................................206
Starting ...................................................... 89, 207
Viewing Properties.............................................32
Instrument Properties Dialog Box..............................32
Instrument Setup Wizard
ASI Window ............................................... 28, 95
Auto Regeneration of IC Solution .....................27
Autosampler Parameters ....................................28
Buzzer ................................................................27
Cell Length ........................................................26
Communication Window...................................30
Configuration .....................................................24
Furnace Temperature .........................................27
History Log ........................................................31
Needle ................................................................28
Options Window ......................................... 24, 94
Oxidation Method ..............................................24
Ready Status Check ...........................................27
SSM Window.....................................................29
System Information Window...................... 23, 94
TOC Window.....................................................26
Tubing Diameter ................................................26
Introduction.................................................................iii
System Administration ...................................... 20
L
Left Side View
TOC-V .................................................................9
Lithium hydroxide, MSDS ......................................336
M
Maintenance .................................................... 235–281
8-Port Sampler ........................................ 254–255
Autosampler ............................................ 252–253
Chemiluminescence Detector ..........................259
Daily Inspection ...................................... 236–237
Gas Sample Analysis .......................................232
History..............................................................269
History Settings..................................................88
Log ...................................................................269
Manual Injection Kit ........................................226
Mechanical Check............................................265
Menu ................................................................261
Parts......................................................... 308–309
Periodic Inspection.................................. 238–251
Software-Controlled................................ 261–269
TN ........................................................... 256–260
Warning Message Limits ...................................88
Manual Contents Overview .........................................v
Manual Injection Kit ................................................296
Analysis............................................................219
Calibration........................................................221
Installation........................................................219
Maintenance .....................................................226
Specifications ...................................................296
Material Safety Data Sheets, See MSDS
Measurment
8-Port Sampler ...................................................80
Mechanical Check....................................................265
Method
Creating New ...................................................135
Viewing Properties ..........................................161
Method Properties
Common Tab ...................................................161
History Tab ......................................................166
NPOC and POC Tabs ......................................165
Parameter Tab ..................................................162
TC Tab .............................................................163
TN Tab.............................................................165
Method Validation ..................................208, 347–365
According to DIN ................................... 347, 364
Creating New File............................................349
Editing File ......................................................356
Exporting Data To ASCII ................................363
Main Window ..................................................348
Opening File ....................................................350
Printing File .....................................................351
Saving File .......................................................351
Setting Number Display Format ......................362
Viewing Parameters.........................................359
Index-5
Index
MSDS ..............................................................333–345
CO2 Absorber .................................................. 335
Halogen Scrubber ............................................ 337
High Sensitivity Catalyst................................. 339
Hydrochloric acid ............................................ 333
Lithium hydroxide........................................... 336
Normal Sensitivity Catalyst............................. 340
Phosphoric acid ............................................... 334
Potassium hydrogen phthalate......................... 344
Potassium nitrate ............................................. 341
Quartz Wool .................................................... 338
Sodium bicarbonate......................................... 342
Sodium carbonate ............................................ 343
Water ............................................................... 345
Multiple Injections ................................. 129, 139, 189
Multi-Point Calibration Curve................................. 290
Method Wizard
Acid Addition Volume .................................... 139
Analysis Information ....................................... 136
Auto Dilution ................................................... 139
Calibration Curve ............................................ 137
Creating New Method ..................................... 135
CV Max ........................................................... 138
Determinations................................................. 136
History Log...................................................... 142
Injection Parameters ........................................ 138
Injection Volume ............................................. 138
Multiple Injections........................................... 139
Number of Injections ....................................... 138
Opening ........................................................... 126
Peak Integration Parameters ............................ 140
SD Max............................................................ 138
System Information ......................................... 135
Using Blank Check Area ................................. 139
USP/EP ............................................................ 141
N
Notation Conventions................................................. vi
Notification Bar ...............................................124, 215
NOx Absorber
Connecting......................................................... 59
Replacement .................................................... 260
Using a CO2 Absorber....................................... 59
NPOC
Acid Addition .................................................... 76
Analysis ............................................................. 76
Principles .................................................286, 288
Number of Injections.......................................138, 188
Needle
Change ............................................................. 268
Coaxial........................................................ 28, 85
Coaxial+Sparge .......................................... 28, 85
Installation, Coaxial......................................... 322
Installation, Sample ......................................... 321
Rinse .................................................................. 85
Rinse after Acid Addition.................................. 86
Sample ........................................................ 28, 85
Sample+Sparge........................................... 28, 85
Setting in Software ..................................... 28, 85
Types ..................................................28, 85, 320
O
OCT-1/2, See 8-Port Sampler
Opening
Calibration Curve Wizard................................ 125
Control Sample Wizard ................................... 126
Method Validation File.................................... 350
Method Wizard ................................................ 126
Sample Group Wizard ..................................... 181
Sample Table ....................................96, 125, 143
Sample Wizard ................................................ 185
Sparge Gas Valve ............................................ 269
Options Menu, Sample Table Editor ....................... 210
Outlier Test.............................................................. 169
Oxidation Method, Selecting..................................... 24
Ozone
Connecting Source .......................................... 329
Generator Replacement ................................... 260
Generator, Low Air Supply Safety.................. 331
Generator, Source Air Pressure ....................... 330
Source Airflow Rate .......................................... 91
Treatment Unit ................................................ 256
P
Page Setup
Calibrations Tab .............................................. 152
Header Tab ...................................................... 153
Instrument Tab................................................. 152
Miscellaneous Tab ........................................... 154
Samples Tab .................................................... 153
Index-6
Parameter Source..................................................... 185
Parameter Table, in Sample Window...................... 167
Index
Parts
Precautions...................................................................3
Gas Sample Analysis .......................................227
High Sensitivity Analysis ..................................63
Preparation
Acid....................................................................51
Analysis ...................................................... 36–82
Dilution Water ...................................................50
High Sensitivity Analysis ........................... 63, 65
Manual Injection Analysis ...............................219
Sample ..................................................63, 72–79
Standard Solution...............................................60
TN Analysis .......................................................59
Pressure
Ozone Generator Source Air............................330
Principles
IC .....................................................................285
NPOC...................................................... 286, 288
Of Analysis ............................................. 284–288
POC..................................................................287
POC+NPOC.....................................................288
TN ....................................................................288
TOC ................................................................. 284
Print
Control Charts..................................................373
Method Validation File.................................... 351
Options.............................................................151
Page Setup........................................................ 152
Preview, Report ...............................................151
Preview, Table .................................................150
Sample Report..................................................150
Sample Table ...................................................149
Product Warranty........................................................iv
Purgeable Organic Carbon, See POC
Consumable
ASI-V .......................................................306
Carrier Gas Purifier Kit............................307
TNM-1 .....................................................307
TOC-VCPH ...............................................304
TOC-VCPN ...............................................305
Maintenance
ASI-V .......................................................308
Manual Injection Kit ................................309
TOC-VCPH ...............................................308
TOC-VCPN ...............................................308
Peak
Area..................................................................289
Integration Parameters ...........133, 140, 190, 198
Shape................................................................289
Start Delay........................................................140
Total Integration Time .....................................140
Phosphoric acid ........................................................334
Plunger Tip Backlash ...............................................281
POC
Analysis Preparation ..........................................58
kit .....................................................................296
Principles..........................................................287
Standard Solution...............................................61
POC+NPOC Principles ............................................288
Post Sale Service.........................................................iv
Potassium hydrogen phthalate, MSDS.....................344
Potassium nitrate, MSDS .........................................341
Power
Furnace...............................................................90
Instrument ..........................................................89
TN ......................................................................84
Power Supply
Changing Voltage ............................................313
Connecting .............................................. 312, 328
Q
Quartz Wool.........................................37, 39, 58, 338
R
Ready Status Check ............................................ 27, 84
Rear View
8-Port Sampler ...................................................15
Autosampler .......................................................14
TN ......................................................................18
TOC-V .................................................................9
Recalculating
All Sample Table Data.....................................158
Control Chart Limits ........................................377
Selected Sample Table Data ............................158
Reference Information .................................... 283–345
Regenerating
Catalyst ................................................... 238, 262
IC Solution................................................ 27, 262
Replacing Sample Table Data..................................157
Replacing the NOx Absorber ...................................260
Residue Removal .....................................................263
Right Side View, TOC-V.............................................8
Rinse
Bottle....................................................... 252, 323
Needle ................................................................85
Needle, After Acid Addition..............................86
Pump Head.......................................................253
Index-7
Index
S
Salt, Effect on Instrument .......................................... 71
Sample
Alkaline ............................................................. 71
Catcher............................................................. 252
Container ........................................................... 80
Containing Acid................................................. 71
Containing High IC Levels................................ 38
Containing Salt .................................................. 71
Group ............................................................... 181
High Sensitivity .......................................... 63, 65
Loading .............................................................. 80
Manual Injection.............................................. 223
Needle .................................................28, 85, 320
Preparation............................................63, 72–79
Report, Printing ............................................... 150
Suspended Solids ............................................... 69
Sample Group Wizard
Calibration Curve ............................................ 183
Controls ........................................................... 184
Measurement Parameters................................. 182
Opening ........................................................... 181
Parameter Source ............................................. 181
Sample Table Editor ....................................... 122–218
Auto Restart ..................................................... 121
Background Monitor........................................ 203
Closing a File................................................... 144
Connecting The Instrument ............................. 205
Creating New Sample Table..................... 98, 125
Deleting All Data............................................. 158
Deleting Selected Data .................................... 159
Directories ....................................................... 217
Edit Menu ........................................................ 156
Editing Rows and Cells ................................... 156
Excluding Data ................................................ 158
Exiting ............................................................. 155
Exporting Data to ASCII ................................. 146
Exporting Data to Database ............................. 148
File Menu......................................................... 125
Finding Cell Content ....................................... 157
General Information Window.......................... 125
Help Menu ....................................................... 218
Importing Data from ASCII ............................ 159
Insert Menu...................................................... 181
Inserting Calibration Curve ............................. 126
Inserting Control Samples ............................... 193
Inserting Sample Group................................... 181
Inserting Samples ............................................ 185
Instrument Menu.............................................. 203
Notification Bar ...................................... 124, 215
Opening File .................................................... 143
Options Menu .................................................. 210
Outlier Test ...................................................... 169
Overview ......................................................... 122
Page Setup Options.......................................... 152
Previewing Sample Report .............................. 151
Previewing Sample Table ................................ 150
Printing Options............................................... 151
Printing Sample Report ................................... 150
Index-8
Printing Sample Table ..................................... 149
Recalculating Data .......................................... 158
Replacing Data ................................................ 157
Reversing Last Action ..................................... 156
Sample Window ......................................114, 167
Saving .............................................................. 144
Saving As ........................................................ 145
Searching for Text ........................................... 157
Sequence Window........................................... 205
Setting Vial Position................................106, 179
Sparging/Acid Addition Window.................... 106
Standby Window ............................................. 206
Starting Instrument .......................................... 207
Status Bar ................................................124, 178
Stopping the Instrument .................................. 207
Toolbar ....................................................122, 178
Toolbar, Customize ......................................... 177
View Menu ...................................................... 160
Viewing Calibration Curve .....................160, 170
Viewing Cell Properties .................................. 170
Viewing Data in Real Time............................. 167
Viewing Method Properties............................. 161
Viewing Vial Positions.................................... 179
Window Menu ................................................. 218
Sample Window ...................................................... 114
Graph ............................................................... 167
Injection Table................................................. 168
Parameter Table............................................... 167
Sample Wizard
Acid Addition .................................................. 189
Analysis Information Window ........................ 186
Auto Dilution................................................... 189
Calibration Curve ............................................ 191
Calibration Curve Window ............................. 187
CV Max ........................................................... 188
Determinations ................................................ 186
Injection Parameters ........................................ 191
Injection Parameters Window ......................... 188
Injection Volume ............................................. 188
Multiple Injections .......................................... 189
Number of Injections....................................... 188
Parameter Source Window .............................. 185
Peak Time Parameters Window ...................... 190
SD Max............................................................ 188
Units ................................................................ 188
USP/EP Window ............................................. 192
Screen Lock ............................................................... 20
SD Max............................................................138, 188
Sequence Window ................................................... 205
Shipping Screw........................................................ 317
Sliding Sample Injector ........................................... 245
Sodium bicarbonate, MSDS .................................... 342
Sodium carbonate, MSDS ....................................... 343
Index
Software
Connecting To Instrument ...............................205
Creating New Method......................................135
Maintenance Functions ....................................261
Maintenance History Settings ............................88
Module .............................................................122
Overview..................................................... 19–33
Ready Status Check ...........................................84
Setting Measurement Parameters................ 83, 87
Setting up a Sequence ......................................125
Source Air (TN Unit)
Pressure ............................................................330
Sparge
Gas Flow Rate....................................................53
Gas Flow Rate, Wet Chemical.........................269
Gas Valve.........................................................269
Needle ....................................................... 28, 320
NPOC Analysis ..................................................77
Time, Setting....................................................139
Sparging/Acid Addition Window ............................106
Special Accessories..................................................303
Specifications .................................................. 294–297
Autosampler .....................................................295
Carrier Gas Purifier Kit....................................296
Gas Sample Injection Kit .................................296
Manual Injection Kit ........................................296
POC Kit............................................................296
TN ....................................................................295
TOC-V .............................................................294
Standard Accessories
ASI ...................................................................299
Manual Injection Kit ........................................301
POC Kit............................................................301
TN ....................................................................301
TOC-VCPH/CPN ................................................298
Standard Solution.......................................................60
Analysis ...........................................................100
High Sensitivity .................................................64
Preparing............................................................60
Sparging ...........................................................292
Storing................................................................62
Standby Window............................................. 120, 206
Starting The Instrument ...........................................207
Starting the Instrument...............................................89
Status Bar........................................................ 124, 178
Stirrer .................................................................. 78, 86
Stopping the Instrument
Halt...................................................................207
Stop Finish Current..........................................207
Stop Peak Stop .................................................207
Suspended Solids ................................................ 54, 69
Syringe
Changing................................................. 226, 268
Installation .........................................................45
Manual Injection Kit........................................226
Plunger Tip ......................................................244
Plunger Tip Backlash.......................................281
Replacing ...........................................................45
Residue Removal .............................................263
Washing with Sample .....................138, 188, 212
Washing with Standard........................... 130, 172
Syringe Pump
8-Port Valve Rotor...........................................246
Zero Point Detection..........................................47
System Administration
Add Event Log...................................................22
Change Password...............................................21
Introduction........................................................20
Screen Lock .......................................................20
System Blank ...........................................................291
System Description ............................................... 7–18
System Information Window
Instrument Setup Wizard ...................................94
T
TC
Analysis, New Catalyst ......................................36
Blank Check.............................................. 66, 269
Principles..........................................................284
Standard Solution...............................................60
TC/TN, Standard Solution .........................................61
TC-IC .......................................................................288
Technical Information..................................... 289–293
Time, Sparge ............................................................139
TN
Analysis Preparation ..........................................59
Analysis, New Catalyst...................................... 36
Connecting Ozone Source Air .........................329
Front and Right Side Views...............................16
Gas Exhaust Tubing.........................................332
Grounding ........................................................ 328
Inside Front View ..............................................17
Installation .......................................................328
Maintenance............................................ 256–260
Ozone Source Airflow Rate...............................91
Power Source .....................................................84
Power Supply...................................................328
Principles .........................................................288
Rear View .......................................................... 18
Specifications...................................................295
Standard Solution...............................................61
Turning On.........................................................91
Unit ..................................................................295
Index-9
Index
TN Unit
Gas Tubing Connection ................................... 330
TOC
Principles ......................................................... 284
Setting Parameters ............................................. 83
Setting Parameters in Software.......................... 26
TOC window of the Instrument Setup Wizard .......... 94
TOC/TN, Catalyst...................................................... 39
TOC-Control V
Administration Tool .......................................... 21
Administrator Window ...................................... 21
TOC-V
Construction......................................................... 8
Front View ........................................................... 8
Grounding ........................................................ 312
High Sensitivity Catalyst ................................... 37
Inside Front View .............................................. 10
Inside Top View ................................................ 11
Installation .............................................. 310–332
Left Side View..................................................... 9
Rear View ............................................................ 9
Right Side View................................................... 8
Specifications................................................... 294
Standard Catalyst ............................................... 37
Troubleshooting...................................... 274–277
Toolbar, Sample Table Editor
Customizing..................................................... 177
Displaying ....................................................... 178
Functions ......................................................... 122
Total Carbon, See TC
Total Nitrogen, See TN
Total Organic Carbon, See TOC
Troubleshooting...............................................270–281
Autosampler ............................................278–280
Flow Charts ..................................................... 274
TOC-V.....................................................274–277
Tubing Diameter........................................................ 83
Turntable, Installation ............................................. 323
Tutorial ..............................................................92–119
Calibration Runs.............................................. 100
Configuring the Instrument ............................... 93
Connecting the Instrument ..........................96, 98
Creating a Sample Table ................................... 98
Evaluating Results........................................... 114
Measurement ................................................... 112
Printing Report ................................................ 117
Unknown Run.................................................. 108
U
Units....................... 87, 130, 138, 163, 171, 188, 212
USP/EP ............................................................141, 192
V
Vial
View Menu, Sample Table Editor ........................... 160
Viewing Measurement Data in Real Time .............. 167
Filling................................................................. 72
Placing in Rack .................................................. 74
Rack Installation ....................................... 74, 323
Sealing ............................................................... 73
Setting Position....................................... 106, 179
Types ................................................................. 72
W
Water
Dilution............................................................ 236
Drain Vessel .................................................... 236
Humidifier ....................................................... 237
MSDS .............................................................. 345
Pure.................................................................... 50
Supply to Cooler Drain Container..................... 48
Zero ................................................................... 60
Warning
Corrosion ............................................................. x
Electric Shock...................................................viii
High Temperature..............................................vii
Injury .................................................................. ix
Warning Labels..........................................................vii
Warning Message, Maintenance................................ 88
Warranty ..................................................................... iv
Washing
Catalyst ............................................................ 239
Combustion Tube ............................................ 242
Flow Lines ................................................ 86, 264
Syringe with Sample.......................138, 188, 212
Syringe with Standard ............................ 130, 172
Z
Zero Point Detection......................................... 47, 261
Zero Shift ........................................................ 129, 172
Index-10
Zero Water................................................................. 60
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