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DuMaster D-480
Operation Manual
Imprint
Product Identification:
Operation Manual (original) DuMaster
D-480
115936
2 6
C
en
Publication date:
06
.201
6
BÜCHI Labortechnik AG
Meierseggstrasse 40
Postfach
CH9230 Flawil 1
EMail: [email protected]
BUCHI reserves the right to make changes to the manual as deemed necessary in the light of experi ence; especially in respect to structure, illustrations and technical detail.
This manual is copyright. Information from it may not be reproduced, distributed, or used for competitive purposes, nor made available to third parties. The manufacture of any component with the aid of this manual without prior written agreement is also prohibited.
Copyright Note
Copyright © BÜCHI Labortechnik AG
All rights reserved
Windows ® , Windows XP ® und Windows 7 ® are trademarks of Microsoft Corporation.
MS-Excel ® und MS-Access ® are trademarks of Microsoft Corporation.
3
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
Contents
Contents
CHAPTER 1 General 13
About this document .................................................................................................................................... 14
Display conventions .................................................................................................................................... 15
General information on the operating instructions ....................................................................................... 15
CHAPTER 2 Basic security settings 17
Working with the operating instructions ....................................................................................................... 18
Representation of safety instructions .......................................................................................................... 18
Instructions for disposal of consumables ..................................................................................................... 18
Intended use of the instrument .................................................................................................................... 19
Warning: residual risks ................................................................................................................................ 19
Safety devices in the analyzer ..................................................................................................................... 20
Warning signs on the analyzer .................................................................................................................... 22
Warning: changes to the instrument ............................................................................................................ 23
Warning: unsuitable spare parts and consumables ..................................................................................... 23
Required user knowledge and skills ............................................................................................................ 23
Required personal safety equipment ........................................................................................................... 24
Warning notes during operation .................................................................................................................. 24
CHAPTER 3 Product description 31
Analytical characteristics and technical specifications ................................................................................. 32
Analytical characteristics .................................................................................................................. 33
Technical specifications ................................................................................................................... 33
Instrument design ........................................................................................................................................ 35
Front view ........................................................................................................................................ 36
Rear view ......................................................................................................................................... 37
Right side view ................................................................................................................................. 37
Left side view ................................................................................................................................... 38
Top view ........................................................................................................................................... 39
Peripherals and their function .......................................................................................................... 40
CHAPTER 4 Understanding the instrument and planning its use 41
Layout and mode of functioning .................................................................................................................. 42
Functional units ................................................................................................................................ 43
The thermal conductivity detector (TCD) .......................................................................................... 45
Processes in the instrument during a measurement ................................................................................... 46
Sample insertion and initiation of measurement .............................................................................. 47
Substance digestion and preparation of the reaction gas mixture .................................................... 47
Detection of measuring components and evaluation of the measuring signal .................................. 48
Formulas for determining element concentration of analysis samples (Solids) ................................ 48
Basic facts about working with the instrument ............................................................................................. 49
Instrument equipment ...................................................................................................................... 50
Background knowledge required for calibration ............................................................................... 51
Calibration curve calculation method criteria .................................................................................... 52
Calibration formulae ......................................................................................................................... 54
Routine measuring work .................................................................................................................. 55
Formulae for blank value determination and compensation ............................................................. 56
Formula for determining the daily factor ........................................................................................... 57
Understanding the operating software ......................................................................................................... 58
Basic functions of the operating software ......................................................................................... 59
Software user interface .................................................................................................................... 60
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
5
Contents 6
Sample view ..................................................................................................................................... 61
Combi view ...................................................................................................................................... 63
Status view ....................................................................................................................................... 66
Right mouse button function ............................................................................................................ 67
Data administration and data security ......................................................................................................... 69
Laboratory information and management system (LIMS) ................................................................ 70
Conditions for operating the LIMS .................................................................................................... 70
21 CFR Part 11 functionality ............................................................................................................ 71
Versioning ........................................................................................................................................ 72
Linking the analyzer and software .................................................................................................... 72
CHAPTER 5 Work performed by the system administrator 73
Installing and updating the software ............................................................................................................ 74
Configure analyzer ...................................................................................................................................... 75
What can you modify in the configuration? ...................................................................................... 76
Defining logon timeout ..................................................................................................................... 76
Creating new sections ...................................................................................................................... 77
Defining LIMS export settings ..................................................................................................................... 78
LIMS export settings ........................................................................................................................ 79
Setting up user administration ..................................................................................................................... 80
User administration .......................................................................................................................... 81
Recommendations for user administration ....................................................................................... 81
Granting authorizations .................................................................................................................... 81
Defining interfaces ....................................................................................................................................... 83
Defining the analyzer / PC interface ................................................................................................. 84
Defining the LIMS / PC interface ...................................................................................................... 84
Defining the balance / PC interface .................................................................................................. 85
Editing analysis data ................................................................................................................................... 86
When does it make sense to edit analysis data? ............................................................................. 87
Limits for modifying analysis data .................................................................................................... 87
Consequences of modifying analysis data ....................................................................................... 87
Performing checks ....................................................................................................................................... 88
Checking documents for authenticity ............................................................................................... 89
Signing documents........................................................................................................................... 89
Viewing the logbook ......................................................................................................................... 90
Working with the database .......................................................................................................................... 91
Database .......................................................................................................................................... 92
Administrative work on the database ............................................................................................... 92
Defining the autoexport directory ..................................................................................................... 93
Database backup ............................................................................................................................. 93
Starting the database backup .......................................................................................................... 94
Reorganize database ....................................................................................................................... 94
Reloading an old database file ......................................................................................................... 95
Ways of optimizing the use of the analyzer ................................................................................................. 96
Optimizing basic instrument settings ................................................................................................ 97
Optimizing sample data editing ........................................................................................................ 97
"Balance" weighing data input program ........................................................................................... 98
Optimizing data evaluation ............................................................................................................... 99
Performing other administrator tasks ......................................................................................................... 100
Modifying the registration ............................................................................................................... 101
Printer setup ................................................................................................................................... 101
CHAPTER 6 Starting up and shutting down the instrument 103
Setting up and starting up the instrument .................................................................................................. 104
Rules for first-time start-up ............................................................................................................. 105
Instructions for operating the furnace ............................................................................................. 105
Installation site requirements ......................................................................................................... 105
Gases and chemicals to be provided ............................................................................................. 106
Start-up .......................................................................................................................................... 107
Connecting peripherals .................................................................................................................. 108
Connecting supply lines and waste gas lines ................................................................................. 109
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
Contents 7
Removing the transport protection ................................................................................................. 110
Switching on ................................................................................................................................... 112
Default instrument settings ............................................................................................................. 112
Heating up the furnace ................................................................................................................... 113
Shutting down the instrument .................................................................................................................... 114
Shutting the instrument down for short measuring breaks (standby) ............................................. 115
Shutting the instrument down for long measuring breaks (switching off) ....................................... 115
CHAPTER 7 Using the instrument 117
Measurement settings ............................................................................................................................... 118
Defining keywords for blank and conditioning samples .................................................................. 119
Viewing list of defined factor, monitor and standard samples ........................................................ 119
Defining custom standard substances ........................................................................................... 119
Defining standard substances as factor and monitor samples ....................................................... 120
Defining standard substances as calibration samples.................................................................... 120
Specifying the computation method for blank value and daily factor .............................................. 121
Enabling/disabling acoustic signals ................................................................................................ 121
Configuring error handling .............................................................................................................. 122
Preparing samples .................................................................................................................................... 123
Sample preparation instructions ..................................................................................................... 124
Determining sample weight ............................................................................................................ 124
Showing or hiding the weight window ............................................................................................ 125
Packing samples ............................................................................................................................ 125
Preparing measurement work ................................................................................................................... 127
Software usage rules ..................................................................................................................... 128
Starting the operating software ...................................................................................................... 128
Showing or hiding the toolbar ......................................................................................................... 128
Waking up the instrument .............................................................................................................. 128
Viewing method settings ................................................................................................................ 129
Defining custom methods ............................................................................................................... 129
Defining the Kjeldahl factor ............................................................................................................ 130
Copy methods ................................................................................................................................ 130
Settings for sample input ................................................................................................................ 131
Importing weighing data ................................................................................................................. 131
Prioritizing urgent samples ............................................................................................................. 132
Optimizing sleep and wake-up behavior ........................................................................................ 132
Performing measurement work ................................................................................................................. 134
Values for oxygen dosing ............................................................................................................... 135
Performing measurements ............................................................................................................. 136
Performing routine measuring work ............................................................................................... 138
Checklist for blank value / conditioning and daily factor measurements ........................................ 139
Checklist for real sample measurement ......................................................................................... 140
Types of blank value determination and their settings ................................................................... 141
Determining blank values ............................................................................................................... 141
Determining the daily factor ........................................................................................................... 142
Stopping continuous analysis ......................................................................................................... 144
Preparing measuring data for evaluation ................................................................................................... 146
Configuring the sample view .......................................................................................................... 147
Determine measuring units and number of decimal places. ........................................................... 147
Saving the sample view ................................................................................................................. 148
Loading a sample view ................................................................................................................... 148
Configure statistics view ................................................................................................................. 148
Generating statistical data .............................................................................................................. 148
Formulae for generating statistical data ......................................................................................... 149
Manual peak integration ................................................................................................................. 150
Configuring the graph view ............................................................................................................ 154
Setting the size of the graph .......................................................................................................... 154
Configure report ............................................................................................................................. 155
Display print preview ...................................................................................................................... 155
Data backup and printing ............................................................................................................... 156
Overview of export and import file formats ..................................................................................... 157
Exporting analysis data to MS Excel and viewing .......................................................................... 157
Exporting LIMS data....................................................................................................................... 158
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
Contents 8
Working with documents ........................................................................................................................... 159
Creating new documents ............................................................................................................... 160
Editing documents.......................................................................................................................... 160
Deleting documents ....................................................................................................................... 161
Finding documents ......................................................................................................................... 161
Copying documents via the clipboard ............................................................................................ 162
Importing documents ...................................................................................................................... 163
Signing documents......................................................................................................................... 163
Checking documents for authenticity ............................................................................................. 164
CHAPTER 8 Maintaining the instrument 165
Important information about maintenance ................................................................................................. 166
Maintenance work to be performed by the customer ..................................................................... 167
Viewing the status of maintenance intervals .................................................................................. 168
Defining maintenance intervals in the software .............................................................................. 168
Installing used tubes ...................................................................................................................... 169
Preparing and following up maintenance work ............................................................................... 169
Conditioning newly installed tubes ................................................................................................. 170
Performing the calibration ......................................................................................................................... 173
Viewing list of defined factor, monitor and standard samples ........................................................ 174
Defining standard substances ........................................................................................................ 174
Viewing calibration coefficients ...................................................................................................... 175
Optimizing instrument condition for calibration ............................................................................... 175
Performing the calibration .............................................................................................................. 175
Assessing the calibration curves .................................................................................................... 179
Calibration tables....................................................................................................................................... 182
Calibration table for nitrogen calibration ......................................................................................... 183
Replacing the ash crucible ........................................................................................................................ 184
Purpose and frequency of crucible replacement ............................................................................ 185
Removing the ash crucible ............................................................................................................. 185
Installing the ash crucible ............................................................................................................... 188
Refill the Regainer ..................................................................................................................................... 190
Purpose and frequency of refilling of the Regainer ........................................................................ 191
Refill the Regainer.......................................................................................................................... 191
Replacing sealing elements ...................................................................................................................... 194
When to replace sealing elements ................................................................................................. 195
Removing sealing elements from grooves ..................................................................................... 196
Ball valve maintenance ............................................................................................................................. 197
Removing and dismantling the ball valve ....................................................................................... 198
Cleaning, assembling and installing the ball valve. ........................................................................ 202
Maintaining the Ni flap and the O2 lance ................................................................................................... 206
Purpose and frequency of maintaining the Ni flap and O2 lance ................................................... 207
Removing and cleaning the Ni flap ................................................................................................ 207
Installing the Ni flap ........................................................................................................................ 209
Removing, cleaning and re-installing the O2 lance ........................................................................ 211
Removing, cleaning and installing the quartz glass bridge ........................................................................ 213
Removing the quartz glass bridge .................................................................................................. 214
Cleaning and installing the quartz glass bridge .............................................................................. 214
Removing, cleaning and installing the carousel ........................................................................................ 217
Removing, cleaning and installing the carousel ............................................................................. 218
Emptying and filling reaction tubes ............................................................................................................ 220
Emptying reaction tubes ................................................................................................................. 221
Filling the combustion tube ............................................................................................................ 221
Filling the post combustion tube ..................................................................................................... 223
Reductor replacing ......................................................................................................................... 224
Removing/installing and conditioning the reaction tubes ........................................................................... 225
Removing the reaction tubes from the furnace .............................................................................. 226
Installing reaction tubes in the furnace and conditioning ................................................................ 228
Filling, removing and installing the absorption and drying tubes ............................................................... 232
Filling the drying tubes ................................................................................................................... 233
Removing and installing the drying tubes ....................................................................................... 235
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
Contents 9
CHAPTER 9 Repairing the instrument 237
Interpreting PC error messages ................................................................................................................ 238
Performing a system test ........................................................................................................................... 239
Performing a leak test ............................................................................................................................... 240
Leak test procedure ................................................................................................................................... 241
Replacing fuses ......................................................................................................................................... 241
What to do after a computer crash ............................................................................................................ 245
Reacting to a power failure ........................................................................................................................ 245
Stopping continuous analysis .................................................................................................................... 248
Re-weighing after sample loss .................................................................................................................. 248
Changing the position of the carousel ....................................................................................................... 249
Export analysis data for support ................................................................................................................ 249
CHAPTER 10 Menu and dialog descriptions 251
Dialog descriptions key ............................................................................................................................. 252
File menu .................................................................................................................................................. 253
File > New (Command) .................................................................................................................. 254
Select document name (Dialog) ..................................................................................................... 254
Select version (Dialog) ................................................................................................................... 256
Save file as (Dialog) ....................................................................................................................... 257
File > Delete (Command) ............................................................................................................... 258
Comment modification (Dialog) ...................................................................................................... 258
Sign (Dialog) .................................................................................................................................. 259
Verify digital signature (Dialog) ...................................................................................................... 259
Export to LIMS (Dialog) .................................................................................................................. 260
Export peak graphics (Dialog) ........................................................................................................ 261
Configure report (Dialog) ................................................................................................................ 261
Print (Dialog) .................................................................................................................................. 263
Print preview (Dialog) ..................................................................................................................... 264
Printer setup (Dialog) ..................................................................................................................... 265
Open (Dialog) ................................................................................................................................. 266
Load balance file (Dialog) .............................................................................................................. 267
Configure backup (Dialog) ............................................................................................................. 267
Clean database (Dialog) ................................................................................................................ 269
Restore database (Dialog) ............................................................................................................. 269
Log in as (Dialog) ........................................................................................................................... 270
File > Logoff (Command) ............................................................................................................... 271
File > Exit (Command) ................................................................................................................... 271
File > Export/Import > Create Excel sheet (Command).................................................................. 271
Edit menu .................................................................................................................................................. 272
Edit > Undo (Command) ................................................................................................................ 273
Edit > Redo (Command) ................................................................................................................ 273
Edit > Cut (Command) ................................................................................................................... 273
Edit > Copy (Command) ................................................................................................................ 273
Edit > Paste (Command) ................................................................................................................ 274
Edit > Insert line (Command) ......................................................................................................... 274
Edit > Delete line (Command) ........................................................................................................ 274
Swap samples (Dialog) .................................................................................................................. 275
Edit > Modify (Command) .............................................................................................................. 275
Set stop tag (Dialog) ...................................................................................................................... 276
Select current sample (Dialog) ....................................................................................................... 276
Set current weighed sample (Dialog) ............................................................................................. 277
View menu ................................................................................................................................................ 278
View > Toggle (Command) ............................................................................................................ 279
Zoom in/out (Dialog) ....................................................................................................................... 279
Configure sample view (Dialog) ..................................................................................................... 279
Save sample pane (Dialog) ............................................................................................................ 280
Load sample pane (Dialog) ............................................................................................................ 281
Delete sample pane (Dialog) .......................................................................................................... 281
View > Gridview > Auto align (Command) ..................................................................................... 282
Configure graph view (Dialog) ........................................................................................................ 282
View > Graphic > Auto align (Command) ....................................................................................... 283
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
Contents 10
Configure statistics view (Dialog) ................................................................................................... 283
View > Statistic > Auto align (Command) ....................................................................................... 284
Select columns (Dialog) ................................................................................................................. 284
Column properties (Dialog) ............................................................................................................ 284
Weighing window (Dialog) .............................................................................................................. 285
System menu ............................................................................................................................................ 287
System > Auto run (Command) ...................................................................................................... 288
System > Single run (Command) ................................................................................................... 288
System > Stop (Command) ............................................................................................................ 288
System > Auto zero (Command) .................................................................................................... 289
Furnace switch off/on (Dialog) ....................................................................................................... 289
Initialize the instrument (Dialog) ..................................................................................................... 289
System > Wake up (Command) ..................................................................................................... 290
Feeding (Dialog)............................................................................................................................. 290
Adjust carousel position (Dialog) .................................................................................................... 290
Math menu ................................................................................................................................................ 292
Math > Blank values > Calculate (Command) ................................................................................ 293
Blank values (Dialog) ..................................................................................................................... 293
Math. > Factor (Command) ............................................................................................................ 294
Define type of peak (Dialog) ........................................................................................................... 294
Define peak start / end (Dialog) ..................................................................................................... 294
Area assignment (Dialog) ............................................................................................................... 295
Standard samples display (Dialog)................................................................................................. 296
Math. > Recalculate (Command) ................................................................................................... 297
Statistics menu .......................................................................................................................................... 298
Statistics > Via names (Command) ................................................................................................ 299
Statistics > Group (Command) ....................................................................................................... 299
Statistics > Sort group (Command) ................................................................................................ 299
Statistics > Delete group (Command) ............................................................................................ 299
Statistics > Clear statistic (Command) ........................................................................................... 299
Statistics > Include/Exclude sample (Command) ........................................................................... 300
Statistics > Include/Exclude value (Command) .............................................................................. 300
Statistics > Create Excel sheet (Command)................................................................................... 300
Calibration menu ....................................................................................................................................... 301
Calibration coefficients (Dialog) ..................................................................................................... 302
Configure calibration (Dialog) ......................................................................................................... 303
Specify lower and upper calibration range (Dialog) ........................................................................ 304
Calibration > Next sample (Command) .......................................................................................... 305
Calibration > Previous sample (Command).................................................................................... 305
Calibration > Next (Command) ....................................................................................................... 305
Calibration > Previous (Command) ................................................................................................ 305
Options menu ............................................................................................................................................ 306
Maintenance intervals (Dialog) ....................................................................................................... 307
Replace part (Dialog) ..................................................................................................................... 308
Adjust carousel (Dialog) ................................................................................................................. 309
Leak test (Dialog) ........................................................................................................................... 310
Leak test: Test phases (Dialog) ..................................................................................................... 311
System test (Dialog) ....................................................................................................................... 312
Error buffer (Dialog) ....................................................................................................................... 314
Error display (Dialog) ..................................................................................................................... 314
Options > Diagnostics > Baseline recording (Command) ............................................................... 315
Input options (Dialog) ..................................................................................................................... 315
Standard samples (Dialog) ............................................................................................................. 316
Keywords (Dialog) .......................................................................................................................... 317
Acoustic signals (Dialog) ................................................................................................................ 318
Configure Calculations (Dialog) ..................................................................................................... 318
LIMS settings (Dialog) .................................................................................................................... 319
Method (Dialog) ............................................................................................................................. 322
Monthly logbook (Dialog) ............................................................................................................... 323
Select period (Dialog) ..................................................................................................................... 324
Device configuration (Dialog) ......................................................................................................... 325
Error handling (Dialog) ................................................................................................................... 328
Sleep / wake-up function (Dialog) .................................................................................................. 329
Configure key value (Dialog) .......................................................................................................... 330
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
Contents 11
Windows menu .......................................................................................................................................... 332
Windows > Toolbar / Run-Bar (Command) .................................................................................... 333
Toolbar ........................................................................................................................................... 333
Windows > Recent sample (Command) ......................................................................................... 334
Windows > Status view (Command) .............................................................................................. 334
Windows > Default layout (Command) ........................................................................................... 334
Help menu ................................................................................................................................................. 335
Help > Content (Command) ........................................................................................................... 336
Help > Find (Command) ................................................................................................................. 336
Help > BÜCHI Labortechnik AG on the WEB (Command) ............................................................. 336
Product registration (Dialog) .......................................................................................................... 336
Help > About... (Command) ........................................................................................................... 337
CHAPTER 11 Appendix 339
Revision history ......................................................................................................................................... 340
Warranty .................................................................................................................................................... 341
Warranty of the overall instrument ................................................................................................. 342
Warranty on the furnace ................................................................................................................. 342
Accessories, spare parts and consumables .............................................................................................. 343
Smallest workable unit ................................................................................................................... 344
Required accessories ..................................................................................................................... 345
Optional accessories ...................................................................................................................... 346
Declaration of conformity ........................................................................................................................... 347
Declaration of conformity ............................................................................................................... 348
Index 349
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
C H A P T E R 1
General
Purpose
This chapter contains general topics of the document.
In this chapter
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
1 - General
About this document
Status of the operating instructions
The status of the operating instructions is: 16.10.2014.
Identification number
The operating instructions identification number is: 11593627.
Validity
The operating instructions are valid for all instruments as from serial number: 16144001.
Analyzer
The operating instructions describe the basis type of the instrument D-480.
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Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
1 - General 15
Display conventions
Before you start using this guide, it is important to understand the terms and typographical conventions used in the documentation. The following kinds of formatting in the text identify special information.
Formatting convention
Triangular bullet ( )
Special bold
Italics
CAPITALS
KEY+KEY
"Quotation marks"
{Symbolic name}
Type of information
Step by step procedure. You can follow these instructions to complete a specific task.
Items you must select, such as menu options (e. g.
File > New
), command buttons (e. g.
Cancel
), or common accentuation.
Used to emphasize the importance of an item or for variable expressions such as parameters.
Names of keys on the keyboard, for example, SHIFT, CTRL, or
ALT.
Key combinations for which the user must press and hold down one key and then press another, for example, CTRL+P, or
ALT+F4.
Denote amongst others the names of dialogs in the software, e. g. the "Replace part" dialog.
Denotes a symbolic name, e. g. {Element} stands for the corresponding name of an element.
General information on the operating instructions
Pictures
The instruments of BÜCHI Labortechnik AG underlie a permanent development and adjustment regarding the optimum parameter settings. This may lead to deviations in terms of picture display of the manual and the current instrument status which are not relevant for the understanding of the instrument operation.
The valid numbers of the parameter settings and/or variables can be found in the current text part.
Therefore, numbers in the pictures of software dialogs are mainly replaced by spaces or only reflect examples. They do not reflect the proper, recommended set values.
Reading aids
Subheadings are displayed in the left margin as reading aids. They sum up the content of the particular section and are useful for quick navigation.
Index
An index is given at the end of the operating instructions that helps you locate certain topics more easily. Index entries always refer to the first page of the section in which the index term is found.
Therefore, don't be confused if the index term does not appear on the first page but rather on one of the following pages.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
C H A P T E R 2
Basic security settings
Target group
Personnel working with the instrument.
Purpose
This section describes basic safety rules required to avoid risks for the user of the analyzer.
In this chapter
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
2 - Basic security settings 18
Working with the operating instructions
Operating the analyzer
Read the operating instructions thoroughly before performing work with the analyzer.
Storing the operating instructions
Store the operating instructions carefully and make sure the instructions are accessible for all relevant personnel.
Passing on the operating instructions
If you pass on the analyzer, always pass on the operating instructions, too.
Representation of safety instructions
Safety signs
This is a safety sign. Instructions with this sign contain warnings about risks of injury and even death.
These instructions must always be observed in order to avoid risks.
Risk levels
The safety instructions are categorized according to the following risk levels:
Risk level
Risk
Consequences
Death / serious injury (irreversible)
Probability high
Warning
Caution
Death / serious injury (irreversible)
Minor injury (reversible) medium medium
Caution Damage to property
Instructions for disposal of consumables
Rules possibly
Observe the following rules for disposal of consumables:
Dispose of the consumables according to the relevant disposal categories.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
2 - Basic security settings
Read the instructions on the individual chemicals in the safety data sheets. The risk notes for individual chemicals can be found in the R-Phrases. Safety advice can be found in the S-
Phrases.
Intended use of the instrument
Intended use
This section describes what the instrument is suitable for and what substances may be analyzed with it.
Description of the instrument
The elementary analyzer is an instrument for fully automatic and quantitative analysis of the element
N.
Suitable analysis samples
Only samples that can be decomposed in a controlled manner under the method-dependent combustion conditions are suitable for analysis.
Advice on difficult applications
You have the following ways of getting advice on difficult applications:
You will find useful tips in the "Application notes" on the provided CD.
You will find also the "Application notes" section on the www.buchi.com website.
Warning: residual risks
Hot components inside the instrument
During operation, the furnaces inside the instrument heat certain components to very high temperatures. Even after switching off the instrument, these components stay hot for long periods of time that you can suffer serious burns if working inappropriately inside the instrument.
Observe the relevant instructions exactly in order to avoid burns.
Live components inside the instrument
There are live parts (up to 230V) inside the instrument. When you are working on the electrical components, you may suffer electrocution if you do not work properly. Never bring liquids or leak-test spray in the vicinity of live components.
Observe the relevant instructions exactly in order to avoid injuries caused by electrocution.
Unsuitable consumables and spare parts
If you use consumables and spare parts of an unsuitable type and quality, you risk:
Injuries to the operating personnel
Damages to the instrument
Distortion of analysis results
loss of warranty.
Only use original spare parts and original consumables that you have purchased from BÜCHI
Labortechnik AG or authorized dealers.
Samples with potential risks
Samples to be analyzed may pose the following risks:
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Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
2 - Basic security settings 20
Contact with the substances may lead to chemical burns or poisoning.
Combustion analysis of larger quantities of the substance may lead to explosions.
These sample substances include:
Aggressive chemicals such as acids or alkaline solutions
Organic solvents
Explosives
Substances that develop toxic or explosive gas mixtures
You are obliged to protect yourself prior to contact with hazardous substances and to reduce the quantity of the substance to a safe amount.
You are also obliged to observe the safety instructions of the chemical manufacturer on the label of the bottle or in the safety data sheets. The safety data sheets contain risk information about a chemical in the R-Phrases and safety information in the S-Phrases.
Safety devices in the analyzer
Note
The analyzer may only be operated if all of the safety devices indicated in this section are in place and in working order.
Gas supply
Gas supply is only possible if the mains switch is switched on and the software is running.
Temperature monitoring
A temperature limiter automatically switches off the instrument in the event of excess temperature inside the instrument. All heating is monitored by an integrated microprocessor controller. All furnaces are automatically shut down in the event of the following malfunctions:
The heating fails to reach setpoint temperature within the set time.
A thermocouple is defective or displays an illegal value.
The set threshold temperature is exceeded.
Instrument casing
The instrument casing comprises the following, as seen from the top left in the picture:
Right side door
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
2 - Basic security settings
Front door
Left side door
Rear wall
Instrument cover.
The casing separates hot, live parts from the surroundings.
Protective earth conductor
The electrical components of the analyzer are grounded by a protective earth conductor:
21
The first protective earth conductor is located on the rear wall of the analyzer.
The second protective earth conductor is located outside the cover of the electrical area (arrow).
The third protective earth conductor is located intside the cover of the electrical area (arrow).
If the protective earth conductor connections need to be detached, they must be re-connected correctly when re-assembling.
Waste gas lines
The operator is obliged to connect waste gas lines if the national limits for toxic gases in workplace air are exceeded. The waste gas lines must discharge into the open or into an exhaust hood. The end of the waste gas lines must discharge into the open at a location protected from the wind as pressure fluctuations, e.g. caused by wind, cause detector instabilities.
In addition, the installation room should be well ventilated.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
2 - Basic security settings
Warning signs on the analyzer
Warning sign furnace
The following picture shows the warning sign on the furnace heat protection cladding:
22
Warning sign electrical area
The following picture shows the warning sign on the electrical section cover:
Meaning of the warning signs
The following table explains the meaning of the warning signs:
Warning sign Meaning
Warning: hot surfaces
Electric current hazard
Note
You are obliged to keep the warning signs on the instrument complete and in a legible condition.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
2 - Basic security settings 23
Warning: changes to the instrument
Safe instrument
The analyzer is designed and delivered in such a way to ensure safe working if you observe the instructions in the operating instructions.
Warning: Changes to the instrument
If you make any changes to the instrument, you risk rendering the instrument unsafe.
The consequences would be:
Injuries to the operating personnel
Damages to the instrument
loss of warranty.
Therefore, never make any unauthorized additions/conversions to the instrument.
Warning: unsuitable spare parts and consumables
Warning
If you use spare parts and consumables of an unsuitable type and quality, you risk:
Injuries to the operating personnel
damage to the instrument
Distortion of analysis results
Loss of warranty.
Only use original spare parts and original consumables that you have purchased from BÜCHI
Labortechnik AG or authorized dealers.
Required user knowledge and skills
Knowledge and skills
Depending on the specific task, the user must have different knowledge and skills. The following table indicates which sections of the operating instructions require what knowledge and skills:
Section
Work performed by the system administrator
Starting up or shutting down the instrument
Using the instrument
Maintaining the instrument
Repairing the instrument
Required knowledge and skills
Personnel with good knowledge of the operating system and administrative settings.
Personnel authorized by BÜCHI and having undergone training.
Personnel with basic knowledge of chemistry and experience with laboratory work (e.g. laboratory worker).
Personnel authorized by BÜCHI.
Personnel authorized by BÜCHI and having undergone training.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
2 - Basic security settings
Required personal safety equipment
Protective glasses
You require protective glasses for many activities. Make sure that protective glasses are always available nearby the analyzer.
Protective gloves
BÜCHI two kinds of protective gloves with the instrument:
The protective leather gloves for protection against cuts on broken glass from cold quartz components.
The heat protection gloves for protection against burns on hot components.
Always keep the protective gloves nearby the analyzer. Replace the protective gloves immediately if required.
Laboratory clothing
For work on and with the instrument you need:
Sturdy shoes
Cotton apron
Hair tie to tie back long hair
Obedience of general rules for safe work in the laboratory
Warning notes during operation
24
Note
Always pay attention to careful handling when working with the instrument, especially for modifications, maintenance and repairing works. The following notes have to be strictly observed when performing the corresponding works.
Replacing the ash crucible/finger
Please observe the following instructions:
Warning
Hot instrument parts and hot ash particles!
Risk of burning due to hot instrument parts.
When replacing:
Wear protective glasses.
Wear the enclosed heat protection gloves.
Place the hot instrument tubes in a tube rack on a level, non-combustible surface.
Protect the hot instrument parts from unauthorized access.
Never leave the instrument unattended when the furnace has been pulled out.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
2 - Basic security settings
Warning
Gas pressure and caustic substances in the instrument
Consumables may escape under pressure and cause chemical burns. Before performing the work:
Shut off the gas supply. To do so, execute the
Options > Maintenance >
Replace parts
command.
Damaged base panel
Please observe the following instruction:
Caution
Damaged base panel!
Damage to the base panel will impair proper functioning of the carousel.
Before starting maintenance work, always remove all samples from the carousel.
When dismantling and cleaning the carousel:
Never use pointed objects to dismantle the carousel.
Never use sharp or aggressive cleaners.
Gas pressure
Please observe the following instruction:
Warning
Gas pressure and caustic substances in the instrument
Consumables may escape under pressure and cause chemical burns. Before performing the work:
Shut off the gas supply. To do so, execute the Options > Maintenance >
Replace parts
command.
Hot instrument parts
Please observe the following instruction:
Warning
Hot instrument parts!
Risk of burning due to hot instrument parts. Before performing the work:
Allow the furnace to cool down
Disconnect the power supply plug
Cleaning and installing/removing the quartz glass bridge
Please observe the following instruction:
Warning
Sharp pieces of broken glass!
When cold quartz or glass components break there is a risk of cut injuries.
Wear the enclosed protective leather gloves and protective glasses when handling cold quartz and glass parts.
25
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
2 - Basic security settings
Removing reaction tubes
Please observe the following instructions:
Warning Hot reaction tubes!
Risk of burning due to hot instrument parts.
Warning
When replacing the reaction tubes:
Wear protective glasses.
Wear the enclosed heat protection gloves.
Place the hot tubes in a tube rack on a level, non-combustible surface.
Protect the hot tubes from unauthorized access.
Never leave the instrument unattended when the furnace has been pulled out.
Gas pressure and caustic substances in the instrument
Consumables may escape under pressure and cause chemical burns. Before performing the work:
Shut off the gas supply. To do so, execute the
Options > Maintenance >
Replace parts
command.
Filling reaction tubes
Please observe the following instructions:
Warning
Sharp pieces of broken glass!
When cold quartz or glass components break there is a risk of cut injuries.
Wear the enclosed protective leather gloves and protective glasses when handling cold quartz and glass parts.
Caution Cutting sealing elements apart/out (o-rings, quad rings, half shells, ferrules).
When cutting sealing elements apart/out with a knife you may damage sealing surfaces.
Never remove sealing elements with a knife but rather with tweezers.
Installing and conditioning the reaction tubes
Please observe the following instructions:
Warning Hot components in the instrument
When working inside the instrument there is a risk of burning as many parts of the instrument are hot.
When working inside the instrument always wear protective glasses and the enclosed heat protection gloves.
Caution Overheating if tube fillings are not appropriate for the operating mode!
Overheated tube fillings melt, run into the furnace area and destroy the furnace.
Make sure that the tube fillings correspond to the selected operating mode.
26
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
2 - Basic security settings
Emptying reaction tubes
Please observe the following instruction:
Warning Sharp pieces of broken glass!
When cold quartz or glass components break there is a risk of cut injuries.
Wear the enclosed protective leather gloves and protective glasses when handling cold quartz and glass parts.
Warning Harmful substances when glass is broken!
When filled quartz or glass components break there is a risk that harmful substances may be released.
Wear a dust mask when handling cold quartz and glass parts.
Replacing fuses
Please observe the following instructions:
Risk
Live parts!
Risk
When replacing fuses there is a risk of electrocution.
Before replacing fuses:
Allow the furnace to cool down.
Disconnect the power supply plug.
High voltage!
Using the wrong fuses can pose a risk of electrocution or fire.
Caution
Only use fuses matching the indicated type and the indicated voltage on the fuse holder.
Lack of ventilation of the analyzer!
A lack of ventilation leads to overheating of the analyzer. Before you switch off the instrument:
Switch off the furnace. To do so, execute the following command:
System >
Furnace
Allow the furnace to cool down until the temperature displayed is less than 55
°C.
Filling the drying tube
Please observe the following instructions:
Warning
Caustic substance Sicapent® (phosphorus pentoxide)!
Danger of chemical burns when handling Sicapent®.
Wear protective glasses and the enclosed protective leather gloves.
Warning
Sharp pieces of broken glass!
When cold quartz or glass components break there is a risk of cut injuries.
Wear the enclosed protective leather gloves and protective glasses when handling cold quartz and glass parts.
27
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
2 - Basic security settings
Installing/removing the drying tube
Please observe the following instructions:
Caution Lack of ventilation of the analyzer!
A lack of ventilation leads to component overheating
Do not open the front door too long when the furnaces are hot and the furnace is not pulled out. Otherwise the ventilation will not work properly.
Warning Caustic substance Sicapent® (phosphorus pentoxide)!
Danger of chemical burns when handling Sicapent®.
Wear protective glasses and the enclosed protective leather gloves.
Overheating of tube fillings
Please observe the following instruction:
Caution
Overheating if tube fillings are not appropriate for the operating mode!
Overheated tube fillings melt, run into the furnace area and destroy the furnace.
Make sure that the tube fillings correspond to the selected operating mode.
Working with the database
Please observe the following instructions:
Caution Data loss
After reorganizing the database via
Clean
all sample data and the contents of the logbook are irrevocably deleted.
Always backup your data before reorganizing the database via
Clean
.
Caution
Data loss
Restoring the database via
Restore
irrevocably overwrites all sample data, the contents of the logbook and the database configfuration parameters.
Always backup your data before restoring the database via
Restore
.
Improper changes
Please observe the following instruction:
Caution
Improper changes impair proper operation of the system and may destroy system components.
Only configure the instrument if you are authorized to do so and observe the operating instructions.
28
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
2 - Basic security settings
Baking out combustion tube and reductor
Please observe the following instructions:
Warning Gas pressure and caustic substances in the instrument!
Consumables may escape under pressure and cause chemical burns. Before performing the work:
Shut off the gas supply. To do so, execute the
Options > Maintenance >
Replace parts
command.
Warning
Hot components in the instrument
When working inside the instrument there is a risk of burning as many parts of the instrument are hot.
When working inside the instrument always wear protective glasses and the enclosed heat protection gloves.
Mixing up gas inlets
Please observe the following instruction:
Caution
A mix-up of the gas inlets may lead to destruction of the instrument.
Connect the supply lines carefully and observe the diagram.
29
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
C H A P T E R 3
Product description
Target group
Personnel working with the instrument.
Purpose
This section provides general information about the instrument.
In this chapter
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
3 - Product description
Analytical characteristics and technical specifications
Target group
Personnel working with the instrument.
Purpose
This section lists the analytical characteristics and technical specifications.
In this section
32
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
3 - Product description
Analytical characteristics
Analytical characteristics
The following table explains the analytical characteristics:
Analytical characteristic
Analysis method
Standards
Detector
Dynamic work range
Precision
Comments
Nitrogen determination from a sample according to Dumas.
Combustion of the samples, transfer to N gases, thermal conductivity detection.
2
, separation of foreign
Analysis method according to (excerpt):
AOAC 99.03, AOAC 993.13, AOAC 968.06, AOAC 992.15,
AOAC 992.23, ASBC, AACC (for fertilizer, meat, meat products, grain, oilseed, brewery grain, flour, animal feed),
DIN 10 467, milk and milk products,
EN 61010
Thermal conductivity detector (TCD). up to 200 mg N abs.
Less than 0.5 % relative standard deviation with test substance glutamic acid (sample weight: approx. 250 mg).
Recovery rate
Duration of analysis
Calibration
Larger than 99.5 % for test substances.
Self-optimizing, 3 to 6 minutes, depending on substance and sample weight.
Linear and non-linear curve adjustment; total work range, if applicable divided into two segments.
Data storage and data output Storage on hard disk or external storage media.
LIMS transfer possible.
Data output to screen and printer.
Technical specifications
Standardization
The instrument conforms to CE standards in accordance with EC Directives:
EMC 89/336/EEC
LVD 73/23/EEC
Control and data processing
The following table contains the technical specifications of the control and data processing system:
Reference value
Control and evaluation unit
Software
Interfaces
Technical specifications
PC with operating system Windows 7 ® Professional or a newer version of Windows Professional
Printer (optional)
German or English
Menu-driven
Status display during analysis
Real-time graphics
USB, RS232 /V24, Safety low voltage as per DIN IEC 380/VDE
0806/08.81
33
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
3 - Product description
Dimensions and weights
The following table contains dimensions and weight of the instrument:
Reference value
Dimensions
Weight
Technical specifications
480 mm x 550 mm x 550 mm (Width x Depth x Height)
65 kg
Electrical and gas supply
The following table contains the technical specifications of the electrical and gas supply:
Reference value
Mains voltage
Power requirement
Connected load
Connected electrical loads and frequency of the complete analysis unit
Technical specifications
100–230 Volt AC ± 10 %; 50–60 Hz
0.6 kWh/h
1.4 kVA
Connected electrical load:
Voltage:
Frequency:
16 A
100V AC ± 10 %
120V AC ± 10 %
230V AC ± 10 %
50-60 Hz
Supply gases Carbon dioxide:
Oxygen:
Purity: 99.995 %
Purity: 99.995 %
Consumption of supply gases Per analysis approx. 2.5 liters carbon dioxide.
Per analysis approx. 0.5 liters oxygen.
Ambient conditions
The following table contains the technical specifications of the ambient conditions:
Reference value
Protection class
Mode of protection
Noise level
Permissible ambient temperature
Technical specifications
Protection class I, protective conductor connection
IP20, installation in dry rooms only
55 dB (A), as per DIN 45635 section 1
Maximum: + 35 °C, minimum: + 15 °C
34
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
3 - Product description
Instrument design
Target group
Personnel involved with the instrument.
Purpose
This section describes the design of the instrument.
In this section
35
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
3 - Product description
Front view
Front view, closed
The following picture shows the front view of the instrument with the front door closed:
36
Front view, open
The following picture shows the front view of the instrument with the front door opened:
Legend:
1 Ball valve
2 Drying tubes
3 Furnace with heat protection cladding
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
3 - Product description
Rear view
Rear view
The following picture shows the rear view of the analyzer:
Legend:
1 Rear wall
2 Air baffle
3 "PC" PC connector (USB)
4 "Reserve" reserve
5 "~" mains connector
6 "CO
2
IN" CO
7 "O
2
IN" O
2
2
gas inlet
gas inlet
8 Gas drying
9 "WASTE" Gas outlet
37
Right side view
Right side view, closed
The following picture shows the right side of the analyzer with the side door closed, as seen from the front:
Legend:
1 Right side door
2 Main switch
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
3 - Product description
Right side view, open
The following picture shows the right side of the analyzer with the side door open, as seen from the front:
Legend:
1 Mainboard
2 Furnace
3 Main switch
38
Left side view
Left side view, closed
The following picture shows the left side of the analyzer with the side door closed, as seen from the front:
Legend:
1 Left side door
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
3 - Product description 39
Left side view, open
The following picture shows the left side of the analyzer with the side door open, as seen from the front:
Legend:
1 Thermal conductivity detector (TCD)
2 Water condenser
3 Gas drying
Top view
Top view of the instrument
The following picture shows the top view of the instrument:
Legend:
1 Carousel cover
2 Carousel, sample magazine and
cover ring
3 Instrument cover
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
3 - Product description
Peripherals and their function
Types of peripherals
The following picture shows the analyzer and its peripherals
Legend:
1 Instrument
2 Balance
3 Printer
4 PC
40
Functions of the peripherals
The following table lists the functions of peripherals:
Peripheral
PC
Printer
Balance
Function
Print out measuring results, etc.
Transmit sample weight
Requirement
Operation of the instrument with operating software required recommended recommended
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
C H A P T E R 4
Understanding the instrument and planning its use
Target group
Personnel with basic chemical knowledge and basic computer knowledge.
Purpose
This section helps you to assess the applications of the instrument and subsequently plan the use of the instrument.
In this chapter
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
4 - Understanding the instrument and planning its use
Layout and mode of functioning
Target group
Personnel with basic chemical knowledge and basic computer knowledge.
Purpose
This section describes what the instrument does, what the analysis parameters mean, and what happens in the instrument during an analysis.
In this section
42
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
4 - Understanding the instrument and planning its use
Functional units
Introduction
The following section describes what units comprise the instrument and what functions the individual units perform in the analysis procedure.
Functional diagram
The following diagram shows the basic setup of the instrument and its division into functional units.
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Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
4 - Understanding the instrument and planning its use 44
I
II
III
IV
Mechanical sample insertion and O
2
dosing system
Furnace area and reaction zone
Gas drying
Detector
Mechanical sample insertion and O
2
dosing system (I)
The following table describes the components of the unit and their functions:
Part
1
2
Name
Carousel
Ball valve with Ni flap
Function
holds all samples in a series.
transports the current sample into the ball valve
allows the metered addition of O
2
during the combustion.
holds the current sample.
shuts the current sample off from the ambient air.
allows the system to displace any ambient air.
transports the current sample into the combustion tube.
protects the ball valve from contamination.
For details on sample insertion, cf. Sample insertion and initiation of measurement
Furnace area and reaction zone (II)
The following table describes the components of the unit and their functions:
Part
3
4
5
Name
Furnace
Combustion tube with tube filling
Ash crucible
Function
holds the combustion tube, post combustion tube and reductor/regainer at a constant temperature and thereby ensures reproducible analysis results.
Space for complete combustion of the sample including combustion catalyst.
Binds disturbing alkali and earth alkali elements.
Holds combustion residues and sample packing of analyzed samples; for fast, easy emptying without replacing the combustion tube.
Oxidation of the combustion products. 6
7
Post combustion tube with tube filling
Reductor Reduces NO
X
to N
2
.
Binds volatile halogen compounds and sulfurous compounds.
For details on the processes in the furnace area, cf. Substance digestion and preparation of the reaction gas mixture.
Gas drying (III)
The following table describes the components of the unit and their functions:
Part
8
Name
Drying tube, gas drying and water condenser
Function
Removes H
2
O from the measuring gas.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
4 - Understanding the instrument and planning its use 45
Detector (IV)
The following table describes the components of the unit and their functions:
Part
9
Name
Reference cell
Function
reacts to fluctuations in the composition of the analysis gas mixture with an electrical signal to which a measuring component can be assigned.
see "Reference cell". 10 Measuring cell
For details on the working principle of the detectors, see
Detecting measuring components and evaluating the measuring signal
The thermal conductivity detector (TCD)
Design
The thermal conductivity detector (TCD) consists of two chambers through which the analysis gas mixture (measuring cell) and the pure carriage gas (reference cell) simultaneously flow through during the analysis. The chambers form a measuring bridge.
Working principle
The thermal conductivity of the carrier gas reacts sensitively on the addition of small amounts of foreign gases such as the measuring component N. If this measuring component exists in the analysis gas mixture, this leads to a disturbance of the measuring bridge that is registered in the form of an electrical signal.
Further processing of the measuring signal
The TCD measuring signal is digitized, integrated and output by the instrument to the PC, where it is
registered in the form of a measuring peak dependent on time,
and the integral is correlated with the absolute quantity of the respective measuring component by calibration functions.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
4 - Understanding the instrument and planning its use
Processes in the instrument during a measurement
Target group
Personnel with basic chemical knowledge and basic computer knowledge.
Purpose
The following section is designed to help you understand the processes that take place during a measurement.
In this section
46
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
4 - Understanding the instrument and planning its use 47
Sample insertion and initiation of measurement
Introduction
The following section explains how to insert the analysis samples into the combustion tube and how to initiate measurement of the reaction products.
Note
The bracketed numbers used below refer to the part numbers listed in Functional units.
Sample insertion processes and initiation of measurement
Sample insertion and initiation of measurement is divided into the following phases:
The thermal conductivity detector (9, 10) performs autozero adjustment of the measuring signal.
A complete pressure drop takes place in the system, together with the emptying of water accumulated in the water condenser (8).
The ball valve (2) opens by turning the ball through 90°.
The carousel (1) moves one step and the sample drops through the ball valve (2) onto the closed
Ni flap.
The ball valve (2) turns through 90° and closes the apparatus.
The carrier gas is reactivated and and the atmospheric nitrogen will be flushed out.
After expiration of a flushing time (Ni flap delay) the Ni flap opens for a short period by means of a pivoting magnetic field.
The sample drops into the ash crucible (5) of the combustion tube (4) and is heated up to the combustion temperature.
Oxygen dosing into the ash crucible begins.
The integrator reset resets integration display to zero. N integration begins.
Substance digestion and preparation of the reaction gas mixture
Introduction
The following section explains
what processes take place in the combustion, post combustion and reductor of the furnace.
how the reaction gas mixture is prepared for the nitrogen determination.
Note
The item numbers used below refer to the picture in Functional units.
Processes during substance digestion and preparation of the reaction gas mixture
Substance digestion and preparation of the reaction gas mixture is divided into the following phases:
The atmosphere in the combustion tube (4) is enriched with oxygen. Nitrogen bound in the sample burns to form N to form CO
2
.
2
and NO
X
. Halogens bound in the sample react to form volatile halogen compounds, sulfur reacts to form SO
2
and SO
3
, hydrogen reacts to form H
2
O and carbon reacts
The carrier gas flow transfers the gaseous combustion products into the post combustion tube (6) and reductor (7), where the following processes take place:
In the reductor, nitrogen oxides are quantitatively transferred to form molecular nitrogen.
Sulfur absorption takes place in the reductor.
Volatile halogen compounds are bound on brass wool.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
4 - Understanding the instrument and planning its use
The post combustion tube is used to complete oxidation of the sample.
The gas stream is predried in the water condenser (8) as well as the gas drying. In the downstream gas drying and drying tube (8), the residual moisture is removed.
Detection of measuring components and evaluation of the measuring signal
Introduction
The following section explains how the measuring components are detected in the reaction gas mixture and how the measuring signal is evaluated.
Process
Detection of the measuring components and evaluation of the measuring signal take place in the following phases:
Depending on the type and concentration of the measuring component, the thermal conductivity detector sends an electrical measuring signal to a microcontroller. This controller integrates the measuring signal. Cf.
The thermal conductivity detector (TCD)
In the PC the measuring signal
is recorded dependent on time
and displayed as an integral.
The integral value is assigned to an absolute nitrogen content of the sample via a non-linear calibration. See
Background knowledge required for calibration
The nitrogen percentage of the sample is calculated from the found absolute nitrogen content and the sample weight. An empirical factor (protein factor) translates the nitrogen content to the protein content.
Formulas for determining element concentration of analysis samples (Solids)
Process
During an analysis, the system first measures the absolute element content of the sample.
The peak area value of the N component of the sample is determined.
The blank value is factored in.
The absolute N content of the sample is computed on the basis of the calibration coefficients.
The daily factor is factored in.
The N concentration of the sample is calculated from the computed absolute N content and the sample weight by the following formula: where: c = element concentration in [%] a = absolute element content in [mg] f = daily factor w = sample weight in [mg]
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Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
4 - Understanding the instrument and planning its use
Basic facts about working with the instrument
Target group
Personnel with basic chemical knowledge and basic computer knowledge.
Purpose
The following section provides basic facts about working rationally and appropriately with the instrument.
In this section
49
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
4 - Understanding the instrument and planning its use 50
Instrument equipment
Combustion tube filling
The following picture shows the fillings and filling heights of the combustion tube:
Legend:
1 Ash crucible
2 Corundum balls (10 mm)
3 80 g CuO + 20 g Corundum balls (87 mm)
4 Corundum balls (26 mm)
5 Wire mesh ronde
6 Spacer
Filling the post combustion tube
The following picture shows the fillings and filling heights of the post combustion tube:
Legend:
1 Plug with embedded 3.3g brass wool
2 53g Regainer (126 mm)
3 Quartz wool (10 mm)
4,180 g CuO + 15 g Pt catalyst (167 mm)
5 Corundum balls (28 mm)
6 Wire mesh ronde
7 Spacer
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
4 - Understanding the instrument and planning its use
Background knowledge required for calibration
51
Important calibration principles
Perfect calibration of the instrument is a key condition for achieving correct analysis results. The calibration has to be carried out over the whole measuring range.
For successful calibration the user must be familiar with the analyzer and the operating instructions.
The personnel performing calibration must therefore be authorized and must have undergone appropriate training.
Purpose of instrument calibration
The analyzer does not measure the absolute content of an element in the sample but rather only changes of the element portion in the combustion gases. These changes cause an electrical signal in the detector that is recorded and integrated by the software depedent on time.
In order to create a correlation between the integrated detector signal and the absolute element content of the analysis samples, a series of calibration samples with known element content and different sample weights are measured. The software computes the calibration factors on the basis of the known element contents and the sample weights of the calibration samples.
Conditions for perfect calibration
In order to be able to calibrate the instrument perfectly, the following conditions must be met:
The instrument must have passed the leak test.
The instrument blank values must be low and roughly constant.
Only use suitable substances of at least p.a. quality or certified standards as calibration samples.
The concentration values of the calibration samples must cover the whole measuring range.
When to calibrate the instrument
It is always necessary to calibrate the instrument when one of the following is true:
You have removed components that influence analysis results, e.g. the detector.
The daily factor for a measuring component is clearly outside of the range of 0.9 to 1.1. Also, it displays fast changes in time from day to day.
Calibration formulae
The formulae used for calibration can be found in
Calibration formulae
Calibration curve calculation method
For details on the various calibration curve calculation methods and when to use them, see
Calibration curve computation method criteria
Notes on performing calibration
For details on practical implementation of calibration, refer to
the section Performing calibration.
the calibration tables.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
4 - Understanding the instrument and planning its use
Calibration curve calculation method criteria
52
Calibration curve configuration options
The user can specify the calibration curve calculation method according to the following criteria:
Calibration can be performed over the whole measuring range either consistently or in two ranges.
For a specific element content you can set a dividing line for two calibration ranges.
For each range, you select a polynomial degree according to which to compute the calibration curve (linear to 4th degree).
Calculation criteria
Look to the calibration view of the combi view for calibration curve calculation method criteria. You get to the calibration view after performing or loading a series of defined calibration samples by selecting
Calibration > Calibrate...
and then the "Configuration calibration" dialog.
Ideal calculation method
If possible, try to compute calibration curves so that they
are uniform over the whole measuring range and/or concentration range
and can be displayed in linear form or on the basis of a polynomial of the lowest order.
To facilitate selecting a calculation method, four typical calibration graphs are shown below along with the suitable calculation method.
Note:
For better understanding the calibration graphics are shown in a simplyfied way.
Linear calculation over the whole range
The following picture shows an example in which a linear calculation over the whole range achieves acceptable calibration curve quality.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
4 - Understanding the instrument and planning its use
Linear calculation over two ranges
The following picture shows an example in which a linear calculation over two ranges achieves acceptable calibration curve quality.
53
Linear and polynomial calculation
The following picture shows an example in which the calibration curve exhibits acceptable quality by means of a linear calculation in the low concentration range and a polynomial calculation in the higher concentration range.
Polynomial calculation over the whole range
The following picture shows an example in which a polynomial calculation over the whole range achieves acceptable calibration curve quality.
Achievable calibration curve quality
Process standard deviation "Proc-SD" and quality factor "r" serve as a measure of achievable calibration curve quality.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
4 - Understanding the instrument and planning its use
Use the following values for process standard deviation "Proc-SD" as guidelines:
Acceptable value: Proc-SD = ±3 µg in the lower range
Very good value:
Proc-SD = ±15 µg in the upper range
Proc-SD = ±1 µg
Use the following values for quality factor "r" as guidelines:
Good value for linear calibration function: r = 0.99 (r should tend to 1)
Good value for polynomial as calibration function r = < 2-4 (r should tend to 0)
If you do not approximately achieve the listed values you can assume that you have chosen the wrong calibration curve calculation method.
Calibration formulae
Calculation of absolute element content
Calibration is performed by analyzing samples with known concentrations (standard samples) where the measured peak areas are correlated with the corresponding absolute element content.
For a standard sample, the following parameters are known:
element concentration
Weight
Absolute element content is computed according to this formula: where: a = absolute element content in [mg] w = sample weight in [mg] c = element concentration in [%]
Computing calibration coefficients
Once the absolute element contents have been computed and the peak areas have been measured for the respective sample, the pairs of values (absolute content / peak area) are transferred into a coordinate system where they form the calibration curve. By means of an algorithm, the calibration coefficients a - e are computed which, entered in a polynomial, constitute the calibration curve.
Absolute element content is computed according to this formula: where: y = absolute element content in [mg] a...e = calibration coefficients x = peak area
Computing the quality factor for polynomials of the 1st degree
In order to assess how well the calibration curve described by the polynomial follows the actual development of the pairs of values, the software computes a quality factor for each calibration process. For a polynomial of the 1st degree (linear equation), this quality factor corresponds to the correlation coefficient. The closer the correlation coefficient tends to 1, the better the fit.
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The correlation coefficient is computed according to this formula: where: r x y i
2 = correlation coefficient i
= peak area of the corresponding sample
= absolute content of the corresponding sample n = number of samples i = index from 1 to n
Computing the quality factor for polynomials of a higher degree
In order to assess how well the calibration curve described by the polynomial follows the actual development of the pairs of values, the software computes a quality factor for each calibration process. For a polynomial of a higher degree, this quality factor corresponds to the sum of the error squares. The closer the sum of error squares tends to 0, the better the fit.
The sum of error squares is computed with these formulae: where: q = quality ssq = sum of error squares act i
= actual absolute content computed respectively theo i
= theoretical absolute content respectively n = number of samples i = index from 1 to n
Routine measuring work
Definitions
Routine measuring work comprises the following activities:
Determination of instrument blank values.
Instrument conditioning with conditioning samples.
Determination of daily factors.
Routine measuring work is performed at set intervals or on defined occasions before, during or after a series of measurements with real samples.
Instrument blank values
Determination of the instrument blank value depends on your needs. The following overview shows the type and purpose of the individual determinations.
Purpose Sample Occasion
Checking gas-tightness
Blank value determination of sample additives and packing materials none
Sample additive
Packing material after maintenance work to allow for sample additives or packing material
For details on determining blank values, cf. Types of blank value determination and their settings.
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Conditioning samples
Conditioning samples are measured with standard substances at the start of every series of analyses.
They are used to check...
... the correct run of the analysis.
... the proper condition of the instrument.
... flow and pressure behavior of the gases.
Daily factor determinations
Determination of the daily factor serves...
... to fine-tune instrument calibration to room conditions at the time of analysis.
... to assess the condition of the instrument by observing daily factor fluctuations and drift trends.
When to perform routine measuring work
Perform routine measuring work...
... at least once a day.
... additionally when measuring breaks last longer than 2 hours.
If a series of analyses exceeds a duration of 5-6 hours (carousel completely loaded), it is advisable to determine the daily factor additionally at the end of the series.
Formulae for blank value determination and compensation
Blank samples and blank values
Blank samples are samples...
... that do not contain sample substance.
... that have a key word for identification by the software as blind samples.
Despite the lack of sample substance, a peak area value is computed on the basis of various factors when analyzing blank samples. This peak area value is referred to as a blank value. In order to compensate for this, the averaged blank value is subtracted from the measured peak area value of every individual analysis sample.
Blank value determination
In blank value determination, the peak area values of the blank samples are averaged. The blank value is computed according to this formula: where:
/b = blank value b i
= peak areas of the individual blank samples n = number of blank samples i = index from 1 to n
Blank value compensation
The peak areas of the other samples are compensated with the aid of this formula: where: a comp
= compensated peak area a = measured peak area of the sample
/b = blank value
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Formula for determining the daily factor
57
Determining the daily factor
Standard samples are analyzed to determine the daily factor. The known element concentration of the standard samples is correlated with the actual element concentration computed.
Daily factor
The daily factor is computed according to this formula: whereas: f = daily factor c theo
= theoretical element concentration c act
= element concentration computed actually
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4 - Understanding the instrument and planning its use
Understanding the operating software
Target group
Personnel with basic chemical knowledge and basic computer knowledge.
Purpose
This section describes
the layout of the user interface
what instrument functions are controlled by the software
what current information is displayed during the analysis process
and how the raw analysis data are further processed, archived and managed
In this section
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Basic functions of the operating software
Introduction
The following section describes the functions of the operating software and what instrument control and data processing operations are possible.
Instrument control and parametrization
Instrument control and parametrization functions:
Starting a single analysis:
Starting and stopping a series of analyses
Entering parameters to prepare the instrument for measuring and for standby mode transitioning
(wake-up and sleep functions)
Determination of methods
Specifying time and temperature parameters of the analyzer
Data input
Data input functions:
Injection volume (via method)
Sample weight (solids mode)
Name
Blank values
Processing measuring data
Measuring data processing functions:
Measurement and numerical output of element contents in absolute values and percentages
Statistical evaluation of analysis data
Management of analysis data; data security
Analysis data management and data security functions
Importing/exporting from and to MS Excel
Interfaces to LIMS
Security functions using digital signatures
Support for maintenance/repair
Maintenance and repair support functions:
Definition of maintenance events and display when due
Calculation of calibration coefficients and assessment criteria for calibration quality
System diagnostics functions
Display analysis values and instrument state
Functions for current analysis value and current instrument state display:
Analysis progress
Temperature of the reaction tubes
Gas flows and pressure conditions in the instrument
Due time/date of next maintenance event
Current detector display
Element content of current sample
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Software user interface
The main window of the operating software
The following screenshot shows the main window of the operating software and designates the various areas and bars:
60
Title bar
The title bar displays the name of the file that you are currently processing. The title bar has the usual functions for displaying the system menu and for minimizing, maximizing and closing the window.
Menu bar
The menu bar shows the top level of the menu tree. You can access dialogs and input windows, etc. from the menubar for the following:
Saving, editing and managing analysis data,
Defining and entering sample data and instrument parameters,
Specifying maintenance events,
Configuring and performing statistical evaluations.
Details on the various dialogs and input windows accessible from the menu bar can be found at
Menu and dialog descriptions
(on page 251) and in the online help.
Toolbar
The toolbar allows you quick access to frequently required commands and functions. Among others, via the toolbar you can...
... create or save analysis series in the form of a file and open existing analysis files.
... cut, copy and paste sample data.
... switch the sample view.
... enable statistical and calibration functions.
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... "wake up" the "sleeping" instrument.
... start and stop individual and continuous analyses.
... display the online help.
Details on the various buttons on the toolbar can be found at
Toolbar
(on page 333) and in the online
help.
Sample view
The sample view displays a table of input, measuring and computed analysis data of all samples in a particular series. If an error occurs while measuring a sample, the table contains an appropriate message. For details on the sample view, see The sample view.
Combi view
The combi view contains different information depending on the selected display mode:
In progression/graph view, it displays the time-dependent development of the detector signals or a diagram of various instrument parameters of the currently selected sample.
In statistics view it displays statistical analysis data of the selected group of samples.
In calibration window view it displays a diagram of the calibration factors for the series under review and the calibration curves of the individual elements.
For details on the combi view and its various display modes, see The combi view.
"Current sample" field
This field displays a zoomed-in view of the data of the current sample. Here you can view the analysis results of the particular sample at a glance, even if you are not directly in front of the screen.
Status view
The status view contains information about the current operating states of the elemental analyzer. For details on the status view, See The status view.
Status bar
The status bar can contain the following information:
If you hover the mouse over a menu command or toolbar button, a short help text on the command is displayed on the left of the status bar.
The name of the current user logged in is displayed in the middle of the status bar.
The name of the user group to which the currently logged in user belongs is displayed on the right.
Sample view
Introduction
The following section describes what you can input in the sample view and what information you can get from the sample view.
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4 - Understanding the instrument and planning its use
View
The sample view looks like a familiar calculation sheet in a spreadsheet program.
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Sample view input functions
In the sample view you define the sequence of your analysis samples. The sequence must match the sequence in which you arrange your samples on the carousel. To enable the instrument to analyze and evaluate a sample correctly, you must have entered the appropriate information in the sample view columns:
Column
Weight [mg]
Name
Method
Explanation
Sample weight in mg (if the instrument is not connected to a balance that automatically transfers the sample weight to the computer).
Name of the sample; for samples used for routine measuring work you must use the reserved names, see Defining standard substances as factor and monitor samples
Defining standard substances as calibration samples
Assignment of an analysis method. If you have entered values for peak anticipation in the "Method" dialog, this overwrites the values for individual samples that were defined in the "Device parameters" dialog for the series.
In the "Memo" column you can input any special features of the sample or the analysis procedure as free text.
Color coding
Some table lines in the sample view are highlighted by a colored background or colored text. The following table indicates the meaning of the various color codes:
Color code green background yellow background red text green text black text
Meaning
Indicates the current sample.
Indicates the current sample.
Indicates a sample with a stop marker set.
Indicates samples with reserved names for routine measuring work or calibration samples.
Indicates all other samples.
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4 - Understanding the instrument and planning its use
Meaning of symbols in the "No." column
In the "No." column a symbol is displayed next to the serial number generated by the system; this symbol indicates the status of the individual samples. The following table lists the possible symbols and what they mean.
Icon Meaning
Sample not yet analyzed, but a measuring method has been set and a sample name exists.
Sample not yet analyzed, but a sample name has been set and a method does not yet exist.
Sample analyzed error-free with valid date information.
Sample without valid date information.
Sample which caused a non-critical error during measurement or when the measured peak area is outside of the specified calibration. The result was interpolated. The error code is entered in the "Info" column, see
Interpreting PC error messages
(on page
Sample at which the series was stopped.
Further information in the sample view
Depending on the selected operating mode, the following values can be displayed in the appropriate columns for each analyzed sample:
the integrals of the samples
the element content percentages of the samples
the daily factors of the elements for the particular sample
the blank values of the elements for the particular sample
date and time of measuring the particular sample
By selecting the
View > Configuration
menu you can show/hide every table column and define the order as desired.
Note on data output
The selected sample view screen view also corresponds to the display in a printed report.
Combi view
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Introduction
The following section describes the various views of the combi view and their information contents. By selecting the
View > Toggle
menu you can switch between the following combi views:
Progression view (graph view)
Statistics view
Calibration view
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4 - Understanding the instrument and planning its use
Progression view (graph view)
64
Progression view displays a graph of the development over time of important instrument parameters and measured values during measurement of the sample selected in the sample view. You can recognize the current sample by the green border around the graph display.
You can display the following individual parameters and measured values:
The CO
2
gas flow through the MFC
The O
2
gas flow through the MFC
The CO
2
gas flow through the flow meter
The intake pressure
The output pressure
The detector output signal
For details on configuring the analysis progression view, see
Data backup and printing
(on page
Statistics view
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The statistics view displays the element content percentages of all samples in a series, grouped by sample name.
For each group of samples, the following calculated statistical values per element are also displayed:
Percentage mean value of the element
The absolute standard deviation of the mean values
The relative standard deviation of the mean values
Difference (Delta) of the highest and lowest content of the group
You can exclude individual samples and/or values of a group from the calculation of statistical values or include them again.
Calibration view
If your series includes samples previously defined as calibration samples, you can use them to calculate calibration coefficients. You can define and determine up to two calibration ranges according to which polynomial degree you want to determine the calibration curve.
In this case, the calibration view displays the following information:
For each defined calibration range a graph display of the calibration curve optimized for the respective calibration samples.
The calibration coefficients computed according to the selected polynomial degree.
The correlation coefficient for the depicted calibration curve that allows you to assess the quality of calibration.
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4 - Understanding the instrument and planning its use
In the graph display, the samples used for compute the calibration curves are displayed as small circles. You can click one of these circles to display further information on the particular sample, see
Background knowledge required for calibration
(on page 51). This information allows you to
assess whether the sample must be treated as an "outlier" and therefore excluded from the calculation of the calibration coefficients. If you have assessed the calibration curves in this way and browse on to the next view, the "calibration coefficient" dialog is displayed with the current computed values. When you confirm this dialog by clicking
OK
, the calibration coefficients for the series are applied and the content of the calibration view is deleted (message: "No calibration or calibration finished").
Note on data output
The selected screen view of the combi view also corresponds to the display in a printed report.
Status view
Introduction
The following section describes what information about the analysis procedure and the condition of the instrument is displayed in the status view.
View
The following screenshot shows the status view in offline status:
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Meaning of the colored background
On the basis of the color of the status view background you can tell straight away whether the PC is properly connected to the analyzer. The meaning of the colors is:
green: The analyzer is connected to the PC and switched on. With the aid of the PC you can
enter analysis or instrument parameters
start or abort analyses
perform maintenance or diagnostics tasks.
gray: The analyzer is not connected to the PC or switched off. The operating software is running in offline status.
The areas of the status view and what they mean
The following table lists the individual areas of the status view and the information they contain:
Area
Process
Detector
Temperatures
Meaning
Displays a list of individual processes during the analysis procedure. The current process is highlighted with a colored background so that you can see the progress of the analysis of the current sample straight away. Displays "Standby" when the instrument is in idle mode.
Displays the following current values of the detector unit:
the current height of the current measuring peak.
Displays the current temperatures of the following units as a bar chart:
Combustion tube
Post combustion tube
Reductor
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Flow
Pressure
Maintenance
The current gas flow is displayed here as a bar chart.
MFC CO2: CO
2
flow through the MFC in the TCD
MFC O2: O
2
flow through the analysis apparatus during the combustion
Flow CO2: CO
2
flow through the analysis apparatus
In addition to bar graph the numerical value of the gas flow is displayed.
Position the cursor on the corresponding end of a bar graph.
Displays the current pressure values in the instrument here as bar diagram:
Input: Pressure value at the entrance section
Output: Pressure value at the exit section
In addition to bar graph the numerical value of the pressure is displayed.
Position the cursor on the corresponding end of a bar graph.
Maintenance intervals for the analyzer are defined on the basis of the maximum number of measured samples until a certain maintenance event occurs, see
Defining maintenance intervals in the software. The "Maintenance" section displays the current percentage of the specified number of samples until the next maintenance interval. This figure is displayed numerically and as a bar chart. The colors of the chart indicates the progress of the the next due maintenance interval.
green: less than 80%
yellow: 80 to 99%
red: more than 99%
When a maintenance interval is due, its name is displayed as text on the bar chart and a symbol flashes drawing the user's attention to this issue.
Right mouse button function
General
For many situations the right mouse key allows easily access to useful functions. This section describes the most important functions which can be invoked via the right mouse key.
In the sample window.
Depending on what is selected, pressing the right mouse button in the sample view displays a selection or all of the following commands:
Command
Copy
Delete
Paste
Set current sample
Set stop tag
Meaning
Copies the contents of a selected line to the clipboard.
Deletes the contents of a selected line.
Inserts the contents of the clipboard in the selected line.
Opens the "Set current sample" dialog. See Adjusting the current sample.
Opens the "Set stop tag" dialog. See Setting a stop marker.
In the combi view
If the statistics view is active in the combi view you can press the right mouse button to display the
Configure view
and
Include/exclude sample
commands:
Command
Configure view
Meaning
Opens the "Configure statistics view" dialog. See Configure statistics view.
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4 - Understanding the instrument and planning its use
Include/exclude sample Includes/excludes a sample from the statistical calculation.
If the graph view is active in the combi view, you can right-click on "Configure view" to display the
"Configure Graphic Pane" dialog. See Configure graph view.
In dialogs
In dialogs you can also press the right mouse button to display certain commands. In the "Configure view" dialog, right click to display the
Properties
command, that opens the "Column properties" dialog. See
Configure view
Further functions
In the "Specify upper and lower calibration range" dialog you can right-click to set the dividing line between the upper and lower calibration range. Position the cursor in the right place and then press the right mouse button. See Specifying the lower and upper calibration range.
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Data administration and data security
Target group
Personnel with basic chemical knowledge and basic computer knowledge.
Purpose
This section describes what options the system offers with regard to data administration and data security.
In this section
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Laboratory information and management system (LIMS)
What does LIMS do?
The
L aboratory
I nformation and
M anagement
S ystem (LIMS) collects and manages data from different systems and thereby facilitates laboratory operation and documentation.
Interaction between the software and LIMS
The following features characterize the interaction between the analyzer software and LIMS:
The flow of data is unidirectional, i. e. it only goes in one direction, from the analyzer to LIMS.
Data transfer is either via the serial interface or through the network.
The data to be transferred can be selected.
The data are transferred as ASCII files.
The names of the ASCII files are formed from a time/date stamp and a freely definable file extension.
Every data transfer includes a freely definable user name and a freely definable instrument identifier.
Data can be sent automatically after every analysis or manually by selecting the appropriate menu command.
File name structure
The file name generated for LIMS has the following format: dddsssss.xxx
, consisting of the following elements:
ddd
: Days since January 1.
sssss
: Seconds since midnight.
xxx
: File extension defined by the user.
Sequence of data transferred.
The sequence of the data transferred corresponds to the list of data in the "LIMS settings" dialog,
"LIMS data" tab, from top to bottom. See
LIMS settings
Conditions for operating the LIMS
Data transfer via the serial interface
Normally, data transfer to LIMS is performed through a network. However, if you want to transfer data via the serial interface, you must make sure that the LIMS port name is not identical to the port name between the PC and the analyzer. This could lead to a system crash.
Identical LIMS and instrument software settings
When transferring data to LIMS, observe the following:
The LIMS program receving the data must be set to the same data volume as the sender BÜCHI program. If you change the LIMS settings, you must therefore adjust the LIMS program appropriately.
The data sent to LIMS are tab-separated. The LIMS program must be able to interpret this correctly.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
4 - Understanding the instrument and planning its use
21 CFR Part 11 functionality
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What is 21 CFR Part 11?
21 CFR Part 11 is a regulation that was published by the American Food and Drug Administration
(FDA), under number 21 CFR part 11, at the end of the 1990s and that has legal force in the USA. It governs technical and organizational requirements to be fulfilled in order to use electronic data and documents instead of paper for development, approval and production.
Whom does 21 CFR Part 11 apply to?
21 CFR Part 11 applies to:
All sectors of the pharmaceutical and medical technology industry in the USA working in FDAregulated areas. They are obliged to keep their electronic data and computer systems in conformance with 21 CFR Part 11.
Also, all companies outside of the USA that manufacture products for the American market or develop products with regard to having them subsequently approved for the US market.
Requirements of 21 CFR Part 11
The system conforms to 21 CFR Part 11 and therefore meets the following requirements:
Generation of exact electronic analysis data.
Protection of the generated analysis data from intentional and unintentional modification.
Possibility of performing audit trails.
Signing of electronic documents with electronic signatures.
Access control to menu functions by password-protected user levels.
Generation of exact electronic analysis data
The data recorded during the analysis process are converted into the respective element contents with the aid of algorithms and reliably saved. Generation of exact results is therefore ensured.
Protection of analysis data
The recorded and computed data are stored in a database. The sample data can only be overwritten as long as these samples have not yet been analyzed. Afterwards, a new file version is created retaining the same file name and the previous version. This allows end-to-end tracking of changes in the series of samples, where unauthorized manipulating of the data is not possible as they are encapsulated in the database. See
Versioning
Performing audit trails
Every user action is recorded and permanently stored in a logfile - the logbook. All actions are given a timestamp and the name of the user currently logged in. Some actions must be justified by the respective user and this justification is also saved to the logfile. The logbook records can be viewed when performing audit trails. This makes it possible to evidence appropriate procedure in generating the data and operating the analyzer.
Signing documents
Every document can be "signed" up to three times by authorized individuals. This is done on the following occasions:
When the document is created
When the document is reviewed
In order to release the document
When signing, the signee enters a password only known to him. With the aid of this password and a key, it is possible to check the correct document signature at other points (for example after sending the document by e-mail). It is thus possible to ascertain whether the data contained are authentic.
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Restricted access to menu functions
The software restricts access to the menu functions on the basis of three user groups:
The lowest user group may only perform actions required in routine operation.
The middle user group may also perform actions requiring experience, e.g. calibration.
The top user group may also perform actions requiring a great deal of experience, e. g. changes to the system configuration.
The software also prevents unauthorized individuals from interfering with the system when the authorized user is not present. If the user has not performed an action for some time, the software prompts him to log in again.
Versioning
Versioning
If 21 CFR Part 11 functionality is enabled, a new version of the document is created as soon as an analyzed sample is changed.
Version identification
Every version is identified as follows:
with an index number,
with the date of creation,
and with the name of the user who made the change.
The current version is number 0, the previous versions are indexed -1, -2, etc.
Protection of previous versions
Previous versions are write-protected, i.e. they cannot be edited but only viewed or printed out.
Linking the analyzer and software
Background
It is important that the analysis data can be unambiguously allocated to the analyzer with which they were generated. This allocation is performed via a serial number. In every instrument, the individual serial number is stored in a memory module and queried by the software when you launch the program. The program can only be operated in combination with the analyzer if the serial number matches the software licence number. This ensures that the analyzer is always operated together with the same software and the settings recorded in the logbook.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
C H A P T E R 5
Work performed by the system administrator
Target group
Personnel with good knowledge of the operating system and administrative settings.
Purpose
This section enables you to perform typical system administrator tasks.
In this chapter
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
5 - Work performed by the system administrator
Installing and updating the software
Conditions for installation
In order to install the software correctly, administrator rights for the PC must be available.
Requirements for operation
Do the following to be able to operate the software without any problems:
On the PC where the software is installed, check power management settings under
Control
Panel > Power Management
or under
Control Panel > Power Options
. The following options must be set to "Never":
"Turn off monitor"
"Turn off hard disks"
"System stand by"
"System hibernates"
Power management must also be disabled in the PC's BIOS.
The PC on which the software is installed must not be overloaded with other software. This could cause unstable operation of the software.
Installing and updating the software
Proceed as follows:
Insert the enclosed CD/DVD in the CD/DVD-ROM drive. The CD/DVD usually starts automatically.
If the CD/DVD does not start automatically, start it by running setup.exe
on the CD/DVD.
Select the desired language.
The installation wizard is displayed. Click
Next
and follow the steps of the installation wizard.
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5 - Work performed by the system administrator
Configure analyzer
Target group
Personnel with basic chemical knowledge and basic computer knowledge.
Purpose
This section describes what the instrument does, what the analysis parameters mean, and what happens in the instrument during an analysis.
In this section
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Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
5 - Work performed by the system administrator
What can you modify in the configuration?
76
Safety instruction
Strictly observe the safety instruction "Improper changes" under
Warning notes during operation
What can you set?
You can set the following in the configuration:
Interface properties
Weighing data properties
Signature program properties
Device parameter
See
Configure analyzer
Defining logon timeout
What is the logon timeout?
The logon timeout defines the time to wait in which the user does not perform any action before the operating software displays a dialog to log in again.
Safety instruction
Strictly observe the safety instruction "Improper changes" under
Warning notes during operation
Defining logon timeout
Proceed as follows:
Open the "Device configuration" dialog by selecting
Options > Configuration
.
Select the "DEVICE.INI" tab. Select the "System" section by clicking the arrow next to the
"Section" dropdown listbox.
Select in the "Items" listbox the entry "Logon Timeout" and click
Edit
. The "Configure key value" dialog is displayed:
Enter the number of seconds to wait before displaying the login dialog again in the "Value" field and click
OK
. The "Comment modification" dialog is displayed.
Enter a justification in the "Comment modification" dialog and click
Close
.
Click
OK
in the "Device configuration" dialog. Your settings are saved and the dialog is closed. A message window appears which informs that the modification will only become operative after the instrument software has been left and re-started.
Click
OK
and quit the operating software.
Restart the operating software as required.
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5 - Work performed by the system administrator
Creating new sections
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Safety instruction
Strictly observe the safety instruction "Improper changes" under
Warning notes during operation
Creating new sections
Proceed as follows:
Open the "Device configuration" dialog by selecting
Options > Configuration
.
Select the tab for which you want to create a new section.
Enter the name of the new section in the "Section" dropdown listbox and click
New Section
to the right of it. The "Comment modification" dialog is displayed:
Enter a justification in the "Comment modification" dialog and click
Close
.
Click
Insert
in the dialog "Device configuration" to insert an entry into the section just created.
The "Configure key value" dialog is displayed:
Enter your values in the "Key" and "Value" fields and click
OK
. The "Comment modification" dialog is displayed.
Enter a justification in the "Comment modification" dialog and click
Close
.
Click
OK
in the "Device configuration" dialog. Your settings are saved and the dialog is closed. A message window appears which informs that the modification will only become operative after the instrument software has been left and re-started.
Click
OK
and quit the operating software.
Restart the operating software as required.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
5 - Work performed by the system administrator
Defining LIMS export settings
Target group
Personnel with good knowledge of the operating system and administrative settings.
Purpose
This section enables you to define export settings for LIMS as system administrator.
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LIMS export settings
What is set?
The following are set for LIMS:
What data to send.
Whether the data is transferred via interface or network.
The interface settings.
What instrument the data belong to.
See
LIMS settings
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Setting up user administration
Target group
Personnel with good knowledge of the operating system and administrative settings.
Purpose
This section enables you to set up the user administration as system administrator.
In this section
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User administration
User groups
Access to menu functions is restricted on the basis of three user groups in the operating software.
These groups are automatically set up when you install the software under Windows:
The user group "DuMaster user" with the lowest authorizations.
The user group "DuMaster superuser" with more authorizations.
The user group "DuMaster administrator" with most authorizations.
Allocating users to user groups
The following standard users are automatically allocated to the user groups:
User group
DuMaster user
DuMaster superuser
DuMaster administrator
Standard user buchiuser buchisuperuser buchiadmin
The system administrator must allocate additional individual users via the Windows control panel.
Refer to the Windows help for further information.
Users belonging to multiple user groups
When you log in, the software searches the user groups for the user, starting with the administrator group. If a user belongs to multiple user groups, he is therefore always offered the higher user group when he logs in.
Passwords
User passwords must correspond to the usual conventions in Windows. Windows has requirements regarding:
The minimum number of characters
The use of letters, numbers and special characters.
Refer to the Windows help for further information on passwords.
Recommendations for user administration
Recommendations
The following is recommended for user administration:
In the operating software you should define individual users in addition to the standard users.
Standard users are buchiuser, buchisuperuser und buchiadmin.
If you are working with a server, you should not work on one domain only. You should set up an emergency group on a local computer so that you can also work if the server crashes.
Granting authorizations
Background
The instrument software offers the possibility to assign the access of menu commands to different user groups, so that individual menus can be invoked only by persons who are authorized accordingly.
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Safety instruction
Strictly observe the safety instruction "Improper changes" under
Warning notes during operation
Granting authorizations
Proceed as follows:
Open the "Device configuration" dialog by selecting
Options > Configuration
.
Select the "DEVICE.INI" tab. Select the "Menu" section by clicking the arrow next to the "Section" dropdown listbox. In the field "Items" all menu commands are listed. The numbers of the menu commands have the following meaning:
1: User, superuser and administrator are authorized to execute the command.
2: Only superuser and administrator are authorized to execute the command.
3: Only the administrator is authorized to execute the command.
In the field "Items" select the command whose authorization you want to change and click
Edit
.
The "Configure key value" dialog is displayed:
In the field "Value" change the menu command's prefixed number to the desired value (1...3) and click
OK
. The "Comment modification" dialog is displayed.
Enter a justification in the "Comment modification" dialog and click
Close
.
Click
OK
in the "Device configuration" dialog. Your settings are saved and the dialog is closed. A message window appears which informs that the modification will only become operative after the instrument software has been left and re-started.
Click
OK
and quit the operating software.
Restart the operating software as required.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
5 - Work performed by the system administrator
Defining interfaces
Target group
Personnel with good knowledge of the operating system and administrative settings.
Purpose
This section enables you to define various interfaces as system administrator.
In this section
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Defining the analyzer / PC interface
Note
The operating software can only be operated in combination with the analyzer if the serial number of the instrument matches the software licence number. This ensures that the analyzer is always operated together with the same software and the settings recorded in the logbook.
84
Safety instruction
Strictly observe the safety instruction "Improper changes" under
Warning notes during operation
Defining the analyzer / PC interface
Proceed as follows:
Open the "Device configuration" dialog by selecting
Options > Configuration
.
Select the "DEVICE.INI" tab. Then select the "Analyzer Port" section by clicking the arrow next to the "Section" dropdown listbox.
Select in the "Items" listbox the entry "Name" and click
Edit
. The "Configure key value" dialog is displayed:
Enter the name of the serial port (e.g. "COM2") in the "Value" field and click
OK
. The "Comment modification" dialog is displayed.
Enter a justification in the "Comment modification" dialog and click
Close
.
Click
OK
in the "Device configuration" dialog. Your settings are saved and the dialog is closed. A message window appears which informs that the modification will only become operative after the instrument software has been left and re-started.
Click
OK
and quit the operating software.
Restart the operating software as required.
Dialog details
Details on the "Device configuration" dialog can be found in
Device configuration
Defining the LIMS / PC interface
Defining the LIMS / PC interface
Proceed as follows:
Open the "LIMS settings" dialog by selecting
Options> Settings> LIMS
.
Select the "Communication" tab. Define your settings.
Click
OK
in the "LIMS settings" dialog. Your settings are saved and the dialog is closed.
Dialog details
Details on the "LIMS settings" dialog can be found in
LIMS settings
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
5 - Work performed by the system administrator
Defining the balance / PC interface
85
Safety instruction
Strictly observe the safety instruction "Improper changes" under
Warning notes during operation
Defining the balance / PC interface
Proceed as follows:
Open the "Device configuration" dialog by selecting
Options > Configuration
.
Select the "DEVICE.INI" tab. Then select the "Balance Port" section by clicking the arrow next to the "Section" dropdown listbox.
In the listbox "Items" select the entry that you want to change and click
Edit
. The "Configure key value" dialog is displayed:
Enter the desired value in the "Value" field and click
OK
. The "Comment modification" dialog is displayed.
Enter a justification in the "Comment modification" dialog and click
Close
.
If necessary, repeat the steps mentioned above to modify further settings.
Click
OK
in the "Device configuration" dialog. Your settings are saved and the dialog is closed. A message window appears which informs that the modification will only become operative after the instrument software has been left and re-started.
Click OK and quit the operating software.
Restart the operating software as required.
Dialog details
Details on the "Device configuration" dialog can be found in
Device configuration
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
5 - Work performed by the system administrator
Editing analysis data
Target group
Personnel with good knowledge of the operating system and administrative settings.
Purpose
This section describes when it makes sense to edit analysis data and to what extent this is possible.
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When does it make sense to edit analysis data?
Reasons for modifying analysis data
The following reasons exist to edit analysis data:
If old calibration coefficients only exist as a hardcopy and you want to load them, you can manually input the calibration coefficients.
If you have created a template of the sample data for the measurements and you need to enter the samples still to be measured in the template.
If you input blank values manually because, for example, the blank value of the sample packing is already known.
Limits for modifying analysis data
Inserting and deleting lines
You cannot insert lines or delete lines between finished samples.
Editing sample data
You cannot edit the data of finished samples by simply clicking on the respective fields. You can recognize finished samples by the fact that they are above the current sample, which is highlighted by a green bar in the sample view. You can only edit finished samples by selecting Edit > Change ; if 21
CFR Part 11 functionality is enabled, this creates a new version.
Consequences of modifying analysis data
Commenting changes
If 21 CFR Part 11 functionality is enabled, the user must comment on certain changes.
Versioning
If 21 CFR Part 11 functionality is enabled, a new version of the document is created as soon as an analyzed sample is changed. The original version of the document is then write-protected.
Recomputing
After performing certain changes, you must update the calculations of the samples by selecting
Math.
> Recalculate
. The changes include:
Manual blank value input.
Subsequent review of calibration, specifying that standard samples should be displayed as monitor samples and no longer as calibration samples.
Changing the sample name.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
5 - Work performed by the system administrator
Performing checks
Target group
Personnel with good knowledge of the operating system and administrative settings.
Purpose
This section enables you to perform various checks as system administrator.
In this section
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Checking documents for authenticity
What signature is checked?
Only those signatures can be checked that are enabled in the "Verify digital signature" dialog and if their radio button is checked; for example the "created" signature. If the document already has multiple signatures, the user must select one to check.
Note
Note the following:
The signature program must be installed.
Signatures can only be checked or created if 21 CFR Part 11 functionality is enabled.
Checking a signature
Proceed as follows:
Open the document to check.
Open the "Verify digital signature" dialog in the operating software by selecting File > Verify .
Check the radio button next to the signature you want to check.
Click
Verify
. The program begins to check. The result is displayed in a message window and indicates whether the signature is authentic or not. "Good signature from..." indicates that the signature is authentic.
Signing documents
What signature is allocated?
The signature that is enabled in the "Sign" dialog and whose radio button is checked is allocated; for example, the "created" signature is allocated. The following rules apply:
The "created" signature is assigned to a document first.
The "checked" signature is assigned to a document if it already has a "created" signature.
The "released" signature is only assigned to a document if it already has a "created" and a
"checked" signature.
Note
Note the following:
The signature program must be installed.
Documents can only be signed if 21 CFR Part 11 functionality is enabled.
Only sign finished documents. After signing, the document is read-only.
Signing documents
Proceed as follows:
Open the "Sign" dialog in the operating software by selecting
File > Sign
.
Enter your name set up in the signature program in the "Name" field.
Enter your password set up in the signature program in the "Password" field.
Click
Sign
. The program checks whether you are authorized to sign the document. The result is displayed in a message window:: "GOOD_PASSPHRASE" indicates that you are authorized to create the signature. The signature has been created.
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Viewing the logbook
Viewing the logbook
Proceed as follows:
Open the logbook by selecting
Options > Logbook
.
Select the period for which to view the logbook. Open the "Select period" dialog by selecting
File
> Load
.
In the "Select period" dialog, use the arrows of the corresponding fields to set the year and month and then click
OK
.
The desired period - if available - is displayed in the logbook.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
5 - Work performed by the system administrator
Working with the database
Target group
Personnel with good knowledge of the operating system and administrative settings.
Purpose
This section enables you to perform various database tasks as system administrator.
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Database
What is a database?
A database is characterized by the following:
A database is an organized collection of data managed by a data management system.
Different users can access shared data in a database.
Databases allow the user to input, edit and delete data.
Databases permit searching and selecting data with the aid of filters.
Databases allow the user to create evaluations and statistics.
Databases allow the user to output data in the form of reports.
Maximum database size
The maximum size of the database is limited to 2 gigabytes. The software displays a warning if the size of the database exceeds 1 gigabyte or if available disk space is less than 1 gigabyte. In this case the database should be reorganized. See
Administrative work on the database
Database protection
If 21 CFR Part 11 functionality is enabled, the database protects you from:
Data loss. The sample data can only be overwritten as long as these samples have not yet been analyzed. Afterwards, a new file version is created retaining the same file name and the previous version. This allows you to track all changes to the sample data.
Data distortion. Authorized individuals can add an electronic signature to data documents; the authenticity of this signature can be verified. In addition, the activities of the indivdiual users are recorded in a logbook for tracking purposes along with a timestamp and user name.
Unauthorized access to data. There are various password-protected user levels. This allows you to restrict access to the various menu functions.
See
21 CFR Part 11 functionality
Administrative work on the database
Reorganizing the database
The software always works with one and the same database. Because the size of the database is limited to 2 gigabytes, it is necessary to reorganize the database regularly. Database reorganization removes all sample data and the contents of the logbook from the database file, but retains the other data such as settings, coefficients, etc.
Datebase backup
"Backup" copies the complete existing database file to a certain directory under a different name, thereby "capturing" a certain state.
Export and import
It is not possible to load and save data from/to a database in the usual way. However, by using the
File > Export/Import > Export
and
File > Export/Import > Import
menu functions it is possible to transport documents "out of" the database and to transport external documents "into" the database.
Restoring the database
"Restore" reloads an old database file and irrevocably deletes the current data.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
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Defining the autoexport directory
93
Safety instruction
Strictly observe the safety instruction "Improper changes" under
Warning notes during operation
Selecting a directory
Proceed as follows:
Open the "Device configuration" dialog by selecting
Options > Configuration
.
Select the "DEVICE.INI" tab. Select the "AutoExport" section by clicking the arrow next to the
"Section" dropdown listbox.
Select in the "Items" listbox the entry "directory" and click
Edit
. The "Configure key value" dialog is displayed:
Enter the desired dirctory in the "Value" field and click
OK
. The "Comment modification" dialog is displayed.
Enter a justification in the "Comment modification" dialog and click
Close
.
Click
OK
in the "Device configuration" dialog. Your settings are saved and the dialog is closed. A message window appears which informs that the modification will only become operative after the instrument software has been left and re-started.
Click
OK
and quit the operating software.
Restart the operating software as required.
Further information
Further information can be found in:
Database backup.
Database backup
What happens during backup?
Backup copies the complete existing database file to a certain directory under a different name, thereby "capturing" a certain state.
Backup settings
The following backup settings are available:
Auto-start backup:
daily
every X minutes
every X hours
once at a certain time
Start backup manually
Auto-save
The document currently open is automatically saved to a temporary file every 3 minutes if it is changed.
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Autoexport
Autoexport creates a backup of the current document as an sqlite file after every save or sub-save process. The advantage of this is that you do not always have to save the whole database. However, autoexport is only performed if you have defined a directory for saving backups. You can set this directory in the Configuration menu. The file name is as follows: xxxxx.YYMMDDhhmmss.mdb
. The file name consists of the following components:
Component xxxxx
YYMMDD hhmmss
Meaning
Document name
Current date (year, month, day)
Current time (hour, minute, second)
Important Notice
It cannot be ruled out that under some circumstances (power failure, defective PC etc.) the database file might be damaged. In most cases, a damaged database file is no longer useable.
Therfore, it is strongly recommended that you perform backups in appropriate intervals in order to allow to restore the damaged database file without major data losses. Backups should not be performed on the local harddisk but a safer strategie should be used (e.g. backup on a
PC of the network or on an external harddisk etc.).
Starting the database backup
Start backup
Proceed as follows:
Open the "Backup configuration" dialog by selecting
File > Backup/Restore > Database >
Backup
.
Click
Select
to specify the directory to save to. This displays the "Find folder" dialog.
Select the desired directory and click
OK
.
Click Backup now in the "Configure backup" dialog. The backup is performed.
Click
OK
in the "Configure backup" dialog to close the dialog.
The backup was successful.
Further information
Further information can be found in:
Database backup.
Configure backup
Reorganize database
What does reorganize mean?
Reorganization removes all sample data and the contents of the logbook from the database file, but retains the other data such as settings, coefficients, etc.
Safety instruction
Strictly observe the safety instruction "Working with the database" under Warning notes during operation
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Reorganize database
Proceed as follows:
Open the "Clean database" dialog by selecting
File > Backup/Restore > Database > Clean up
.
Click Backup now . You cannot reorganize the database without backing up. This displays the
"Select backup file name" dialog:
Enter a file name in the "File name" field and click
Save
. The database is saved.
Click
Reorganize
in the "Reorganize database" dialog. A message window appears which informs that now all sample data will be deleted.
Click
Yes
to continue the clean up procedure. The database is reorganized and the "Comment changes" dialog is displayed.
Enter a justification in the "Comment modification" dialog and click
Close
. You have now reorganized the databsse.
Reloading an old database file
Safety instruction
Strictly observe the safety instruction "Working with the database" under
Warning notes during operation
Reloading an old database file
Proceed as follows:
Open the "Restore Database" dialog by selecting
File > Backup/Restore > Restore
.
Perform a backup. To do so, click
Backup now
. This displays the "Select backup file name" dialog.
Enter a file name in the "File name" field and click
Save
. The database is saved.
Click
Restore
in the "Restore Database" dialog. This displays the "Select backup file name to restore" dialog.
Select the desired database file and click
Open
. A message window appears which informs that now all sample data will be deleted.
Click
Yes
to continue. The database is restored and the "Comment changes" dialog is displayed.
Enter a justification in the "Comment modification" dialog and click
Close
. A message window appears which informs that now the instrument software will be left automatically.
Click
OK
. This closes the operating software.
Restart the operating software as required.
Further information
Further information can be found in:
Restore database
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
5 - Work performed by the system administrator
Ways of optimizing the use of the analyzer
Target group
Personnel with good knowledge of the operating system and administrative settings.
Purpose
This section gives an overview of the ways in which you can optimize the use of the analyzer for your own particular application.
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Optimizing basic instrument settings
Analyzer configuration
You can optimize the following by means of configuration:
Interface properties
Signature program properties
Device parameter
See
Configure analyzer
Reacting to irregularities
If irregularities occur during the analysis, it is important for the user to quickly identify any errors. In the "Error handling" dialog the user defines how the analyzer is to react to incidents.
Incident
During analysis, the computed element contents exceed the defined tolerances.
A critical error occurs.
A non-critical error occurs.
Consequences
If standard tolerance monitoring is enabled, the analysis is aborted. "Tol" is displayed in the information column of the particular sample.
The analyzer is stopped after the analysis.
If you have set the analyzer to stop after a set number of non-critical errors and this number has been reached, the analyzer is stopped after the analysis.
See
Error handling
Defining custom methods
Depending on what sample substances you want to analyze, it may be necessary to define custom methods in addition to the default methods.
Methods allow to set certain parameters for sample specific requirements.
See
Defining custom methods
Sleep/wake-up behavior
For sleep/wake-up behavior, you can specify that conditioning samples in a series are measured before the first user starts work on the instrument in the morning. See
Optimizing sleep and wakeup behavior
Optimizing sample data editing
Facilitating input of samples
In the "Input options" dialog you can define settings that facilitate sample data input in the following cases:
An identical sample name is used several times.
You need to increment or decrement a figure in the sample names.
One method is used for numerous samples.
You need to input a daily factor for numerous samples.
You need to input a blank value for numerous samples.
See
Input options
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Prioritizing urgent samples
Via
Edit > Swap
you can prioritize urgent samples and analyze them earlier than scheduled.
However, in the solids modes the samples are only swapped in sample memory, and you have to swap the samples on the carousel by hand. If multiple determination is activated you always should swap all samples from one vial to all samples from the other vial instead of swapping only single samples.
See
Swap samples
Showing the weight window
Via
View > Weight window
you can show and hide the weight window. The weight window displays the last five sample weights input and the names of the associated samples. The current sample weight is displayed in a larger font. The weight window makes it easier for you to check whether the values were correctly transferred, particularly when automatically transferring weighing data.
Weighing in samples during the analysis
While one analysis is running, you want to weigh in further samples for another document. However, this is not possible as long as the analysis is running and the current document is open. However, you can generate the weighing data on another PC with the aid of the "Balance" program. Weighing data generated and saved with the "Balance" program can then be imported to the control PC via
File >
Import
. The condition is that the analyzer is back in standby mode or "sleeping".
Cf. "Balance" weighing data input program.
"Balance" weighing data input program
Ways of capturing weighing data
You can capture weighing data in the following ways:
Manually.
Automatically if the balance is connected to the control PC of the analyzer.
With the "Balance" weighing data program from BÜCHI Labortechnik AG.
Purpose of the program
The "Balance" program is used to capture weighing data in the following cases:
the balance is located in a different place to the analyzer and control PC.
While one analysis is running, you want to weigh in samples for another document. This is only possible, however, when the analyzer is "sleeping" or when no analysis is running. However, you can capture the weighing data with the aid of the "Balance" program and, if necessary, generate them on a different PC.
Weighing data format
The weighing data are in *dat format. Files with this extension created with the "Balance" program can be imported to the control PC. It is not, however, possible to import other files with the *dat extension.
Importing weighing data
Weighing data generated and saved with the "Balance" program can then be imported to the control
PC via
File > Export/Import > Import
. One of the following conditions must be met for import:
The analyzer is in standby mode, i.e. no analysis is currently running
or the analyzer is "sleeping".
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The following import options are available:
Import into an empty sample memory.
Import into a sample memory that is not empty.
Importing into an empty sample memory
After importing into an empty sample memory, the weighing data and any sample names are now in the sample memory. The weighing data are input starting from sample No. 1.
Importing into a sample memory that is not empty
Before importing into a sample memory that is not empty, a dialog is displayed in which the user must choose between two options:
The weighing data can be appended after the current weighed sample. This allows you to import multiple weighing data records.
The weighing data can be saved in a new document. The weighing data are saved there starting from sample No. 1. The current open document must be saved and then closed.
Optimizing data evaluation
Optimizing the view
The user can customize the view to his own needs:
Type of view
View of the sample view
Combi view in graph view
Combi view in calibration view
Combi view in statistics view
Cross-reference
Cf:
Configuring the sample view
Specifying the number of decimal places
Saving the sample view
Cf:
Configuring the graph view
Setting the size of the graph
See Setting the size of the graph
See
Configure statistics view
Optimizing report settings
The user can customize report settings to his own needs: possibilities of customization
Designing an analysis log
Printer setup
Defining printer settings
Assessing the print view
Cross-reference
See
See
See
See
Configure report
Printer setup
Print preview
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
5 - Work performed by the system administrator
Performing other administrator tasks
Target group
Personnel with good knowledge of the operating system and administrative settings.
Purpose
This section enables you to perform various tasks as system administrator.
In this section
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Modifying the registration
Dialog: "Product registration"
When you start the operating software for the first time, the "Product Registration" dialog is displayed.
Once you have registered, the dialog is no longer displayed when you launch the program.
Changing the registration
You must have administrator rights to modify the registration.
Modifying
Proceed as follows:
Launch the operating software.
Open the "Product registration" dialog by selecting
Help > Registration
.
If you want, enter your address data in the "User" section.
Enter the serial number in the field "Serial num." of the "Analyzer" section if you have not already done so. The serial number is found on the type plate on the back of the analyzer. This number should match the serial number of the installation CD cover when installing for the first time.
Enter the software ID in the field "Software ID" of the "Software" section. If installing for the first time, this number is found on the installation CD cover. If installing and upgrading, you must send the registration details in this dialog to BÜCHI. You will then receive an identification code to be entered here.
Click
OK
. This closes the dialog and saves the settings.
Printer setup
Printer setup
Proceed as follows:
Open the "Printer setup" dialog by selecting
File > Printer Setup
.
Select the desired printer type from the "Name" dropdown listbox.
Click
Properties
. A "Properties" dialog is displayed that varies depending on the type of printer connected.
Define your settings in the "Properties" dialog and then click
OK
. Your settings are saved and the dialog is closed.
Click
OK
in the "Printer setup" dialog. Your settings are saved and the dialog is closed.
You have successfully setup the printer.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
C H A P T E R 6
Starting up and shutting down the instrument
Target group
Personnel authorized by BÜCHI Labortechnik AG and having undergone training.
Purpose
This section enables you to start up or shut down the instrument according to instructions.
In this chapter
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
6 - Starting up and shutting down the instrument
Setting up and starting up the instrument
Target group
Personnel authorized by BÜCHI Labortechnik AG and having undergone training.
Purpose
This section enables you to set up and commission the instrument according to instructions.
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Rules for first-time start-up
First-time start-up
Observe the following rules for first-time start-up.
First-time start-up is performed by a trained service technician. Only the service technician may open the transport packaging. If the customer opens the transport packaging, this results in loss of warranty.
Make sure that the user is completely available for instruction and hand-over of the equipment at the time of first-time start-up. If additional instruction by our service technician is required, this must be billed separately.
If you do not order the PC and peripherals from BÜCHI, BÜCHI reserves the right to perform start-up with their own equipment. Any modifications of the analyzer must be performed by the customer.
The instrument is installed by a trained service technician, demonstrating performance with analyses of max. 10 standard measurments.
For special analysis problems, BÜCHI's application laboratory will draw up specific work instructions at the customers request and against payment.
Requirements for installing the instrument software
In order to install the software correctly, administrator rights for the PC must be available.
Conditions for operating the instrument software
Do the following to be able to operate the software without any problems:
On the PC where the software is installed, check power management settings under
Control
Panel > Power Management
or under
Control Panel > Power Options
. The following options must be set to "Never":
"Turn off monitor"
"Turn off hard disks"
"System stand by"
"System hibernates"
Power management must also be disabled in the PC's BIOS.
The PC on which the software is installed must not be overloaded with other software. This could cause unstable operation of the software.
Instructions for operating the furnace
Note
Observe the instructions for using the furnace so that the warranty is upheld. Further details can be found under Warranty on the furnace.
Installation site requirements
General requirements
Observe the general installation site requirements:
The analyzer must not be installed in areas with explosive atmosphere (in accordance with the
ATEX guideline).
Good ventilation.
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Room temperature should be constant.
Analyzer and peripherals must be protected from drafts and direct heat.
An air-conditioned room is advantageous as the analyzer emits heat.
Take suitable action to avoid electrostatic discharge. Electrical discharges can lead to malfunctions of the instrument.
Specific requirements
The following lists specific requirements to be met by the installation site
Type
Room
Instrument setup
Specific requirements
Mode of protection IP 20.
Dry room.
Well ventilated.
Only on heat-resistant surface.
A stable lab table is suitable as well.
Space required including PC and printer 1.30 m x 0.55 m (W x D).
Space required by instrument alone 0.48 m x 0.55 m x 0.55 m (W x D x H).
Clearance from instrument to wall
Ambient temperature
Mains voltage
Power connections
Gas supply
Waste gas lines
At least 20 cm clearance all round so that the fans will work.
Minimum: + 15°C.
Maximum: + 35°C.
100–230 Volt AC ± 10 %; 50–60 Hz.
Connection 1,4 kVA.
Mains voltage and frequency must match the specifications on the instrument's type plate.
2 power sockets and socket strip with 4 sockets to connect peripherals or 5 sockets.
Protection class I, protective conductor connection.
Fusing 16 A delay action.
Gas supply must be available nearby the instrument.
Connection to device by means of a pressure reducer.
Pressure reducer CO
2
and O
2
, two-stage each (2nd stage 0-3 bar), if possible with stop valve.
Necessary gas connection downstream of the pressure reducer: 2 x clamp ring screw connection for
6 mm tube diameter.
The complete gas intake line must use gas-loss-free components (copper, stainless steel, etc.).
The waste gas line "WASTE" must discharge into the open or into a vent, since otherwise the emitted carrier gas CO
2
will be enriched in the laboratory.
The end of the waste gas line must discharge into the open at a location protected from the wind.
Gases and chemicals to be provided
Gases and chemicals to be provided
The following lists the gases and chemicals required.
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6 - Starting up and shutting down the instrument 107
Category
Carrier gas
Combustion gas
Reagents
Calibration standards
Type
CO
2
:
Purity: 99.995 %
Consumption approx. 700 ml/min
Adjust the intake pressure at the delivery point until the PC pressure display "Input" reads 1350 mbar.
Oxygen:
Purity: 99.995 %
Intake pressure 2.5 bar
Various chemicals for filling the reaction tubes
Part of initial equipment
No
No
Yes
You need a consumables set for further analyses.
Yes Aspartic acid
Substances must have at least p.a. quality or be certified for elemental analysis.
Start-up
Who performs first-time start-up?
First-time start-up is performed by a trained service technician, not the customer.
Note
In order to ensure proper working order of the instrument:
the work processes described in this section must be performed precisely.
the basic instrument and the peripherals must be switched on in the sequence described here.
Process
The section is divided into the following phases:
Preparing instrument for switching on
Preparing the Instrument for measurements
Performing instrument checks
Phase 1: Preparing instrument for switching on
Proceed as follows:
Set up the instrument. Observe the instructions concerning the installation site. See Installation site requirements.
Connect the peripherals. See
Connecting peripherals
Connect supply lines and waste gas lines. See Connecting supply lines and waste gas lines.
Remove the transport lock. See Removing the transport lock.
Check the fillings of the required glass and quartz components. Replace filling if necessary. See
Filling the drying tube
Filling the combustion tube.
Filling the post combustion tube.
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Install the required parts. Leave the tube outlets open for subsequent conditioning. Used tubes also need to be conditioned. See
Installing reaction tubes in the furnace and conditioning.
Removing and installing the drying tube.
The instrument is now ready for switching on.
Phase 2: Instrument must be ready to measure
Proceed as follows:
Perform all steps of the switching on process. See
Switching on
Switch on the operating gases. See Default instrument settings for recommended gas pressure.
Launch the operating software. The standard operating parameters are factory-set. See
Starting the operating software
Heat up the furnace. See Heating up the furnace .
Condition the reaction tubes. See Installing reaction tubes in the furnace and conditioning.
Define the main settings for measurement. See Measurement settings
The instrument is then ready to measure.
Phase 3: Performing instrument checks
Proceed as follows:
Perform a leak test. See Performing a leak test.
If the leak test reveals any leaks, eliminate them.
Condition newly installed and used tubes. For used tubes, humidity must be eliminated by baking them out for at least two hours. See Installing reaction tubes in the furnace and conditioning.
Check proper working order of the instrument by means of
Blank value determination
Conditioning measurement
Standard measurement
Observe gas flows and pressures. See Performing routine measuring work.
After routine measuring work you can measure real samples. See
Performing measurement work
Connecting peripherals
Note
The following section is part of initial start-up. All steps described in initial startup before connecting peripherals must have already been performed. See Start-up.
Peripherals
A PC must be connected. It is essential for operation.
A printer should be connected so that you can print out measuring results.
A balance should be connected, so you do not need to enter the sample weight by hand.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
6 - Starting up and shutting down the instrument
Connecting peripherals
The following picture shows a detail of the rear of the analyzer with the corresponding connections:
Legend:
1 "PC" PC connector (USB)
2 "Reserve" reserve
3 "~" mains connector
109
Configuring the balance
The serial interface parameters of a connected balance must match the parameters of the PC's serial interface. If you have not entered anything different, the operating software configuration file sets the
PC's serial interface as follows:
Baud: 2400
Data bits: 7
Stop bits: 1
Parity: odd
Select
Options > Configuration
to edit the parameters of the PC's serial interface if your balance requires different settings.
Connecting supply lines and waste gas lines
Note
Proceed as follows:
Connect the PC to the appropriate connector (1) on the back of the analyzer using the correct cable.
Connect the power supply cable to the mains connector (3).
If you wish, connect a printer to the PC.
If you wish, connect a balance to the PC.
The following section is part of initial start-up. All steps described in initial startup before connecting supply lines and waste gas lines must have already been performed. See Start-up.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
6 - Starting up and shutting down the instrument
Detail of the rear
The following picture shows a detail of the rear of the analyzer with the corresponding gas connections:
Legend:
1 "CO
2 "O
2
IN" CO
2
IN" O
2
2
gas inlet
gas inlet
3 Gas outlet
4 "WASTE" waste water outlet
110
Connecting supply lines
Safety instruction
Strictly observe the safety instruction "Mixing up gas inlets" under
Warning notes during operation
Proceed as follows:
Connect the CO
2
supply tube to the CO
2
gas inlet (1).
Connect the oxygen supply line to the oxygen gas inlet (2).
Connecting waste gas lines
Proceed as follows:
Connect the waste gas line to the gas outlet (3).
Install the other end of the waste gas line so it discharges into the open or into a vent.
If the waste gas lines discharge into the open, make sure that the waste gas lines discharge into the open at a location protected from the wind. Otherwise detector instabilities may occur.
Connect the wastewater line to the wastewater outlet (4).
Lead the upper end of the wastewater line into the storage vessel.
Check the fill level of the vessel regularly.
Removing the transport protection
Types of transport protections
There are two types of transport protections:
Furnace transport protection.
Water trap transport protection
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6 - Starting up and shutting down the instrument 111
Purpose of the transport protections
The transport protections prevent...
... the furnace section from slipping on its rails while the analyzer is being transported.
... the loosely attached water trap from damages while the analyzer is being transported.
Removing the furnace transport protection
Proceed as follows:
Open the front door of the instrument.
Push the right side door open from inside (magnetic lock). The transport protection is now visible in the form of a bracket (1).
Unscrew the screws and remove the bracket.
Fasten the bracket on the rear casing angle (1). It should be stored there so it does not get lost.
Close the right side door and screw the big screw back in that keeps the door closed.
Removing the water trap transport protection
Proceed as follows:
Open the front door of the instrument.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
6 - Starting up and shutting down the instrument
Push the left side door open from inside (magnetic lock). The water trap (1) and the transport protection (5) are now visible.
112
Loosen the ground-in clamp (3) which connects the glass tube with the gas drying and the water trap.
Unscrew the two caps (2) with the ground joint (4).
Remove the two transport protection (5).
Screw the two caps with the ground joint (4) firmly.
By means of the ground-in clamps (3), connect the ground-in ball-and-socket joints with the glass tube again.
Switching on
Note
The following section is part of initial start-up. All steps described in initial startup before switching on must have already been performed. See Start-up.
Switching on
Proceed as follows:
If not done so far, plug the power supply plugs of the analyzer and the peripherals into the sockets.
Turn on PC, monitor and printer. Wait until the boot process is completed.
Install the operating software if you have not already done so. See
Installing and updating the software
Switch the main instrument switch on. The instrument performs an initialization routine as well as a reference run of the ball valve and the sample carousel. Wait until this process is complete.
You have now switched on the instrument.
Default instrument settings
Default instrument settings
The default gas pressure and mass flow settings are listed below. The settings require the analyzer to be leak-free.
O
2
intake pressure
O
2
intake pressure is set to 2.5 bar at the delivery point.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
6 - Starting up and shutting down the instrument
CO
2
intake pressure
CO
2
intake pressure is set at the delivery point so that the following value are displayed on screen:
The "Input" display shows approx. 1350 mbar.
Flow rate
The following flow rate settings are typical:
The "MFC CO2" display shows approx. 700 ml/min for the measuring gas outlet.
During standby, the "MFC O2" display shows 0 ml/min. Only during the combustion the corresponding O2-value will be displayed.
During standby, the "Flow CO2" display shows the carbon dioxide flow approx. 700 ml/min.
The flow value may fluctuate during the combustion.
Heating up the furnace
113
Heating up the furnace
Note
Note the following:
The following section is part of initial start-up. All steps described in initial startup before "Heating up the furnace" must have already been performed. See Start-up.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
6 - Starting up and shutting down the instrument
Shutting down the instrument
Target group
Personnel authorized by BÜCHI Labortechnik AG and having undergone training.
Purpose
This section enables you to shut down the instrument according to instructions.
In this section
114
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6 - Starting up and shutting down the instrument 115
Shutting the instrument down for short measuring breaks (standby)
What are short measuring breaks?
Short measuring breaks are breaks that last overnight or for 2-5 days.
Procedure
The analyzer and the PC stay online during short measuring breaks. Only the sleep function is activated for the instrument.
Setting the analyzer sleep function.
Proceed as follows:
Open the "Sleep/wake-up functions" dialog in the operating software by selecting
Options >
Settings > Sleep/Wake-up
.
Define when to enable the sleep function. Select one of the following options:
Sleep now...
(button): The instrument is shut down immediately.
"Sleep after end of sample": The instrument is shut down after finishing the last sample.
"Sleep at sample No.:": The instrument is shut down prior to the appropriate sample.
Check "Shut off carrier gas".
Check the appropriate checkbox in front of the combustion tube and turn off the associated heater.
Specify when to "wake up" the instrument again. The working temperatures are increased again and the instrument is flushed with gas. Choose one of the following options:
Enter "Date" and "Time" when to "wake up" the instrument and select the box next to "Onetime wake-up at above time/date".
Enter a "Time", select the box next to "Daily wake-up at above time, except:" and select the weekdays on which you do not want to wake up the instrument.
If you shut down the instrument in the middle of a series, you can continue this series after
"wake-up". To do so, check "Continue after wake-up if there are samples".
Click
OK
to close the window and save your settings. The instrument is shut down and woken up again according to your settings.
Shutting the instrument down for long measuring breaks (switching off)
What are long measuring breaks?
Long measuring breaks are breaks that last longer than 5 days.
Preparing the instrument for long measuring breaks.
Proceed as follows:
Shut off the gas supply.
Switch off the furnace in the operating software. Open the dialog via
System > Furnace
.
Wait 2–3 hours until the instrument has cooled down to <55 °C.
Quit the operating software. Execute the following command:
File > Exit
.
Switch off the analyzer and its peripherals.
Disconnect the analyzer from the mains. Disconnect the power supply plug. The instrument is ready for long measuring breaks.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
6 - Starting up and shutting down the instrument
In case the analyzer has to be transported, mount the corresponding transport protection(s) again.
116
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
C H A P T E R 7
Using the instrument
Target group
Personnel with basic knowledge of chemistry and experience with laboratory work, e. g. chemistry laboratory workers.
Purpose
This section enables you to perform measurements with the instrument.
In this chapter
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
7 - Using the instrument
Measurement settings
Target group
Personnel with basic knowledge of chemistry and experience with laboratory work, e. g. chemistry laboratory workers.
Purpose
This section enables you to define the necessary settings for measurements.
In this section
118
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7 - Using the instrument 119
Defining keywords for blank and conditioning samples
Keywords
Names of blank samples and conditioning samples must be defined as keywords so the software recognizes and handles the samples as blank or conditioning samples.
Factory-set key words
The following keywords are factory-set:
For blank samples:
Blnk
For conditioning samples:
Run In
Defining custom keywords
Proceed as follows:
Open the "Keywords" dialog in the operating software by selecting
Options > Settings >
Keywords
.
Enter the desired keywords in the appropriate boxes.
Click
OK
. This closes the dialog and saves the settings.
Viewing list of defined factor, monitor and standard samples
Viewing the list
Proceed as follows:
Open the "Standard samples" dialog in the operating software by selecting
Options > Settings >
Standards
.
The list box displays all currently defined standards. By checking the requested standard sample the settings are displayed in the right area of the dialog.
Defining custom standard substances
Defining custom standard substances
Proceed as follows:
Open the "Standard samples" dialog in the operating software by selecting
Options > Settings >
Standards
.
Click
New
. The input boxes on the right area are now empty. Enter the data of the standard sample to be newly defined.
For the substance, enter...
... the name of the substance in the "name" field.
... the theoretical element content in percent in the "Conc. [%]" fields (or in ppm in the
"Conc. [ppm]" fields respectively). If you enter 0 for the theoretical element content of a substance element, the element is ignored in the calculation.
... the permissible tolerance for each element in the "Tolerance [%]" fields (usually 5%).
Click Create . Your new standard sample will now be included in the list in the left area of the dialog.
You have now defined the standard substance.
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Click
Close
to close the dialog.
Required substances
Different amino acids like e.g. aspartic acid, glutamic acid or uric acid have been proven to be advantageous.
Theoretical element contents of standard substances
The following tables lists the theoretical nitrogen contents of the standard substances used in the calibration tables:
Standard substance
Aspartic acid
Glutamic acid
Uric acid
N theor
[%]
10.52
9.52
33.33
Defining standard substances as factor and monitor samples
Background
Factor samples are required for routine measuring work. Monitor samples are required for standard tolerance monitoring. In order to compute factor and monitor samples correctly and to display them with their computed element contents in the sample view, it is necessary to define the standard substances as factor and monitor samples.
Defining standard substances as factor and monitor samples
Proceed as follows:
Open the "Standard samples display" dialog in the operating software by selecting
Math. >
Standard samples
.
Select the option "Show as measuring sample (measured concentration)".
Click
OK
. This closes the dialog and saves the settings.
Defining standard substances as calibration samples
Background
These operating instructions contain specific rules for the calibration. If you want to use these rules, you must define the standard substances used there as calibration samples. Of course, you can also use different substances but then you must develop the calibration rule yourself.
Defined calibration samples are displayed along with their theoretical contents in the sample view.
Defining standard substances as calibration samples
Proceed as follows:
Open the "Standard samples display" dialog in the operating software by selecting
Math. >
Standard samples
.
Select the option "Show as calibration sample (theoretical concentration)".
Click
OK
. This closes the dialog and saves your settings.
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Specifying the computation method for blank value and daily factor
121
Defining the blank value calculation method
Proceed as follows:
Open the "Configure Calculations" dialog in the operating software by selecting
Options >
Settings > Calculation
.
In section "Blank value determination" define the calculation method:
If you...
... select "sequentially" a separate blank value is computed for every element in every group of blank value samples; this value is entered in the respective blank value column until the next group of blank value samples.
... select "entirely" all blank value samples in the series are used to compute the blank value. This blank value is then applied to all samples in the series.
... select "manual input" blank value calculation is not performed - even if there are blank samples in the series. This allows manual input of blank values for individual samples.
... "autom. activate "automatic blank value calculation" the blank value is automatically computed at the end of every analysis. This option ist not available if manual input has been checked.
Then click
OK
to save your settings.
Defining the daily factor calculation method
Proceed as follows:
Open the "Configure Calculations" dialog in the operating software by selecting
Options >
Settings > Calculation
.
In section "Factor determination" define the calculation method:
If you...
... select "sequentially" then the daily factor is computed group-by-group and changes throughout the day.
... select "entirely" the daily factor is computed on the basis of all factor samples in the file.
An average factor is computed.
... select "manual input" factor calculation is not performed - even if there are factor samples in the series. This allows manual input of daily factors for individual samples.
... "autom. activate "automatic factor calculation" the factor is automatically computed at the end of every analysis. This option ist not available if manual input has been checked.
... activate "upper/lower calib. range distinction" both for the upper and lower calibration range separate factors will be calculated. This requires separate factor samples for each range.
Then click
OK
to save your settings.
Enabling/disabling acoustic signals
Enabling/disabling acoustic signals
Proceed as follows:
Open the "Acoustic signals" dialog by selecting
Options > Settings > Acoustic Signals
.
Decide:
If you want to...
... switch on a signal, check the appropriate checkbox.
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7 - Using the instrument 122
... switch off a signal, uncheck the appropriate checkbox.
Click
OK
. This closes the dialog and saves the settings.
Configuring error handling
Reacting to irregularities
If irregularities occur during the analysis, it is important for the user to quickly identify any errors. In the "Error handling" dialog the user defines how the analyzer is to react to incidents.
Incident
During analysis, the computed element contents exceed the defined tolerances.
A critical error occurs.
A non-critical error occurs.
Consequences
If standard tolerance monitoring is enabled, the analysis is aborted.
Tol
is displayed in the information column of the particular sample.
The analyzer is stopped after the analysis.
If you have set the analyzer to stop after a set number of non-critical errors and this number has been reached, the analyzer is stopped after the analysis.
Configuring error handling
Proceed as follows:
Open the "Error handling" dialog in the operating software by selecting
Options > Settings >
Error handling
.
If you want to enable standard tolerance monitoring, check the "activated" checkbox in the
"Standard tolerance monitoring" section. The tolerance thresholds are defined via
Options >
Settings > Standards
.
If you want to abort the analysis after several non-critical errors, enter the number of errors in the
"No. of errors" textbox of the "Abort auto analysis" section. Enter
0
to ignore non-critical errors.
Click
OK
. This closes the dialog and saves the settings.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
7 - Using the instrument
Preparing samples
Target group
Personnel with basic knowledge of chemistry and experience with laboratory work, e. g. chemistry laboratory workers.
Purpose
This section enables you to prepare samples properly.
In this section
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Sample preparation instructions
Samples with potential risks
Various sample substances can pose a risk to the user during the analysis:
Contact with the substances may lead to chemical burns or poisoning.
Combustion analysis of larger quantities of the substance may lead to explosions.
These sample substances include:
Aggressive chemicals such as acids or alkaline solutions
Organic solvents
Explosives
Substances that develop toxic or explosive gas mixtures.
Users are obliged to protect themselves prior to contact with hazardous substances and to reduce the quantity of the substance to a safe amount. Users are also obliged to observe the safety instructions of the chemical manufacturer on the label of the bottle or in the safety data sheets. The safety data sheets contain risk information about a chemical in the R-Phrases and safety information in the S-
Phrases.
Sampling and homogenization
Refer to the relevant literature concerning the problem of sampling and homogenization.
Sample crushing and drying
When crushing and drying samples you may lose highly volatile constituents. Also, the sample may get contaminated with foreign substances.
What influences analysis results?
The following influences analysis results:
In nitrogen analysis, inclusions of air in the samples influence analysis results. Inclusions of air must therefore be avoided.
The moisture content of samples influences the analysis result through its weight proportion.
Determining sample weight
What is optimal sample weight?
Optimal sample weight is determined by the following
the N content of the corresponding sample to be measured,
the homogeneity,
the valid calibration,
the combustion behavior of the sample,
the oxygen requirement,
the pressure arising during combustion,
and that combustion of the sample is limited in time and controllable in terms of pressure.
Determining sample weight with known substances
The following rule of thumb applies to determine the sample weight of known substances:
The sample weight should be as high as necessary and as low as possible.
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The result will be that the nitrogen content is well measurable and you will achieve an optimum in catalyst consumption as well as in maintenance effort. Generally, you should prefer to carry out multiple measurements with lower weights instead of fewer measurments with higher weights.
Determining sample weight with unknown substances
Proceed as follows:
Start with a sample weight at approx. 300 mg.
Observe the behavior of the pressure during combustion at the flow meters of the instrument.
It has to be observed that during combustion phase the PC display "Flow CO2" does not drop below 200 ml/min. Otherwise there is a risk of pressing soot and tar into the gas supply tubes
(soot filter will turn to a dark color).
Caution:
In case of too high combustion pressure (PC display "Flow CO2" shows 0) the gas flow control unit of the instrument will soil!
Showing or hiding the weight window
Showing or hiding the weight window
Select
View > Weight window
to show or hide the weight window:
If "Weight window" is checked, the weight window is displayed.
If "Weight window" is not checked, the weight window is hidden.
Packing samples
Sample packing
The following types of sample packing may be used depending on the type of sample:
Foils
Boats
Capsules
Pelletizing in nitrogen-free paper
Pelletizing wihout packing material
The following sample packing materials may be used depending on the type of sample:
Tin
Nitrogen-free paper
Sample packing rules
Observe the following rules in order to achieve reliable measuring results:
There must be no body fat or sweat on the packing material. Therefore, do not touch the boats or other packing material with your hands. Work with tweezers or with gloves. Flush capsules free of air with CO
2
if necessary.
Avoid loss of substance after weighing. Therefore, wrap the substance exactly in the foil and close capsules gas-tight.
Minimize air inclusions in the sample material as they distort the N value. Therefore, compress sample packets and flush capsules free of air.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
7 - Using the instrument
Packing fatty, humid and non-pelletizeable solid samples - packing with tin film and/or tin boats
Examples of solid samples of this matrix include sausage, cheese, meat, yeast (fat and humid), dry yeast, soil, oily samples which release oil when pressed and small sample weights (calibration standards). Proceed as follows:
Tare the tin film or tin boat to zero.
Fill in the sample.
Close the tin film or tin boat over the sample either by hand or with the aid of tweezers.
Use the hand press to shape the sample and press out any air.
Weigh the sample and insert it on the carousel.
Packing dry and very fine solid samples - pelletizing in nitrogen-free paper
Examples of such samples include among others milk powder, whey powder, fertilizer and factor samples (300 mg aspartic acid). Proceed as follows:
Shape the paper into a cup shape.
Tare the paper to zero.
Fill in the sample.
Twist the paper edges above the sample together.
Place the packet into the pressing tool.
Apply the press ram.
Shape a pellet with the pelletizer (lever press).
Weigh the pellet.
Insert the pellet on the carousel.
126
Packing pelletizeable solid samples - pelletizing without packing material
Examples of such samples include grain and animal feed. Proceed as follows:
Fill sample directly into the pressing tool.
Apply the press ram.
Shape a pellet with the pelletizer (lever press).
Weigh the pellet.
Insert the pellet on the carousel.
Packing liquid or pasty samples - packing with tin capsules
Examples of such samples include juice, ice cream, mush, molasses, curd and yogurt. Proceed as follows:
Tare the tin capsule to zero.
Put the tin capsule into the capsule press.
Fill in the sample using a pipette or syringe.
Flush the capsule free of air with CO
2
.
Close the capsule air-tight.
Weigh the sample
Insert the capsule on the carousel.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
7 - Using the instrument
Preparing measurement work
Target group
Personnel with basic knowledge of chemistry and experience with laboratory work, e. g. chemistry laboratory workers.
Purpose
This section enables you to prepare measurement work.
In this section
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Software usage rules
Software usage rules
Observe th following rules in order to avoid disruptions during analysis:
The control PC must not be used simultaneously as an office workstation as this may lead to software instability.
Observe the following if using the operating software and other software at the same time:
Programs that heavily burden the PC may cause disturbances.
Programs that access the same serial interface as the analyzer operating software cause the analyzer to crash totally! Therefore, avoid running multiple programs simultaneously if you are not sure about how they work.
Only standard Windows screensavers may be used.
Starting the operating software
Starting the operating software
Proceed as follows:
Launch the operating software:
by double-clicking the appropriate icon on your screen or
by launching the program via
Start > Programs
or
by executing the program via the appropriate path.
Enter the following in the "Log in as" dialog:
In the field...
... "User" enter your user name.
... "Password" enter your password.
... "Domain" enter the name of your domain if the PC is connected to a network and the user management is defined on that network. If the PC is operated without a network or the user management is defined on the local PC this field has to be kept empty.
Click
OK
in the "Log in as" dialog. The user interface is displayed.
Showing or hiding the toolbar
Showing or hiding the toolbar
Select
Windows > Toolbar
to show or hide the toolbar:
If the menu command is checked, the toolbar is displayed.
If the menu command is not checked, the toolbar is hidden.
Waking up the instrument
Waking up the instrument
Proceed as follows:
Wake up the analyzer by selecting
System > Wake Up
.
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The carrier gas is reactivated and the furnace is heated back up to their working temperatures.
Viewing method settings
Background
A method includes several parameters which are necessary for the measurement.
Viewing the settings
Proceed as follows:
Open the "Methods" dialog in the operating software by selecting
Options > Settings >
Methods
.
Select the requested method from the list in the left area of the dialog. In the right area of the dialog the settings of the individual parameters of the selected method are displayed.
Click
Close
to close the dialog again.
Defining custom methods
View and define methods
In the "Methods" dialog you can view existing methods or define new methods.
View existing methods
Proceed as follows:
Open the "Methods" dialog in the operating software by selecting
Options > Settings >
Methods
.
In the left field, select the appropriate method. In the fields at the right side the parameters of the selected method are now displayed.
Click
Close
to close the dialog again.
Defining custom methods
Proceed as follows:
Open the "Methods" dialog in the operating software by selecting
Options > Settings >
Methods
.
Click
New
. The input boxes on the right of the dialog are now empty. Enter the parameters of the method to be newly defined:
Enter the following:
Enter the name of your method in the "ID" field.
Enter the purpose of the method, for example, in the "Description" field.
Input the corresponding method parameters in the other boxes.
Click
Create
. Your new method will now be included in the list in the left area of the dialog. You have now defined the method.
Click
Close
to close the dialog.
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Defining the Kjeldahl factor
130
What is the Kjeldahl factor used for?
It has been well documented that measurement bias exists between the classic wet chemical Kjeldahl method and the high temperature combustion Dumas method (cube instruments). Bias has also been documented between Kjeldahl methods using mercury based catalysts and other less toxic catalysts.
The basis of the bias is generally believed due to the less than 100% recovery for the Kjeldahl method for certain forms of nitrogen. So, the Dumas method will often measure a higher value of nitrogen compared to Kjeldahl.
Certain industries still require nitrogen values based on the historical Kjeldahl recovery. The “Kjeldahl
Factor” may be used to normalize the nitrogen results measured by the D-480 to their Kjeldahl equivalent values.
A Kjeldahl factor can be assigned to each Method. This factor (typically between 0.99 to 0.97) is multiplied to the nitrogen (and protein) results. The Kjeldahl factor however does not influence the values for standard samples. If the Kjeldahl factor is set to 1.00, no Kjeldahl adjustment will be made.
The inclusion of the Kjeldahl factor into the methods allows users to specify different factors for different types of samples.
Defining Kjeldahl factor in a method
Proceed as follows:
Open the "Methods" dialog in the operating software by selecting
Options > Settings >
Methods
.
In the left field, select the appropriate method.
Enter the appropriate value in field "Kjeldahl factor".
Then click Save . Your modifications will be saved.
Click
Close
to close the dialog. You have now defined the Kjeldahl factor in a method.
Copy methods
Defining custom methods
The existing method can be copied with the option "Copy methods" and subsequently the parameters of the corresponding requirements can be changed accordingy. In a lot of cases this is more efficient than creating a new method and entering all parameters.
Copy methods
Proceed as follows:
Open the "Methods" dialog in the operating software by selecting
Options > Settings >
Methods
.
Select a method from a list in the left area which parameters are most similar to the new method.
Enter the parameters of the method to be newly defined:
Enter the following:
Enter the name of the new method in the "ID" field.
Enter the purpose of the method, for example, in the "Description" field.
Change the corresponding method parameters in the other boxes accordingly.
Click
Create
. Your new method will now be included in the list in the left area of the dialog. You have now successfully copied and defined the method.
Click
Close
to close the dialog.
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Settings for sample input
Facilitating input of samples
You can define settings to facilitate sample insertion in the following cases:
An identical sample name is used several times.
You need to increment or decrement a figure in the sample names.
One method is used for numerous samples.
You need to input a daily factor for numerous samples.
You need to input a blank value for numerous samples.
Define settings
Proceed as follows:
Open the "Input options" dialog in the operating software by selecting Options > Settings >
Input
.
Select one of the radio buttons to specify sample name input. For selection of one of the bottom two radio buttons you must also specify the increment/decrement interval by using the arrows buttons.
Effect of the option...
... "Normal sample name input": The sample name is entered in the appropriate column as it is input.
... "Apply sample name": After entering the sample name and pressing Enter, the input name is applied to the next line as a suggestion.
... autom...."Auto-increment the number in the sample name": If a sample name ends with a number (e.g. "Name001"), this figure is automatically incremented by a certain amount and suggested for the next sample (e.g. "Name002").
... "Auto-decrement the number in the sample name": Works the same way as autoincrement, only the figure in the name is decremented.
... "Increment/decrement interval": Defines the amount the number in the sample name is increased/decreased.
If you have activated one of the options "Auto-increment the number in the sample name" or
"Auto-decrement the number in the sample name" you have to set the interval value in the textbox "Increase/decrease interval" by means of the arrow buttons.
Check the checkbox next to the appropriate options.
Effect of the option...
... "Fill method names to stop marker": The method name input for the first sample is entered for all subsequent samples up to the stop marker.
... "Fill daily factors to last sample": The daily factor input for the first sample is entered for all subsequent samples.
... "Fill blank values to last sample": The blank value input for the first sample is entered for all subsequent samples.
Click
OK
. This closes the dialog and saves the settings.
Importing weighing data
Importing weighing data
Proceed as follows:
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Open the "Open" dialog by selecting
File > Export/Import > Import
.
Select the "Balance Files (*.dat)" file type from the "File type" dropdown listbox.
From the dropdown listbox select the directory containing the weighing data file.
Select a file and click
Open
.
Decide:
If you import into...
... an empty sample memory: The weighing data are saved to sample memory starting at
No. 1. Save the document. The import is finished.
... a sample memory that is not empty: The "Reading Balance file" dialog is displayed. Go to the next step.
Select the desired radiobutton in the dialog:
If you...
... select "Append samples as from the current weighed sample": The weighing data are stored starting after the current sample weight.
... select "Create new document": The weighing data are saved in a new document.
Click
OK
. The weighing data are imported and displayed in the sample field.
Save the document. The import is finished.
Prioritizing urgent samples
Prioritizing urgent samples
Proceed as follows:
Open the "Swap samples" dialog in the operating software by selecting
Edit > Swap
.
Enter the numbers of the samples to swap in the textboxes in the dialog. Then click
OK
.
This closes the dialog and the samples are swapped in the sample memory.
Manually swap samples in the carousel.
Optimizing sleep and wake-up behavior
What can you optimize?
You can set sleep/wake-up behavior so that conditioning samples in a series are measured before the first user starts work on the instrument in the morning.
Note
Remember to prepare the appropriate conditioning samples and to sort them into the carousel after the samples of the last measurement of the day.
Optimizing sleep and wake-up behavior
Proceed as follows:
Open the "Sleep/wake-up functions" dialog in the operating software by selecting
Options >
Settings > Sleep/Wake-up
.
The last measurement of the day must be stopped before the appended conditioning samples.
To do so, select the radio button next to "Sleep at sample No." in the "Sleep" section. In the box next to it, enter the sample number at which you want the instrument to sleep; it corresponds to the first conditioning sample.
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In the "Wake-up" section, enter the time and days on which to wake up the instrument.
To do so, check the checkbox next to "Continue after wake-up if there are samples".
Click
OK
. This closes the dialog and saves the settings. The conditioning samples will be processed the next time the instrument wakes up.
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Performing measurement work
Target group
Personnel with basic knowledge of chemistry and experience with laboratory work, e. g. chemistry laboratory workers.
Purpose
This section enables you to perform all measurement work.
In this section
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Values for oxygen dosing
Meaning of oxygen dosing
The following illustrate the meaning of oxygen dosing:
If oxygen supply is insufficient, the catalysts are reduced and thus limited in their effect and durability. The unburnt sample substance remains in the ash finger and distorts the results of analysis of subsequent samples.
If your sample matrix is always the same, it is advisable to optimize oxygen dosing for reasons of costs.
How oxygen dosing takes place
Oxygen dosing takes place by allocation of the corresponding dosing parameters via a method.
By choosing a method you specify values for the following parameters:
O
2
dosing time
O
2
dosing flow
O
2
cut-off threshold
Comments:
The O
2
dosing time is a minimum dosing time.
The O
2
dosing flow is based upon the weight and the carbon and/or fat content of the sample.
Rule of thumb: 500 mg organic substance requires 0.4 - 0.5 litres oxygen for combustion. At a present O
2
dosing time of 120 sec, a flow value should be set to 200 - 250 ml/min.
The percentage of the O
2
cut off threshold is referred to the peak maximum (e.g. 10% - 30%).
The software automatically scans the course of the peak; the peak maximum will be registered.
The O
2
dosing cuts off after the current peak value has dropped below the cut off threshold
(percent of the maximum peak value) and if the O
2
dosing time has expired.
Further method parameters
By choosing a method you also specify values for the following parameters in addition to O
2 time:
dosing
Autozero delay
Peak anticipation
Integrator reset delay
Base weight
Kjeldahl factor
Viewing the settings
Information can be found under
Viewing method settings
Optimize O
2
dosing
If your sample matrix is always the same, it is advisable to optimize oxygen dosing for reasons of costs. Proceed as follows:
Measure a typical sample of known element content several times with the same sample weight
(max. ± 2 mg fluctuation).
Systematically increase O
2 widening of the N peak.
cut off threshold until you get a false low reading or a substantial
Set the O
2
cut off threshold of the last successful measurement before the false low reading occurred. These settings are optimal for this matrix and sample weight.
Check whether oxygen dosing is generally usable. To do so, measure several known samples of similar matrix.
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Example for optimization of oxygen dosing
136
O
2
cut off threshold = 30 %, total O
2
O
2
cut off threshold = 40 %, total O
2
amount = 589 ml
amount = 478 ml
Performing measurements
What you need to know
You must have read the Oxygen dosing values section so you can set the correct values for measuring.
When is routine measuring work necessary?
You must perform routine measuring work before measuring real samples:
if you have not performed any routine measuring work today
if measuring breaks exceed a duration of 2 hours.
Measuring real samples with preceding routine measuring work
Please observe the following instruction:
Caution Inserting multiple samples into the ball valve (for solids mode only)
If there are samples in the carousel while you are changing the position of the carousel via System > Sample Position , multiple samples may fall into the ball valve at the same time. In this case, a service technician is required.
Before changing the position of the carousel, always remove all samples from the carousel.
Proceed as follows:
Move the empty carousel to zero position. To do so, open the "Set carousel position" dialog in the operating software by selecting
System > Sample Position
.
Select the radio button next to "Reference run" and click
OK
. The carousel moves to zero position.
Prepare the samples.
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If necessary, prepare samples for determining the blank value.See Types of blank value determination and their settings.
Prepare conditioning samples for conditioning. Settings can be found in Performing routine measuring work.
Prepare the samples for determining the daily factor. Settings can be found in Performing routine measuring work.
Prepare the real samples. Cf. Sample preparation instructions
Insert the samples on the carousel.
Enter the weight in [mg] in the sample view (text view) on the PC if it has not already been transmitted online by the balance.
Enter the sample name (max. 32 characters) in the sample view (text view):
Blank values must have the keyword defined via
Options > Settings > Keywords
(factory set to "Blnk").
Daily factor or calibration samples must have the name defined in
Options > Settings >
Standards .
Set method in the sample view (text view):
For blank samples, cf. Types of blank value determination and their settings.
For conditioning samples, cf. Performing routine measurement work.
For daily factor samples, cf. Performing routine measurement work.
For real samples, cd. Values for oxygen dosing.
Go through the measuring start checklist. Cf. Checklist for blank value / conditioning and daily factor measurements.
Start the analysis process in the operating software:
Select
System > Auto run
to start a multiple-sample analysis.
Select
System > Single run
to start a single-sample analysis.
Once measurement is finished, evaluate the measurement.
Save the data or print them out. See
Data backup and printing
When can routine measuring work be omitted?
You can measure real samples without preceding routine measuring work:
if you have already performed routine measuring work today
if measuring breaks last less than 2 hours.
Measuring real samples without preceding routine measuring work
Please observe the following instruction:
Caution Inserting multiple samples into the ball valve (only for solid operation)
If there are samples in the carousel while you are changing the position of the carousel via
System > Sample Position
, multiple samples may fall into the ball valve at the same time. In this case, a service technician is required.
Before changing the position of the carousel, always remove all samples from the carousel.
Proceed as follows:
Move the empty carousel to zero position. To do so, open the "Set carousel position" dialog in the operating software by selecting
System > Sample Position
.
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Select the radio button next to "Reference run" and click
OK
. The carousel moves to zero position.
Prepare the samples. Cf.
Sample preparation instructions
Insert the samples on the carousel.
Enter the weight in [mg] in the sample view (text view) on the PC if it has not already been transmitted online by the balance.
Enter the sample name (max. 32 characters) in the sample view (text view).
Select a suitable method. See Values for oxygen dosing.
Go through the measuring start checklist. See Checklist for real sample measurement.
Start the analysis process in the operating software:
Select
System > Auto run
to start a multiple-sample analysis.
Select
System > Single run
to start a single-sample analysis.
Once measurement is finished, evaluate the measurement.
Save the data or print them out. See
Data backup and printing
Performing routine measuring work
Overview
This section provides information about
types of routine measuring work,
the purpose of routine measuring work,
and how to perform this routine measuring work depending on the mode.
Definitions
Routine measuring work comprises the following activities:
Determination of instrument blank values.
Instrument conditioning with conditioning samples.
Determination of daily factors.
Routine measuring work is performed at set intervals or on defined occasions before, during or after a series of measurements with real samples.
Instrument blank values
Determination of the instrument blank value depends on your needs. The following overview shows the type and purpose of the determination.
Purpose
Checking gas-tightness
Blank value determination of sample additives and packing materials
Sample none
Sample additive
Packing material
Blank value Occasion
N after maintenance work
N to allow for sample additives or packing material
For details on determining blank values, cf. Types of blank value determination and their settings.
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Conditioning samples
Conditioning samples are measured with standard substances at the start of every series of analyses.
They are used to check...
... the correct run of the analysis.
... the proper condition of the instrument.
... flow and pressure behavior of the gases.
Daily factor determinations
Determination of the daily factor serves...
... to fine-tune instrument calibration to room conditions at the time of analysis.
... to assess the condition of the instrument by observing daily factor fluctuations and drift trends.
When to perform routine measuring work
Perform routine measuring work...
... at least once a day.
... additionally when measuring breaks last longer than 2 hours.
If a series of analyses exceeds a duration of 5-6 hours (carousel completely loaded), it is advisable to determine the daily factor additionally at the end of the series.
Performing routine measuring work
Proceed as follows:
If desired, perform a blank value determination. For details, see Types of blank value determination and their settings.
Measure the conditioning sample twice. Use a standard as run-in sample which corresponds your sample matrix:
250 mg aspartic acid with method "250mgStandard".
Measure the following daily factor sample three times and compute the daily factor:
250 mg aspartic acid with method "250mgStandard".
Measure a maximum of 50 real samples.
At the end of the series, measure the following daily factor sample four times and check the daily factor:
250 mg aspartic acid with method "250mgStandard".
Checklist for blank value / conditioning and daily factor measurements
Purpose
The checklist helps you to check whether the instrument is ready to measure blank value, conditioning and daily factor samples.
Checklist
Go through the following list:
Are the operating gases on?
Are the furnaces at setpoint temperature?
Is pressure OK?
Display on the PC "Press. Input": 1300 - 1350 mbar
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Display on the PC "Press. Output": 900 - 1000 mbar
Is the flow meter display OK?
Measuring gas flow meter on the PC "MFC CO2": 700 ml/min
CO
2
flow meter on the PC "Flow CO2": approx. 700 ml/min
O
2
flow meter on the PC during O
2
dosing "MFC O2": as selected in the method
Does the desiccant still have sufficient capacity?
At least the last third should still be unused.
Have the maintenance intervals been observed? Check:
The drying tube.
The Ash crucible / ash finger.
The Regainer.
The Reductor.
Is the detector signal small and stable?
Is the proper method allocated to the respective samples?
Is the carousel loaded?
If you answer yes to all of the above, you can start measuring blank value, conditioning and daily factor samples.
Checklist for real sample measurement
Purpose
The checklist helps you to check whether the instrument is ready to measure real samples.
Checklist
Go through the following list:
Were the results of a blank value determination OK?
Were the results of the conditioning sample measurement OK?
Have you processed a series of measurements with daily factor samples?
Are the operating gases on?
Are the furnaces at setpoint temperature?
Is pressure OK?
Display on the PC "Press. Input": 1300 - 1350 mbar
Display on the PC "Press. Output": 900 - 1000 mbar
Is the flow meter display OK?
Measuring gas flow meter on the PC "MFC CO2": 700 ml/min
CO
2
flow meter on the PC "Flow CO2": approx. 700 ml/min
O
2
flow meter on the PC during O
2
dosing "MFC O2": as selected in the method
Does the desiccant still have sufficient capacity?
At least the last third should still be unused.
Have the maintenance intervals been observed? Check:
The drying tube.
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The Ash crucible / ash finger.
The Regainer.
The Reductor.
Is the detector signal small and stable?
Is the proper method allocated to the respective samples?
Is the carousel loaded?
If you answer yes to all of the above, you can start measuring real samples.
Types of blank value determination and their settings
Background
Blank value determination can be used for various purposes and is therefore performed in different ways. The different types of blank value determination are described below with an explanation of the respective settings.
Degree of gas tightness (N blank value)
This blank value determination is performed as a routine task. It makes sense after gas cylinder replacement and after maintenance work.
The blank value determination is performed without a sample.
Use the method "Blank with O2".
The N integral values should be between 10 and 50 after stabilization. If your N integral values are significantly higher than 50, repeat the blank value determination with methods which is associated with an oxygen dosing time. If the N integral values are then normal, the oxygen was contaminated. Otherwise, the system has probably a leak.
Sample additives or packing material
Blank samples are measured for blank value determination of sample additives (e.g. WO
3 packing material:
powder) or
prepare blank samples:
without sample substance
with equal amount of sample additives
with the same packing material and the same packing method.
For the blank sample, use the same method used for the real sample.
The mean value of the blank value integrals is then entered in the software and deducted from the samples.
Only if the blank value always remains the same by preparing the sample accordingly, it can also be "calibrated" and does not have to be deducted. However, in this case standard substances must be prepared in the same way as the samples for calibration and daily factors.
Determining blank values
Condition
The name of the blank sample must be defined in
Options > Settings > Keywords
. Ex works, "Blnk" is already defined as the key word of the blank sample. If you want to change this, you must define the new name via Options > Settings > Keywords .
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Note
The first blank value is always too high after prolonged breaks between measurements or after maintenance. If you want to perform an exact blank value determination, you must exclude the first blank value from the calculation. Use a different name for the first blank value sample than the key word in order to exclude the sample from the calculation.
Determining blank values
Proceed as follows:
If you have not already done so, set the mode of blank value determination. For that purpose, open the "Configure Calculations" dialog in the operating software by selecting Options >
Settings > Calculation
.
Define the mode of blank value determination:
If you select the following in "Blank value determination"
... ...select "sequentially" a separate blank value is computed for every element for every group of blank value samples; this value is entered in the respective blank value column until the next group of blank value samples.
... ...select "entirely" all blank value samples in the series are used to compute the blank value. This blank value is then applied to all samples in the series.
Then click
OK
to save your settings.
Usually, do not
place a sample on the carousel.
Only exception: When determining blank values of sample additives or packing materials, place a blank sample on the carousel. Cf. Types of blank value determination and their settings.
Enter the following for the sample in the sample view (text view) on the PC:
Name:
Blnk
Weight:
1 mg
Click
Method
in the line of the appropriate sample. An arrow is displayed with which you can open a dropdown list with various methods.
Select the appropriate method for the blank value sample. Cf. Types of blank value determination and their settings.
Start the blank value determination via
System > Auto run
.
Once the measurements are finished you can compute the blank value. To do so, open the
"Blank values" dialog by selecting
Math. > Blank values > Calculate
.
If "total" blank value calculation has been selected, the "Blank values" dialog will now open. Here, the blank value just computed is displayed. Click
OK
to accept the blank value.
The blank value is now automatically used for the following measurements.
Determining the daily factor
Why is the daily factor determined?
The daily factor is determined in order to correct calibration according to atmospheric conditions (air pressure, temperature) at the time of performing the analysis. The daily factor is factored into subsequent measurements.
When must daily factor samples be measured?
Daily factor samples are measured on the following occasions:
During routine measuring work, once a day.
When the carousel is full daily factor samples are measured at the end (and between if necessary) in order to check the condition of the instrument.
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Ways of determining the daily factor
There are three ways to determine the daily factor:
You can compute the daily factor manually. This makes sense if you do not want to define the substance as a factor sample.
You can selectively trigger determination of the daily factor:
You can then choose the time for determining the daily factor yourself.
You can choose the standard samples with which the daily factor is determined yourself.
Condition: The daily factor samples must have a name defined in
Options > Settings >
Standards
and the standard substance must be enabled as a factor sample.
Daily factor determination can be set to fully automatic.
If you measure substances defined as factor samples, they are recognized and the daily factor is automatically computed from them.
Because the daily factor is determined several times a day, it will also offset any fluctuations in the course of the day. Condition: The daily factor samples must have a name defined in
Options > Settings > Standards
and the standard substance must be enabled as a factor sample.
Computing the daily factor by hand
Proceed as follows:
Measure any substance, that need not be defined in
Options > Settings > Standard samples
.
Compute the daily factor. Daily factor = (theoretical content / actual content).
Allocate the daily factor to the real samples in the sample view (text view). Enter the daily factor in the corresponding factor column.
How to selectively trigger the daily factor
Proceed as follows:
Define the type of factor calculation. For that purpose, open the "Configure Calculations" dialog in the operating software by selecting
Options > Settings > Calculation
.
Define the mode of factor determination:
If you in section "Factor determination"...
... select "sequentially" then the daily factor is computed group-by-group and changes throughout the day.
... select "entirely" the daily factor is computed on the basis of all factor samples in the file.
An average factor is computed.
Then click OK to save your settings.
Measure a standard substance, that must be defined in
Options > Settings > Standard
Samples
, as a factor sample.
If you only want to determine the daily factor from a certain number of samples, select these samples in the sample view (text view).
Open the "Daily factors" dialog in the operating software by selecting
Math. > Factor
.
If you selected a certain number of samples for the calculation, check "Use standard samples only".
Click
Yes
to continue. The daily factor is computed automatically and allocated to the subsequent samples.
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How to set automatic daily factor determination
Proceed as follows:
Define the type and degree of automation for factor calculation. For that purpose, open the
"Configure Calculations" dialog in the operating software by selecting Options > Settings >
Calculation
.
Define the mode of factor determination:
If you in section "Factor determination"...
... select "sequentially" then the daily factor is computed group-by-group and changes throughout the day.
... select "entirely" the daily factor is computed on the basis of all factor samples in the file.
An average factor is computed.
Specify the degree of automation for factor determination. Check "Automatic factor determination". factor calculation.
Then click
OK
to save your settings. As soon as you measure a substance defined as a factor sample, the daily factors are automatically computed afterwards.
Recommendation for automated daily factor determination
When automatically computing the daily factor, it is useful to enable the "Standard tolerance monitoring" function. This checks standard samples for fluctuations of results. If the tolerance define in
Options > Settings > Standards is exceeded, continuous analysis is stopped.
Enabling "Standard tolerance monitoring"
Proceed as follows:
Open the "Error handling" dialog in the operating software by selecting
Options > Settings >
Error handling
.
Check "Standard tolerance monitoring".
Click
OK
. "Standard tolerance monitoring" is now enabled.
Stopping continuous analysis
When do I stop continuous analysis?
It makes sense to stop a continuous analysis in the following cases:
If the result of the blank value indicates that the instrument is leaky.
If the results of the conditioning sample indicate that parts of the instrument are defective or that gas pressure and flow behaviors are not OK.
If results of the daily factor deviate substantially from the last results.
Stopping a continuous analysis spontaneously
Proceed as follows:
Execute the command
System > Single run
in the operating software.
This stops the analysis after measuring the current sample.
Moving a stop marker
The program automatically moves the stop marker to the last sample position during sample data input. It is therefore only necessary to move the stop marker in special cases.
Nevertheless, if for any reason you have to move the stop marker proceed as follows:
Open the "Set stop marker" dialog by selecting
Edit > Stop tag
.
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Use the arrow buttons to set the sample number at which to set a stop marker.
Click
OK
. This closes the dialog and moves the stop marker to the desired position.
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7 - Using the instrument
Preparing measuring data for evaluation
Target group
Personnel with basic knowledge of chemistry and experience with laboratory work, e. g. chemistry laboratory workers.
Purpose
This section enables you to prepare measuring data for evaluation.
In this section
146
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7 - Using the instrument 147
Configuring the sample view
Configuring the sample view
Proceed as follows:
Select cells in the sample view.
Specify what you want to have displayed in the view. Open the "Configure view" dialog by selecting
View > Gridview > Configure
.
Decide:
If you want to...
... show a column: Select the entry in the "Hide" column and click
<<<
. The entry is moved to the "Show" column.
... hide a column: Select the entry in the "Show" column and click
>>>
. The entry is moved to the "Hide" column.
Change the column display order using the
^
and v
buttons.
Click
OK
. This closes the dialog and saves your settings.
Auto-optimizing a view
You can automatically adjust the width of individual columns to fit the whole headers and entries in the cells.
Proceed as follows:
Select cells in the sample view.
Optimize sample view by selecting
View > Gridview > Auto align
. This optimizes the sample view.
Determine measuring units and number of decimal places.
Determine measuring units and number of decimal places.
Proceed as follows:
Select cells in the sample view.
Open the "Configure view" dialog in the operating software by selecting
View > Gridview >
Configure
.
Select the column in the "Show" section whose measuring units or decimal places you want to set and click the right mouse button. A context menu opens.
Open the "Column properties" dialog by selecting the
Properties...
menu item.
Enter the desired measuring unit in the "Unit" filed.
Note:
This function is not available for all columns/systems.
Enter the desired number of decimal places in the "Decimal places" field.
Note:
This function is not available for all columns.
Click
OK
in the "Column properties" dialog.
Click
OK
in the "Configure view" dialog. This closes the dialog and saves the settings.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
7 - Using the instrument
Saving the sample view
148
Saving the sample view
Proceed as follows:
Open the "View configuration" dialog by selecting
View > Gridview > Save configuration
.
Enter the name of the view in the text box at the top and click
Save
. The view is saved and can be loaded at a later point.
Loading a sample view
Loading a sample view
Proceed as follows:
Open the "View configuration" dialog by selecting
View > Gridview > Load configuration
.
Select the desired view in the listbox and click
Load
. The desired view is loaded.
Configure statistics view
Configure statistics view
Proceed as follows:
If the statistics view of the combi view is not already being displayed, execute the command
View
> Toggle
until statistics view appears or click on
Statistic field
in the menu bar above the combi view.
Klick on the statistic view to highlight it.
Specify what you want to have displayed in the view. Open the "Configure Statistic Pane" dialog by selecting
View > Statistic > Configure
.
Decide:
If you want to...
... show a value: Check the appropriate checkbox.
... hide a value: Uncheck the appropriate checkbox.
Click
OK
. This closes the dialog and saves your settings.
Generating statistical data
What are statistical data?
Statistical data are mean values and standard deviations computed from groups of measuring data.
The operator compiles the groups, that may consist of analyzed samples and samples not yet measured.
Ways of generating statistical data
There are two ways of generating statistical data:
You can generate statistical data fully automated. In this case, the software combines all samples of the same name into groups. The user can only exclude specific samples from the calculation.
Statistical data are then automatically generated for these groups.
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You can generate statistical data manually. In this case, the user combines any samples in groups. Statistical data are then automatically generated for these groups.
Generating statistical data fully automated
Proceed as follows:
Click
Statistics > By names
. A warning appears which has to be confirmed.
Respond to the warning note:
If statistics memory...
... may be deleted: Click
Yes
.
... must not be deleted: Click
No
and safe your data. Afterwards, repeat the steps descibed above.
Samples of the same name are combined in groups and the mean values and standard deviation are computed automatically and displayed in the statistics view.
If you want to exclude a sample from the calculation afterwards, select the appropriate sample line in the statistics view. Subsequently execute the command
Statistics > Include/Exclude sample
or click the button updates automatically.
in the toolbar . The sample is discarded and the calculation
Generating statistical data manually
Proceed as follows:
Select all samples that you want to combine in a group in the sample view (text view). To do so, click the "No." cell of the corresponding line.
Select multiple contiguous samples by clicking and holding the SHIFT key.
Select multiple non-contiguous samples by clicking and holding the CTRL key.
Select
Statistics > Group
. The selected samples are displayed as a group in statistics view.
Mean values and standard deviation are computed automatically.
If you want to exclude a sample from the calculation afterwards, select the appropriate sample line in the statistics view. Subsequently execute the command
Statistics > Include/Exclude sample
or click the button updates automatically.
in the toolbar . The sample is discarded and the calculation
Formulae for generating statistical data
Statistical data
The following statistical data can be generated fron sample groups:
Mean value of the sample group
Absolute standard deviation of the sample group
Relative standard deviation of the sample group
Delta of the sample group
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
7 - Using the instrument
Mean value
The mean value of "n" element concentrations is computed with this formula: whereas:
/c = Mean value of concentrations c i
= Individual concentrations in the group n = Number of group members i = index from 1 to n
Absolute standard deviation
Absolute standard deviation is computed according to this formula: whereas: s = Absolute standard deviation c i
= Individual concentrations in the group n = Number of group members i = index from 1 to n
Relative standard deviation
Relative standard deviation is computed according to this formula: whereas: s rel
= Relative standard deviation s = Absolute standard deviation
/c = Mean value of concentrations
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Delta
Delta is computed according to this formula: whereas:
δ = Delta c max
= Highest element concentration in a group c min
= Lowest element concentration in a group
Manual peak integration
What is "manual peak integration"?
The instrument software offers the possibility to manually determine area values of peaks measured during an analysis run.
Why manual peak integration?
Normally the measurement of the peak areas (integration) is done automatically in the control electronic and/or the firmware of the analyzer itself. In few cases, it may be possible that the automatic integration algorithm does not give satisfactory results, in particular if two peaks are superimposed etc. In these cases the "manual reintegration" is recommended.
Peak types
In these instructions you will find different peak types. Their characteristics are listed in the follwing.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
7 - Using the instrument
Single peaks
In general a single peak looks as follows:
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Superimposed peaks
These are two peaks where one superimposes the other. Peak 1 is designated as "socket" and peak
2 is designated as "superimposed". The following picture shows such a run.
Melted peaks
These are two consecutive peaks where the second peak already starts although the first is not yet finished. The graphic appears as follows:
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7 - Using the instrument 152
Manual integratability
Regarding the integratability there are certain differences between the individual peak types.
Well integrable are:
Sinple peaks with clear beginning and tailing. This peak type normally is integrated without any problem from the firmware implemented in the algorithm. However, a reintegration may be necessary, in particular if the peak is very small and therefore the end mark was set too early.
Superimposed peaks where a significant difference in width between socket (large) and
"superimposed" (small) is noticeable.
Limited integrable are:
Superimposed peaks, where a significant difference in width between socket and "superimposed" is not noticeable.
Poorly or not at all integrable are:
Melted peaks, since due to the undefined peak form no conclusions for the actual separation points between the first and the second peak are possible.
Baseline
The instrument software allows to select a straight or bevel baseline for integration. The automatic integration always assumes a straight baseline. Therefore, also the manual peak integration should be done with a straight baseline. The height of the baseline will be defined during the auto zero adjust. During the manual integration the baseline can be specifically adjusted in height. The option to perform the manual peak integration with a bevel baseline can be selected for special cases.
Procedure
Important note:
Prior to the manual peak integration, create a copy of the actual loaded document and only perform the manual peak integration there. A copy can be created via
File > Save As
with subsequent input of a suitable (different) document name.
Depending from the predominant peak shape there are two different procedures:
Integration of single peaks. Here, the requested peak start and end marks are set as well as the adjustment of the height of the baseline
Integration of superimposed peaks. Here, first the peak start and end marks of the socket and the height of the baseline are set, subsequently the peak start and end marks of the "superimposed" peak. If requested, an intermediate point for the separation of socket and "superimposed" peak can be set. This serves as a better adjustment of the socket course.
Integration of single peaks
Proceed as follows:
Open in the instrument software the dialog "Define type of peak" via Math. > Manual peak integration > Type
.
Note:
The menu command is only accessible, if the grafic view is activated.
Activate "single peak" and "straight baseline" and subsequently click
OK
, to leave the dialog.
Select the requested sample so its peak course is displayed in the graphic view.
Open the instrument software via the dialog "Define peak start/end" via
Math. > Manual Peak
Integration > Integrate
.
Note:
The menu command is only accessible if the graphic view is activated and configured that way only the single corresponding peak course is displayed. If necessary, deactivate other graphics (e.g. pressure, temperature, etc.).
Click and mark the peak start as follows: position the mouse pointer to the position where the peak begins and click the left mouse key. The peak start tag is displayed as a vertical blue line.
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Click and mark the peak end in the same way as described in the previous step for the peak start. As soon as peak start and end are marked, a baseline is drawn automatically and the integration result is displayed below the peak graphic. Furthermore, the area content appears in light blue.
Click to adjust the height of the baseline. To find out the original height which was determined during the automatic integration, first place the peak start and end tags directly over the tags generated from the automatic (magenta crosses). Then move the baseline until the manual integration result matches the automatic one. Subsequently, you can move the peak start and end tag to the requested position, if necessary (see description of the two previous steps).
Click Assign , if the integration result meets your requirements. The dialog "Area assignment" opens. Select the element which shall be assigned to the manually integrated peak area. Leave the dialog by clicking OK .
The peak area was entered in the corresponding cell in the sample view and the new concentration value was calculated. Furthermore, the date for the corresponding sample was deleted and the text "ManInt" was entered in the info column. Now the process of the manual integration of single peaks is completed.
Integration of superimposed peaks
Proceed as follows:
Open in the instrument software the dialog "Define type of peak" via
Math. > Manual peak integration > Type
.
Note:
The menu command is only accessible, if the grafic view is activated.
Activate "superimposed peak" and "straight baseline" and subsequently click
OK
, to leave the dialog.
Select the requested sample so its peak course is displayed in the graphic view.
Open the instrument software via the dialog "Define peak start/end" via
Math. > Manual Peak
Integration > Integrate
.
Note:
The menu command is only accessible if the graphic view is activated and configured that way only the single corresponding peak course is displayed. If necessary, deactivate other graphics (e.g. pressure, temperature, etc.).
Click and/or to tag the peak start and and of the socket as described in the section of the procedure of single peaks.
Click to adjust the height of the baseline, as described in the section of the procedure for single peaks.
Click and mark the peak start of the "superimposed" peak as follows: position the mouse pointer to the position where the superimposed peak begins and click the left mouse key. The peak start tag is displayed as a vertical red line.
Click and mark the peak end of the superimposed peak in the same way as described in the previous step for the peak start. As soon as peak start and end are tagged, a red baseline is drawn automatically and the integration result is displayed below the peak graphic. Furthermore, the peak area of the superimposed peak is displayed in light red.
Click , to set an intermediate point. By doing so, you may reach a better adjustment of the socket course.
Click
Assign
, if the integration result meets your requirements. The dialog "Area assignment" opens. Select the manually integrated peak area and the element which shall be assigned. Leave the dialog by clicking
OK
.
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The peak area was entered in the corresponding cell in the sample view and the new concentration value was calculated. Furthermore, the date for the corresponding sample was deleted and the text "ManInt" was entered in the info column. Now the process of the manual integration of superimposed peak is completed.
Configuring the graph view
Configuring the graph view
Proceed as follows:
If the graphic view of the combi view is not already being displayed, execute the command
View
> Toggle
until the graphic view appears or click
Graphic field
in the menu bar above the combi view.
Klick on the graphic view to highlight it.
Specify what you want to have displayed in the view. Open the "Configure Graphic Pane" dialog by selecting View > Graphic > Configure .
Decide for the section "Y axis configuration":
If you want to...
... show a value: Check the appropriate checkbox. Enter the graph scale range in the textbox next to it. You can have a max. of 4 checks, for the sake of clarity.
... hide a value: Uncheck the appropriate checkbox.
In the "Zero line" section, specify which of the horizontal grid lines to take as the zero line for the graph view. A value of 0 means that the zero line is at the bottom edge of the graph view. Use the arrows to set the desired value.
Specify the division of the time axis (X axis) in the "X-axis configuration" section. Enter the desired value in the textbox.
Specify what graph to display during analysis. Decide:
During an analysis, you want...
... to show only the graphic of the current sample: Check the checkbox next to "During analysis run display current sample only".
... to show also the graphics of all samples: Uncheck the checkbox next to "During analysis run display current sample only".
Click OK . This closes the dialog and saves your settings.
Auto-optimizing a view
By selecting
View > Graphic > Auto align
you can auto-scale the graph to fit it completely in the window.
Setting the size of the graph
Setting the size of the graph in the dialog
Proceed as follows:
Open the "Zoom In/Out" dialog in the operating software by selecting
View > Zoom
.
Use the arrow button to open a listbox which lists the possible zoom factors.
Select the the requested zoom factor from the list.
Click
OK
. This closes the dialog and displays the graph according to your settings.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
7 - Using the instrument
Setting the size of the graph with the mouse
Proceed as follows:
Drag a rectangle in graph view using the mouse.
The selected area is displayed larger.
Setting the zoom factor back to 1
155
By clicking the button at the upper left corner of the graphic filed you can set the zoom factor from any value back to 1.
Configure report
Configure report
Proceed as follows:
Open the "Configure Report" dialog by selecting
File > Report configuration
.
Define the print settings as required:
Enter up to three headers in the "Title" section.
Check the appropriate options in the "Report options" section.
Click OK . This closes the dialog and saves the settings.
Display print preview
Display print preview
Proceed as follows:
Open the "Configure report" dialog in the operating software by selecting
File > Print preview
.
Define your report settings. See Configure report
(on page 155). You can also change the
report type in this dialog below the icon. Then click
OK
. Print preview is displayed.
Assess the print preview:
The
Next
and
Previous
buttons allow you to browse multiple page documents.
The Two Pages and One Page buttons allow you to view two pages next to each other or a single page.
The
Zoom in
and
Zoom out
buttons allow you to zoom the document in/out in order to see it better.
Decide:
If the print preview...
... is OK and you want to print out the document: Click Print . The "Configure report" dialog is displayed again, click
OK
. The "Print" dialog is displayed.
... is not OK and you want to change it: Click
Close
. Open the "Configure Report" dialog by selecting
File > Report configuration
. See
Configure report
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
7 - Using the instrument
Data backup and printing
156
Why backup and print data?
The measuring data of a sample are displayed on screen and saved to a temporary file after every analysis. In order to save the data permanently, it is necessary to save them separately or print them out.
Graph view
All graphical information (pressure, peaks, etc.) of a sample are saved. This allows you to view and print various measuring variables in a graph. If any error messages or fluctuating measuring values occur, it is useful to consult the graph.
Viewing and printing the graph
Proceed as follows:
In the sample view (text view), select the sample line whose graph you wish to display.
If the graphic view of the combi view is not already being displayed, execute the command
View
> Toggle
until the graphic view appears or click
Graphic field
in the menu bar above the combi view.
Specify what measuring variables you want to display in the graph. Open the "Configure Graphic
Pane" dialog by selecting
View > Graphic > Configure
.
Define your settings:
Check the measuring variables to display. You can select up to 4 measuring variables.
In the "Zero line" section you can move the zero line up.
In the "X-axis configuration" section you can influence the graph display area.
Click
OK
. The graph is displayed with your settings.
Execute the command
File > Print
to print out the graphic. The "Configure report" dialog is displayed.
Define the print settings as required:
Enter a title in the "Title" section. It can consist of up to three lines.
Check the appropriate options in the "Report options" section.
Click
OK
. The "Print" dialog is displayed in which you can start printing.
Permanently backing up measuring data and graphical information
Proceed as follows:
Execute the following command:
File > Save
.
If the document...
... has already a name: The document is automatically updated. The storing process has been completed.
... has not yet a name: The "Save document" dialog appears.
Enter the desired document name in the header of the "Save document" dialog.
Click
OK
. The measuring data are saved.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
7 - Using the instrument
Overview of export and import file formats
157
Export and import
The analysis data are managed in a database, so it is not possible to load and save them as files in the usual way. However, by using the
File > Export/Import > Export
and
File > Export/Import >
Import
menu functions it is possible to transport documents "out of" the database and to transport external documents "into" the database.
Export and import file formats
The following table lists the file formats and their uses:
File type Import
*.sqlite yes
*.xls
*.dat yes yes
Export yes yes no
Description
SQLite Database file. Requires more memory than the other file types. Includes graphical informations in the export.
Suitable for transferring files to be evaluated by someone else, e.g. by the service department.
MS Excel file. Does not include graphical informations in the export. Suitable for further numerical processing in MS Excel.
It is possible, but not advisable, to import these files because graphical information is deleted if a file of the same name exists.
Balance file Files with weighing data generated by the
"Balance" program (product from BÜCHI Labortechnik AG) can be imported. It is not, however, possible to import other files with the *.dat extension.
Exporting analysis data to MS Excel and viewing
Exporting analysis data to MS Excel
Proceed as follows:
Open the "Export document" dialog in the operating software by selecting
File > Export/Import >
Export
.
Select the desired file in the listbox and click
OK
.
This displays the "Save file as" dialog.
Select the directory to save to in the "Save" field.
Select "MS Excel Files" in the "File type" field and click
Save
.
A message dialog appears which informs that exporting to MS Excel will be done without graphics. Click
Yes
to begin exporting.
The export process is performed.
Viewing analysis data in MS Excel
Proceed as follows:
Launch MS Excel.
Open the "Open" dialog by selecting
File > Open
.
Select "All Microsoft Excel Files" as the file type to open in the "File type" field.
Select the directory containing the desired analysis file in the "Search in" field.
Select the desired analysis file in the list below and click Open .
The data are displayed on different tabs in MS Excel.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
7 - Using the instrument
Edit the imported data as required and save them when you are finished.
Exporting LIMS data
Selecting data to send
Proceed as follows:
Open the "LIMS settings" dialog by selecting
Options > Settings > LIMS
.
Open the "LIMS data" tab.
Decide:
If you want to...
... send data: Check the appropriate checkbox in the "Data to send" section.
... not send data: Uncheck the appropriate checkbox in the "Data to send" section.
Click OK in the "LIMS settings" dialog. Your settings are saved and the dialog is closed.
Auto-exporting LIMS data
Proceed as follows:
Open the "LIMS settings" dialog by selecting
Options > Settings > LIMS
.
Open the "LIMS data" tab.
Check the "Auto-export data after every analysis" checkbox.
Click
OK
in the "LIMS settings" dialog. Your settings are saved and the dialog is closed. The software now sends analysis data to LIMS after every analysis.
Exporting LIMS data manually
Proceed as follows:
Open the "Export to LIMS" dialog by selecting File > Export/Import > Export to LIMS .
Select the desired option.
Click
OK
in the "Export to LIMS" dialog. The export process is performed.
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Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
7 - Using the instrument
Working with documents
Target group
Personnel with basic knowledge of chemistry and experience with laboratory work, e. g. chemistry laboratory workers.
Purpose
This section enables you to work with database documents.
In this section
159
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Creating new documents
Usual procedure
Usually, one document is created per day. The data are separated and evaluated by customer at the end of the day.
Document capacity
A document can store sample data from a maximum of 5 carousels.
Creating new documents
Proceed as follows:
Select
File > New
to create a new document.
Save the new document by selecting
File > Save
. The "Save document" dialog appears.
Enter the desired document name in the text box at the top and click OK . This closes the dialog and saves the document.
Editing documents
Note
Cell contents and lines can only be deleted or inserted until the samples have been completely processed.
Deleting cell contents
Proceed as follows:
Select the cell whose contents you want to delete.
Delete the contents by selecting
Edit > Cut
. The cell now contains its default contents, for example 0.0000. The deleted contents are in the clipboard.
Deleting lines
Proceed as follows:
Select the line by clicking the number next to the line.
Delete the line by selecting
Edit > Delete Line
. This deletes the line and the other samples move up.
Inserting cell contents
Proceed as follows:
Copy the desired contents to the clipboard.
Select the cell in which to insert the contents.
Insert the contents in the cell by selecting
Edit > Paste
.
Inserting lines
Proceed as follows:
Select the line above which to insert the empty line by clicking the number next to the line.
Insert the line by selecting
Edit > Insert Line
. This inserts the line and all of the following samples move down one line.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
7 - Using the instrument
Swap samples
Proceed as follows:
Open the "Swap samples" dialog via
Edit > Swap
.
Enter the sample numbers to be swapped and confirm with OK .
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Editing finished samples
Finished samples are only edited in special cases. See Editing analysis data
Deleting documents
Who is allowed to delete?
Deleting documents is reserved for the Administrator level.
What is deleted?
The document itself is deleted along with all previous versions of the document.
Consequences
If 21 CFR Part 11 functionality is enabled, the user is prompted to input a comment after deleting the document.
Finding documents
Searching with filter criteria
Proceed as follows:
Open the "Open document" dialog in the operating software by selecting File > Open . Activate the "Selection" checkbox to show the document search filter criteria.
Decide:
If you want to...
... look for documents beginning from a certain date: Enter a date in the "From" textbox and check the checkbox next to it.
... look for documents ending at a certain date: Enter a date in the "To" textbox and check the checkbox next to it.
... look for documents of a certain period: Enter a date in the "From" and "To" textboxes and check the checkboxes next to them.
... look for documents with a certain name: Enter the document name you are looking for in the "Name" textbox. Wildcards such as ? and * are also allowed.
... look for documents of a certain author: Enter the name of the author in the "Author" textbox.
The software now only displays documents matching your filter criteria. Select the desired document in the listbox and click
OK
.
Make a decision for the further proceeding:
If the coefficients of the selected document...
... match the current coefficients: The document is displayed immediately. Herewith, the searching is finished.
... do not match the current coefficients: A message appears. Go to the next step.
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A message appears which informs that the coefficients included in the document are different and the current coefficients will be overwritten during the document is loaded. This message must be confirmed by you. Click
Yes
to continue. The document is displayed.
Finding previous versions
Note:
This function is only accessible if 21 CFR Part 11 functionality is enabled.
Proceed as follows:
Open the "Open document" dialog in the operating software by selecting
File > Open
.
In the listbox select the document whose previous versions you want to view.
Click
Previous versions
. The "Select version" dialog is displayed.
Select the desired version in the listbox and click
OK
. The current version is indicated by number
0, previous versions are indicated by a minus sign.
Decide:
If the coefficients of the selected previous version...
... match the current coefficients: The previous version is displayed immediately. Herewith, the searching is finished.
... do not match the current coefficients: A message appears. Go to the next step.
A message appears which informs that the coefficients included in the document are different and the current coefficients will be overwritten during the document is loaded. This message must be confirmed by you. Click
Yes
to continue. The previous version is displayed.
Copying documents via the clipboard
What can you copy?
You can only copy the contents of the sample view to the clipboard via
Edit > Copy
; you cannot copy graphics. You must select the cells to copy in the sample view. The next paragraph explains how to select cells.
Selecting cells
You can select cells in the sample view in the following ways:
Select the whole sample view by left-clicking on the "No." field.
Select a whole line by left-clicking on the number next to the line.
Select a whole column by left-clicking on the title of the column.
You can select multiple successive lines by clicking and holding the SHIFT key.
You can select multiple non-contiguous cells, lines or columns by clicking and holding the CTRL key.
Left-click to select a single cell.
Inserting data
You can insert data from the clipboard by selecting
Edit > Paste
:
to insert them into a new document in the database or
into an MS Excel document.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
7 - Using the instrument
Importing documents
Importing documents
Proceed as follows:
Open the "Open" dialog by selecting
File > Export/Import > Import
.
From the "Look in" dropdown listbox select the directory containing the document.
Select the document file and click
Open
.
Decide:
If the coefficients of the selected document...
... match the current coefficients: The document is imported immediately. Herewith, the import is finished.
... do not match the current coefficients: A message appears. Go to the next step.
A message appears which informs that the coefficients included in the document are different and the current coefficients will be overwritten during the document is loaded. This message must be confirmed by you. Click
Yes
to continue. The document is imported.
Signing documents
163
What signature is allocated?
The signature that is enabled in the "Sign" dialog and whose radio button is checked is allocated; for example, the "created" signature is allocated. The following rules apply:
The "created" signature is assigned to a document first.
The "checked" signature is assigned to a document if it already has a "created" signature.
The "released" signature is only assigned to a document if it already has a "created" and a
"checked" signature.
Note
Note the following:
The signature program must be installed.
Documents can only be signed if 21 CFR Part 11 functionality is enabled.
Only sign finished documents. After signing, the document is read-only.
Signing documents
Proceed as follows:
Open the "Sign" dialog in the operating software by selecting
File > Sign
.
Enter your name set up in the signature program in the "Name" field.
Enter your password set up in the signature program in the "Password" field.
Click
Sign
. The program checks whether you are authorized to sign the document. The result is displayed in a message window:: "GOOD_PASSPHRASE" indicates that you are authorized to create the signature. The signature has been created.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
7 - Using the instrument
Checking documents for authenticity
What signature is checked?
Only those signatures can be checked that are enabled in the "Verify digital signature" dialog and if their radio button is checked; for example the "created" signature. If the document already has multiple signatures, the user must select one to check.
Note
Checking a signature
Proceed as follows:
Open the document to check.
Open the "Verify digital signature" dialog in the operating software by selecting File > Verify .
Check the radio button next to the signature you want to check.
Click
Verify
. The program begins to check. The result is displayed in a message window and indicates whether the signature is authentic or not. "Good signature from..." indicates that the signature is authentic.
Note the following:
The signature program must be installed.
Signatures can only be checked or created if 21 CFR Part 11 functionality is enabled.
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Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
C H A P T E R 8
Maintaining the instrument
Target group
Personnel authorized by BÜCHI Labortechnik AG and having undergone training.
Purpose
This section is designed to maintain proper working order of the instrument.
In this chapter
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Important information about maintenance
Target group
Personnel authorized by BÜCHI Labortechnik AG and having undergone training.
Purpose
This section provides important information about maintenance.
In this section
166
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 167
Maintenance work to be performed by the customer
Note
Observe that the maintenance or replacement times indicated here are greatly dependent on the respective sample matrix. All intervals and figures indicated are only examples and by no means guarantee service life of consumables or wear and tear parts.
Maintenance work to be performed by the customer
The following table lists the maintenance work that you can perform yourself as customer and the intervals for these tasks.
Maintenance work Interval See ...
Replacement of the ash crucible Depending on the sample matrix. Replacing the ash crucible.
Cleaning the Ni flap
Instrument and supply lines leak test
When replacing the ash crucible Cleaning the Ni flap.
At least every 2 months. Performing a leak test.
Checking hard disk capacity and relocating data if necessary.
Calibration
Backup every week, relocate data to disk as required.
When the daily factor is no longer between 0.9 and 1.1, but not later than every 2 years.
Every 1500 analyses.
Starting the database backup
Performing calibration.
Ball valve maintenance. Clean ball valve, possibly replacing seals.
Replace sealing elements (orings, quad rings, half shells)
As required. When to replace sealing elements.
Cleaning the carousel
Check/clean quartz glass bridge, check o-rings at the same time
Replace reaction tubes
(combustion tube / post combustion tube / reductor), replace fillings, check plugs and orings at the same time
Check/replace drying tube; check o-rings at the same time
Check supply gases for correct intake pressure and sufficient volume
As required.
Removing sealing elements from grooves
Removing, cleaning and installing the carousel.
Whenever you change tubes.
Replacement intervals, see
Options > Maintenance >
Intervals
in the operating software.
Daily visual inspection
Removing, cleaning and installing the quartz glass bridge.
Removing/installing and conditioning the reaction tubes.
Emptying and filling reaction tubes.
Removing and installing the drying tube.
Filling the drying tube
(on
Before every series of analyses. Gases and chemicals to be provided.
Recommendation
Taking out a service contract for full annual maintenance saves time and money. Contact your service office for details.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Viewing the status of maintenance intervals
168
Viewing maintenance intervals
Proceed as follows:
Open the "Maintenance intervals" dialog in the operating software by selecting
Options >
Maintenance > Intervals
.
In the overview field on the left all maintenance events are displayed, i.e. the corresponding assignment as well as the percentaged count as a highlighted bar.
Click the respective event in the overview field. On the right, the "Status" field displays the number of individual sample measurements performed since the last maintenance. The "Interval" field indicates how many measurements until maintenance is due.
Defining maintenance intervals in the software
Background
In order to make it easier to observe replacement and maintenance intervals, you can define
"maintenance events" with set intervals in the operating software. Several maintenance events are already defined by default and need to be adjusted according to the customer's long-term experience.
Defining maintenance intervals
Proceed as follows:
Open the "Maintenance intervals" dialog in the operating software by selecting
Options >
Maintenance > Intervals
.
Click
New
. The fields in the right area are set to their default values.
Enter the following:
In the "Event" field enter the maintenance event, e.g. "combustion tube".
In the "Interval" field specify the number of measurements of individual samples after which the combustion tube has to be serviced.
Select the following in the "If becoming due" section:
Either "Indication only" if you just want to have a message displayed on screen when the maintenance is due.
Or "Indication and abort the auto run" if you want to have message displayed on screen and contonuous analysis to be stopped when maintenance is due.
Click
OK
to save your settings.
The maintenance event is now defined.
Notes regarding further operation
Observe the notes regarding further operation:
The left area displays the number of measurements since the last maintenance in percent for all maintenance intervals.
For the selected event, the "Status" field displays the number of individual sample measurements performed since the last maintenance.
If the maximum number of measurements is reached, a message is displayed in the status view in the "Maintenance" field reminding the user of the maintenance. See Fig. "Status view message".
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 169
Status view message
If the maximum number of measurements is reached for a maintenance event:
the due maintenance event is displayed in the status view in the "Maintenance" field
the background of the "Maintenance" field turns red
To be observed after maintenance
If you have performed the due maintenance you must manually reset the "Status" field to zero for the respective event.
Installing used tubes
Note
When you install an used tube, and if a maintenance event has been defined for this maintenance work, you must increment the interval counter in the "Maintenance intervals" dialog accordingly. See
Defining maintenance intervals in the software.
Preparing and following up maintenance work
Why prepare and follow up maintenance work?
In order to perform maintenance work it is necessary to make certain preparations so as to avoid risks for the user. This also prevents the instrument from sending an error message and shutting down automatically. It is also necessary to perform follow-up work after maintenance in order to get the instrument ready to measure again.
Decision table
The following table helps you with further procedure:
... then... If you are going to perform the following maintenance work...
Replacing the ash crucible
Replacing sealing elements
Pulling the furnace out of the instrument
Removing or installing the quartz glass bridge
Removing the reaction tubes from the furnace
Installing reaction tubes in the furnace
Removing the reaction tubes plugs
Removing and installing the drying tube
Removing the combustion tube connection
Ball valve maintenance
Cleaning the Ni flap
... go to the following in this section:
"Preparing the instrument: Gas pressure" and to
"Follow-up instrument preparation: Gas pressure / gas-tightness".
... requires special preparation/follow-up work. This is explained in the specific instructions.
... go to Ball valve maintenance.
... got to Cleaning the Ni flap.
Safety instruction
Strictly observe the safety instruction "Gas pressure" under
Warning notes during operation
(on
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 170
"Preparing the instrument: Gas pressure"
Proceed as follows:
Shut off gas supply. Open the "Replace part" dialog in the operating software by selecting
Options > Maintenance > Replace Part .
Wait for pressure drop without pressing any buttons until the message "Part can now be replaced." is displayed and the
Finish
button becomes accessible.
Pressure has been reduced when the following displays show "0" on screen:
"MFC CO2".
"Flow CO2".
"Pressure".
The instrument is now ready for replacement of the part.
Follow-up instrument preparation: Gas pressure / gas-tightness
Proceed as follows:
Close the "Replace part" dialog in the operating software. To do so, click
Finish
in the "Replace part" dialog. This automatically switches on the gas again and the atmospheric nitrogen is removed by flushing with CO
2
.
Decide:
If...
... approximately the same flow and pressure values as prior to maintenance work are displayed: The instrument is ready to measure again.
... distinctly different flow and pressure values to those displayed prior to maintenance work are displayed: Perform a leak test. See Performing a leak test. The instrument is only ready to measure when the leak test is successful.
Conditioning newly installed tubes
Purpose of conditioning
Newly installed tubes must be conditioned:
to remove nitrogen from air inclusions in the filling material
to remove moisture from the tube fillings
to remove contaminations
Reductor ready for meaurement
Without conditioning, analysis results would be distorted.
Types of conditioning
There are the following types of conditioning new tubes:
Flushing tubes to remove nitrogen from air inclusions in the filling material. The following are flushed:
Large drying tube
Small drying tube
Baking out tubes to remove moisture and contaminations from the tube fillings. The following are baked out:
Combustion tube
Post combustion tube
Reductor
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Flushing tubes
Requirements:
A new tube has been installed.
The analyzer is in "Replace part" status.
The tube ends are closed.
171
Safety instruction
Strictly observe the safety instruction "Gas pressure" under
Warning notes during operation
(on
Proceed as follows:
Close the "Replace part" dialog in the operating software. To do so, click
Finish
in the "Replace part" dialog. This automatically switches on the gas again and the atmospheric nitrogen is removed by flushing with CO
2
.
Decide:
If the operating software status view displays...
... approximately the same flow and pressure values as prior to maintenance work are displayed: The instrument is ready to measure again. Go to the next step.
... distinctly different flow and pressure values to those displayed prior to maintenance work are displayed: Perform a leak test. See Performing a leak test. Only move on to the next step once the leak test is successful.
Performing blank value determinations. See
Determining blank values
the method "Blank with O2" to the samples.
Only stop blank value determination when the N blank value is stable and small. See "Measure of gas-tightness" in Types of blank value determination and their settings. The instrument is then ready to measure again.
Conditioning combustion tube, post combustion tube and Reductor
The following tables explains conditioning rules for the various modes:
Mode
N
Reaction tube
Combustion tube
Post combustion tube
Reductor
Conditioning rule
Bake out at working temperature for 15 minutes.
Conditioning when replacing.
Conditioning when replacing.
Heat out combustion tube, post combustion tube
Requirements:
A new combustion tube, post conbustion tube and/or Reductor has been installed.
The tube ends must be open. For this,...
... the quartz glass bridge must not be attached to the end of the combustion tube.
... the ground joint must not be clipped onto the end of the post combustion tube.
Safety instruction
Strictly observe the safety instruction "Baking out combustion and reduction tube" under
Warning notes during operation
Proceed as follows:
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 172
Close the "Replace part" dialog in the operating software. To do so, click
Finish
in the "Replace part" dialog. This automatically switches on the gas again and the atmospheric nitrogen is removed by flushing with CO
2
.
Reduce the carrier gas pressure at the delivery point until the CO
2
400 ml/min "Flow CO2" on the screen.
flow meter displays approx.
Wait the required conditioning time. Refer to the above table "Conditioning for combustion tube, post combustion and Reductor".
Close all open ends of the reaction tubes again.
Set the carrier gas intake pressure on the cylinder manometer so that...
... the "Pressure" display shows 1300 - 1350 mbar on screen.
... the measuring gas flow meter "MFC CO2" displays 700 ml/min on screen.
the CO
2
flow meter "Flow CO2" displays approx. 700 ml/min on screen.
Decide:
If the operating software status view displays...
... approximately the same flow and pressure values as prior to maintenance work are displayed: The instrument is ready to measure again.
... distinctly different flow and pressure values to those displayed prior to maintenance work are displayed: Perform a leak test. See Performing a leak test. The instrument is only ready to measure when the leak test is successful.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Performing the calibration
Target group
Personnel authorized by BÜCHI Labortechnik AG and having undergone training.
Purpose
This section provides facts about calibration and also enables you to perform calibration.
In this section
173
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 174
Viewing list of defined factor, monitor and standard samples
Viewing the list
Proceed as follows:
Open the "Standard samples" dialog in the operating software by selecting
Options > Settings >
Standards
.
The list box displays all currently defined standards. By checking the requested standard sample the settings are displayed in the right area of the dialog.
Defining standard substances
Background
These operating instructions contain specific rules for the calibration. If you want to use these rules, you must define the standard substances used there as calibration samples. Of course, you can also use different substances but then you must develop the calibration rule yourself.
Defined calibration samples are displayed along with their theoretical contents in the sample view.
Required substances
The instrument needs standard substances which represent the sample matrix to be measured.
By means of the dialog opened by
Options > Settings > Standards
you can define and/or edit the standard substances.
Defining custom standard substances
Proceed as follows:
Open the "Standard samples" dialog in the operating software by selecting
Options > Settings >
Standards .
Click
New
. The input boxes on the right area are now empty. Enter the data of the standard sample to be newly defined.
For the substance, enter...
... the name of the substance in the "name" field.
... the theoretical element content in percent in the "Conc. [%]" fields (or in ppm in the
"Conc. [ppm]" fields respectively). If you enter 0 for the theoretical element content of a substance element, the element is ignored in the calculation.
... the permissible tolerance for each element in the "Tolerance [%]" fields (usually 5%).
Click
Create
. Your new standard sample will now be included in the list in the left area of the dialog.
You have now defined the standard substance.
Click
Close
to close the dialog.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Viewing calibration coefficients
Viewing calibration coefficients
Proceed as follows:
Open the "Calibration coefficients" dialog in the operating software by selecting
Calibration >
Coefficients
.
Highlight the name of a coefficient set in the listbox.
The calibration coefficients of the coefficient set and the limits the calibration is valid within are displayed.
Optimizing instrument condition for calibration
175
Note
Note that calibration only makes sense if you have previously checked and optimized the condition of the instrument.
Why does the condition of the instrument need to be checked and optimized?
The condition of the instrument needs to be checked and optimized in order to avoid...
... leaks of the instrument.
... old tube fillings from distorting results.
Checking and optimizing the condition of the instrument
Proceed as follows:
Replace all tube fillings. See
Emptying and filling reaction tubes.
Filling the drying tube
Replace the ash crucible. See Replacing the ash crucible.
Perform a leak test. See Performing a leak test.
Determine the blank value as a measure of gas-tightness. Perform blank value determination during calibration measurement.See Types of blank value determination and their settings.
Perform test measurements so that the instrument is stable when you subsequently perform the calibration measurement. Measure 10 x 250 mg aspartic acid.
Performing the calibration
Target group
Personnel authorized by the customer. Successful calibration is only possible if the user is familiar with the operating instructions and the analyzer.
Note
Perform calibration carefully as perfect calibration is a condition for correct measuring results.
Calibration must comprise the complete working range.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 176
Process
The section is divided into the following phases:
Prepare samples and perform measurement
Ascertaining appropriate calculation methods
Set calculation methods, perform calculation
Optimizing calibration curves and apply calibration
Requirements:
Before starting work, the following requirements must be met:
Read
Background knowledge required for calibration
Assessing the calibration curves
Prepare a suitable balance. A reading precision of 0.01 mg is usually sufficient.
If you have not already done so, define the following by selecting Options > Settings >
Standards
...
... the required calibration substances. See
Defining standard substances as calibration samples
... the required substances for daily factor determination. See
Defining standard substances as factor and monitor samples
Check and optimize the condition of the instrument. Otherwise it makes no sense to calibrate.
See Optimizing instrument condition for calibration.
Phase 1: Prepare samples and perform measurement
Please observe the following instruction:
Caution
Inserting multiple samples into the ball valve (only for solid operation)
If there are samples in the carousel while you are changing the position of the carousel via System > Carousel position , multiple samples may fall into the ball valve at the same time. In this case, a service technician is required.
Before changing the position of the carousel, always remove all samples from the carousel.
Proceed as follows:
Move the empty carousel to zero position. To do so, open the "Set carousel position" dialog in the operating software by selecting
System > Sample Position
.
Select the radio button next to "Reference run" and click
OK
. The carousel moves to zero position.
Prepare the samples. Cf.
Preparing samples
Prepare the samples for determining the daily factor. Use 3 x aspartic acid at 250 mg with method "Standard".
Prepare conditioning samples and calibration samples. Refer to Calibration tables for the recommended settings for each mode.
Insert the samples on the carousel.
Enter the following sample data in the sample view (text view) on the PC:
weight in [mg] if it has not been transmitted by the balance,
the name of the sample (max. 32 characters):
"Blnk" for blank samples,
Daily factor or calibration samples must have the name defined in
Options > Settings >
Standards
.
Select an appropriate method for run-in and calibration samples according to the following list:
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 177
CalibrationLow (0 - 300 mg):
O
2
dosing time 90 sec.
O
2
flow = 225 ml/min.
O
2
cut-off threshold = 15 %.
CalibrationHigh (300 - 700 mg):
O
2
dosing time 150 sec.
O
2
flow = 300 ml/min.
O
2
cut-off threshold = 20 %.
Start the analysis process by selecting
System > Auto run
.
Check whether the O
2
field "MFC O2" on the screen displays the expected setpoint value during the combustion time. See Values for oxygen dosing.
Observe the measuring results. If the N blank value is not below 50 after stabilization: Stop continuous analysis via
System > Single
. Find out the reason of the increased blank value and correct it. Cf. Types of blank value determination and their settings.
Save the original values. See
Data backup and printing
Phase 2: Ascertaining appropriate calculation methods
Proceed as follows:
Execute the following command:
Math. > Calibration
. If sequential blank value determination is activated a message window opens showing the corresponding information.
Click Yes to continue. The "Configure calibration" dialog appears.
Define the following settings:
Check the box next to "Two calibration ranges".
Enter 1 as the polynomial degree for the lower and upper range. This corresponds to linear calculation.
Click
OK
to save your settings and close the dialog. The "Specify lower and upper calibration range" dialog appears. It displays a graph generated from the absolute contents of the samples and their peak areas in a linear calculation. The graph displays deviations of the measuring points from these lines.
Observe the measuring points and decide
what calculation would be suitable
whether you would separate the the ranges
and, if so, where you would separate the ranges.
See
Calibration curve calculation method criteria
Write down your considerations.
Click
OK
to view the readings for the other elements. For each element, decide as described before.
Write down your considerations.
Click
Cancel
.
Phase 3: Set calculation methods, perform calculation
Proceed as follows:
Execute the following command again:
Math. > Calibration
. If sequential blank value determination is activated a message window opens showing the corresponding information.
Click
Yes
to continue. The "Configure calibration" dialog appears.
Define the settings that you ascertained in the preceding phase.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 178
Click
OK
to save your settings and close the dialog.
If you have decided to split the calibration into a lower and an upper range the "Specify lower and upper calibration range" dialog appears. Set the dividing line by clicking the
<
and
>
buttons and then click
OK
.
First, the calibration curve for the lower range appears in the calibration view.
Phase 4: Optimizing calibration curves and apply calibration
Background information can be found in
Assessing the calibration curves
In order to optimize the calibration curve for each element you must exclude samples that deviate significantly from the curve. Deviations of up to ± 1.3 µg are tolerable.
Proceed as follows:
Zoom in/out the graph by selecting
View > Zoom in/out
so that you can check the overall curve.
Click the and buttons to move from sample to sample in the calibration curve and check the deviation "Diff.". Samples that display excessive deviation must be deleted.
Select a sample to delete. Then click the "Include/Exclude" button" highlighted red.
. The deleted sample is
Compare "r" (new value) and "r_old" (old value) of the calibration curve and check whether deleting has had the desired effect. See Assessing the calibration curves
If deleting has not had the desired effect, you can undo it. To do so, select the deleted sample and click the "Include/Exclude" button again. The sample is now included again.
Once you have excluded all samples with significant deviations from the calibration curve, click the "Next" button. The next calibration curve appears in the calibration view.
Once you have optimized the last calibration curve and clicked the "Next"
"Calibration coefficients" dialog is displayed.
button, the
Check...
... the calibration coefficients "a" to "e".
Note:
For the lower calibration range it is important that coefficient "a" is 1x10 -3 ... 3x10 -2 or less.
Coefficient "a" corresponds to a calibrated blank value and should be as small as possible.
... the possible working range defined in "Min." and "Max.".
Decide:
If...
... you accept the calibration coefficients: Click
OK
. The calibration coefficients are applied.
... you do not accept the calibration coefficients: Click
Cancel
. Calibration is aborted.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Assessing the calibration curves
Calibration curve display in the calibration view
After the calibration curves have been computed, the calibration points and the calibration curve for the respective element are displayed in the calibration view. The individual calibration points are displayed as circles. The following picture shows an example of a calibration curve for the nitrogen element.
179
Displayed characteristics
The following table explains the characteristics relating to the calibration curve, as displayed in the above picture:
Characteristic
Zoom a...e r r_old
Proc-SD
Description
Shows the current graph zoom factor.
Coefficients of the current polynomial.
Quality factor for the degree of fit of the current curve calculation.
For a polynomial calculation of the first degree, "r" is the correlation coefficient. The optimum is 1.
For polynomial calculations of a higher degree, "r" is the sum of error squares. The optimum is 0.
Quality factor for the degree of fit of the last curve calculation. It is used for comparison with "r". This allows you, for example, to check whether it makes sense to delete certain samples.
Process standard deviation: a measure of the degree of distribution of sample values around the calibration curve.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 180
The following table explains the characteristics relating to the sample, as displayed in the above picture:
Characteristic
Sample No.
Area
Description
Shows the analysis number of the sample selected at the cursor.
Integral of the selected sample. slope Slope of the curve at the calibration point of the selected sample.
{Element name} theo
Theoretical absolute content of the selected sample
{Element name} act
Diff.
Diff.
Absolute content of the selected sample, computed with the current curve
Difference between "theo" and "act", absolute
Difference between "theo" and "act", relative
Aids for assessing the calibration curve
The following aids are available for assessing the calibration curve:
Via
View > Zoom in / Zoom out
you can display the graph so that you can visually check the curve.
You can click on the circle to select any sample. This displays the characteristics of the sample.
You can also select a sample using the buttons characteristics of the sample.
and
Assessing the calibration curve
The following are used to assess the calibration curve:
Process standard deviation "Proc-SD"
Quality factor "r"
Coefficient "a", that corresponds to a calibrated blank value.
. This displays the
Process standard deviation "Proc-SD"
Use the following values for process standard deviation "Proc-SD" as guidelines:
Acceptable value Proc-SD = ± 3 µg in the lower range
Proc-SD = ± 15 µg in the upper range
Very good value Proc-SD = ± 1 µg
Quality factor "r"
Use the following values for quality factor "r" as guidelines:
Good value for linear calibration function r = 0.99 (r should tend to 1)
Good value for polynomial as calibration function r = < 2-4
Coefficient "a"
Use the following values for coefficient "a" as guidelines:
Acceptable range a = 1 x 10 -3 to 3 x 10 -2 or smaller
The range given here applies to calibration with one calibration range and, when calibrating with two calibration ranges, only for the lower range, while "a" may be greater in the second range.
If you do not approximately achieve the listed values you can assume that:
either you have selected the wrong calibration curve calculation mode,
or the calibration measurement has failed (weighing error, etc.).
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Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 182
Calibration tables
Target group
Personnel authorized by BÜCHI Labortechnik AG and having undergone training.
Purpose
This section contains specific rules for the calibration. If you want to use these rules, you must define the standard substances used there as calibration samples. Of course, you can also use different substances but then you must develop the calibration rule yourself.
In this section
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 183
Calibration table for nitrogen calibration
Suggestion
The following table is a recommendation for a calibration. The user can customize settings to the specific analytical task.
Number Sample type Name Method
2
1
2
20
4
Conditioning
Conditioning
Conditioning
Calibration samples
Calibration samples
Substance/
Sample weight
Aspartic acid /
300 mg ±10 mg
Aspartic acid /
10 mg
Aspartic acid /
1 mg
Aspartic acid /
1, 2, 3, 4, 5, 7 ,10,
15, 20, 25, 30, 50,
75, 100, 125, 150,
175, 200, 250,
300 mg
Aspartic acid /
350, 450, 550,
650 mg
Absolute content
1 mg ≅
0.105 mg N
650 mg ≅
68.38 mg N
RunIn
RunIn
RunIn
Aspartic acid
Aspartic acid
CalibrationLow
CalibrationLow
CalibrationLow
CalibrationLow
CalibrationHigh
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Replacing the ash crucible
Target group
Personnel authorized by BÜCHI Labortechnik AG and having undergone training.
Purpose
This section enables you to replace the ash crucible.
In this section
184
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 185
Purpose and frequency of crucible replacement
Why replace the ash crucible?
It is necessary to replace the ash crucible because combustion residue in the ash crucible can distort readings.
When to replace the ash crucible?
The intervals at which to replace the ash crucible depend very much on what substanmces you are analyzing. Generally speaking, it has to be replaced after 150 analyzed samples. When analyzing samples with extremely high mineral compound content a replacement becomes necessary.
Types of ash crucibles
The following table lists the various types of ash crucibles and their usage:
Ash crucible type
Steel ash crucible
Usage
Standard application
When analyzing liquid samples (mandatory).
Removing the ash crucible
Note
The following section describes the first part of replacing the ash crucible. The topic is continued in
Installing the ash crucible.
Process
The section is divided into the following phases:
Preparing the instrument, Gas pressure
Removing the ash crucible
Safety instruction
Strictly observe the safety instruction "Replacing the ash crucible/finger" under
Warning notes during operation
Requirements
Before starting work, the following requirements must be met:
Keep a tube rack ready to hold hot components.
Keep a tube extractor ready.
Phase 1: Preparing the instrument, cool down the furnace / gas pressure
Safety instruction
Strictly observe the safety instruction "Gas pressure" under
Warning notes during operation
(on
To prepare the instrument for maintenance work follow the instructions in "Preparing the instrument,
Gas pressure" in Preparing and following up maintenance work.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Top view furnace
The following picture shows a top view of the furnace pulled out:
Legend:
1 Post combustion tube plug
2 Post combustion tube
3 Combustion tube connection
4 Combustion tube
5 Plug of Reductor
6 Reductor
186
Phase 2: Removing the ash crucible
Proceed as follows:
Open the front door.
Unscrew the combustion tube connector. To do so, turn the bayonet catch handle (2) slowly to the right.
Remove the ground-in clamp on the reductor (3).
Remove the O
2
supply tube (6) by opening the two ground-in clamps.
Remove the ground-in clamp (5) on the post combustion tube (7).
Top view furnace
The following picture shows a top view of the furnace pulled out:
Legend:
1 Post combustion tube plug
2 Post combustion tube
3 Combustion tube connection
4 Combustion tube
5 Plug of Reductor
6 Reductor
Phase 2: Removing the ash crucible (continued)
Proceed as follows:
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 187
Press the post combustion tube plug (1) and the combustion tube connection (3) down lightly and pull the furnace out of the instrument to the front.
Pull the combustion tube connection (3) out of the combustion tube (4) with careful jiggling motions.
Place the combustion tube connection (3) on the tube rack.
Insert the tube extractor into the combustion tube (4). After clamping the crucible tongs in the ash crucible, pull the ash crucible out.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 188
Place the ash crucible in the tube rack into the vent or else on a heat-resistant surface until it has completely cooled down.
Protect the hot ash crucible from unauthorized access.
If there are any corundum balls sticking on the bottom of the ash crucible, top up some balls in the combustion tube.
Installing the ash crucible
Note
The following section is a continuation of Removing the ash crucible. All steps described there must already have been performed.
Process
The section is divided into the following phases:
Installing the ash crucible
Follow-up instrument preparation: Gas pressure / gas-tightness
Safety instruction
Strictly observe the safety instruction "Replacing the ash crucible/finger" under
Warning notes during operation
Requirements
The instrument must be in "Replace part" status. See instructions "Preparing the instrument, Gas pressure" in Preparing and following up maintenance work.
Keep a tube extractor ready.
Keep a filled ash finger ready. See Filling the combustion tube.
Top view furnace
The following picture shows a top view of the furnace pulled out:
Legend:
1 Post combustion tube plug
2 Post combustion tube
3 Combustion tube connection
4 Combustion tube
5 Plug of Reductor
6 Reductor
Phase 1: Installing the ash crucible
Proceed as follows:
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 189
Insert the new ash crucible into the combustion tube (4).
Place the combustion tube connection (3) onto the combustion tube (4). The lance must extend into the ash crucible approx. 5 - 10 mm.
Place the ungreased seal on the combustion tube connection (3) at the top.
Furnace area
The following picture shows the details of the furnace area:
Legend:
1 Bayonet catch
2 Handle
3 Connection Reductor
4 Ball valve fastening
5 Ground-in clamp
6 O
2
supply tube
7 Post combustion tube connection
Phase 1: Installing the ash crucible (continued)
Proceed as follows:
Push the furnace back:
Lift the bayonet catch (1) slightly so as not to damage the seal on the combustion tube connection.
Close the bayonet catch by turning the bayonet catch handle (2) to the left.
Close the ground-in clamp (5,3) on the Reductor again.
Connect the post combustion tube (7) with the two ground-in clamps (5) again.
Connect the O
2
supply tube (6) with a ground-in clamp (5).
Close the front door.
Phase 2: Follow-up work, gas pressure/ tightness
After completing all maintenance work, put the instrument back into a state ready for measurement.
See "Follow-up preparation of the instrument: Gas pressure / tightness" in Preparing and following up maintenance work.
To be observed after maintenance
If you have performed maintenance work that has a defined maintenance interval, you must manually reset the "Status" field to zero on the "Maintenance intervals" dialog (accessible via Options >
Maintenance > Intervals
. See Defining maintenance intervals in the software.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Refill the Regainer
Target group
Personnel authorized by BÜCHI Labortechnik AG and having undergone training.
Purpose
This section enables you to refill the Regainer.
In this section
190
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 191
Purpose and frequency of refilling of the Regainer
Why will the Regainer refilled?
It is necessary to refill the Regainer to ensure complete implementation of the sample and to avoid measurement errors. If the Regainer will not be filled up, the lifetime of the Reductor reduces drastically. For an economic operation we recommend to observe a sufficient fill level. For a refill, use the rod by pressing it tightly onto the Regainer. Due to pressure surges the Regainer may shift toward the top.
When will the Regainer refilled?
The intervals at which to refill the Regainer depend very much on what substanmces you are analyzing. Usually the Regainer should be refilled when the ash crucible will be emptied. When analyzing samples with extremely high mineral compound content a replacement becomes necessary earlier.
Refill the Regainer
Note
The following section describes the first part of refilling of the Regainer. The topic is continued in
"Refill the Regainer".
Process
The section is divided into the following phases:
Preparing the instrument, Gas pressure
Refill the Regainer
Safety instruction
Strictly observe the safety instruction "Replacing the ash crucible/finger" under
Warning notes during operation
Requirements
Before starting work, the following requirements must be met:
Keep the Regainer ready.
Keep the metal funnel ready.
Phase 1: Preparing the instrument, cool down the furnace / gas pressure
Safety instruction
Strictly observe the safety instruction "Gas pressure" under
Warning notes during operation
(on
To prepare the instrument for maintenance work follow the instructions in "Preparing the instrument,
Gas pressure" in Preparing and following up maintenance work.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Furnace area
The following picture shows the details of the furnace area:
Legend:
1 Bayonet catch
2 Handle
3 Connection Reductor
4 Ball valve fastening
5 Ground-in clamp
6 O
2
supply tube
7 Post combustion tube connection
Phase 2: Refill the Regainer
Proceed as follows:
Open the front door.
Unscrew the combustion tube connector. To do so, turn the bayonet catch handle (2) slowly to the right.
Remove the ground-in clamp (5) on the reductor (3).
Remove the O
2
supply tube (6) by opening the two ground-in clamps (5).
Remove the ground-in clamp (5) on the post combustion tube (7).
Top view furnace
The following picture shows a top view of the furnace pulled out:
Legend:
1 Post combustion tube plug
2 Post combustion tube
3 Combustion tube connection
4 Combustion tube
5 Plug of Reductor
6 Reductor
192
Phase 2: Refill the Regainer
Proceed as follows:
Press the post combustion tube plug (1) and the combustion tube connection (3) down lightly and pull the furnace out of the instrument to the front.
Pull the combustion tube connection (1) out of the combustion tube (2) with careful jiggling motions.
Place the post combustion tube plug (1) on the tube rack.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 193
Check the brass wool of the post combustion tube plug. If necessary, replace the brass wool.
Fill the Regainer by means a metal funnel into the post combustion tube (2).
To check the fill level use the rod, market with "full" and "empty".
Tap slightly against the post combustion tube after refilling the Regainer. Thus, the Regainer will be compacted in the post combustion tube.
Phase 3: Insert of the post combustion tube
Top view furnace
The following picture shows a top view of the furnace pulled out:
Legend:
1 Post combustion tube plug
2 Post combustion tube
3 Combustion tube connection
4 Combustion tube
5 Plug of Reductor
6 Reductor
Push the post combustion tube plug (1) onto the post combustion tube (2).
Push the furnace back:
Lift the bayonet catch (2) slightly so as not to damage the seal on the combustion tube connection.
Close the bayonet catch by turning the bayonet catch handle (1) to the left.
Close the ground-in clamp (3) on the Reductor again.
Connect the post combustion tube with the two ground-in clamps again.
Connect the O
2
supply tube with a ground-in clamp.
Close the front door.
Phase 4: Follow-up work, gas pressure/ tightness
After completing all maintenance work, put the instrument back into a state ready for measurement.
See "Follow-up preparation of the instrument: Gas pressure / tightness" in Preparing and following up maintenance work.
To be observed after maintenance
If you have performed maintenance work that has a defined maintenance interval, you must manually reset the "Status" field to zero on the "Maintenance intervals" dialog (accessible via Options >
Maintenance > Intervals. See Defining maintenance intervals in the software.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Replacing sealing elements
Target group
Personnel authorized by BÜCHI Labortechnik AG.
Purpose
Replacing sealing elements prevents leaks. As a result of chemical corrosion, mechanical and thermal stress, sealing elements in various components of the instrument can become leaky over time.
In this section
194
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 195
When to replace sealing elements
What sealing elements are used?
The following sealing elements are used:
Half shells
O-rings
Quad rings
Ferrules
When to replace sealing elements
The following table gives an overview of what instrument components contain which sealing elements and when to replace these sealing elements:
Instrument component
Ball valve
Quartz glass bridge
Plug of Reductor ®
Drying tube (small, left)
Combustion tube connection with Ni flap
Post combustion tube
Drying tube (large, right)
What to replace
Half shells
O-rings
O-rings
O-rings
Quad ring
O-rings
O-rings
O-ring
Quad ring
O-rings
To be replaced when...
... the ball valve is serviced and the half shells exhibit grooves.
... the ball valve is serviced and
the o-rings exhibit cracks or other damage or
the o-rings no longer protrude round out of the grooves.
... you cannot feel any elastic resistance when you press in the o-rings when installing the quartz glass bridge.
... you can hardly feel any contact pressure when inserting the Reductor plug.
... the o-rings no longer protrude round out of the grooves of the plug.
... you cannot feel any elastic resistance when pressing on the ball.
... the o-rings no longer protrude round out of the grooves of the plug.
... you can hardly feel any contact pressure when inserting the combustion tube connector into the combustion tube.
... the o-rings no longer protrude round out of the grooves of the combustion tube connector.
... you can hardly feel any contact pressure when inserting the post combustion tube plug.
... the o-rings no longer protrude round out of the grooves of the plug.
... you cannot feel any elastic resistance when pressing on the ball.
... the o-rings no longer protrude round out of the grooves of the plug.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 196
Visual o-ring/quad ring check
You can tell when o-rings or quad rings need to be replaced if they no longer protrude round out of the grooves of the respective component. The following picture shows o-rings in a closing plug as an example:
Removing sealing elements from grooves
Note
Please observe the following instruction:
Caution
Cutting sealing elements apart/out (o-rings, quad rings, half shells, ferrules).
When cutting sealing elements apart/out with a knife you may damage sealing surfaces.
Never remove sealing elements with a knife but rather with tweezers.
Removing sealing elements
Proceed as follows:
Grasp the sealing element (o-ring, quad ring, half shell, ferrule) between your thumb and forefinger.
Push the sealing element out to the side so that it forms a loop.
Grasp the loop with a pair of tweezers and pull the sealing element off.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Ball valve maintenance
Target group
Personnel authorized by BÜCHI Labortechnik AG and having undergone training.
Purpose
This section enables you to maintain the ball valve.
In this section
197
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Removing and dismantling the ball valve
Note
The following section describes the first part of "Ball valve maintenance". The topic is continued in
Cleaning, assembling and installing the ball valve.
Purpose of maintenance
Maintenance of the ball valve serves to avoid ball valve leaks. For this purpose, it is necessary to remove particles such as dust or sample abrasion that sticks between the ball and the Teflon half shells. If necessary, half shells and o-rings must also be replaced.
Process
The section is divided into the following phases:
Allow instrument to cool down and disconnect from the mains
Pulling the furnace out of the instrument
Removing the ball valve
Dismantling the ball valve
Requirements:
Before starting work, the following requirements must be met:
Remove all samples from the carousel.
Keep acetone ready to clean components.
Keep the following tools ready:
Knock-out
Hook wrench
Phillips screwdriver / Allen wrench 3 mm
Open jawed wrench, 8 mm
Open jawed wrench, 22 mm
Phase 1: Allow instrument to cool down and disconnect from the mains
198
Safety instruction
Strictly observe the safety instruction "Hot instrument parts" under
Warning notes during operation
Proceed as follows:
Switch off the furnace by means the command in the operating software
System > Furnace
.
Wait 2-3 hours until the instrument has cooled down to at least 55 °C.
Quit the operating software. Execute the following command:
File > Exit
.
Switch off the analyzer and its peripherals.
Disconnect the power supply plug.
The instrument is now ready for removal of the ball valve.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 199
Furnace area
The following picture shows the details of the furnace area:
Legend:
1 Bayonet catch
2 Handle
3 Connection Reductor
4 Ball valve fastening
5 Ground-in clamp
6 O
2
supply tube
7 Post combustion tube connection
Phase 2: Pulling the furnace out of the instrument
Proceed as follows:
Open the front door.
Unscrew the combustion tube connector. To do so, turn the bayonet catch handle (2) to the right.
Remove the ground-in clamp (5) on the reductor (3).
Remove the ground-in clamp (5) on the post combustion tube (7).
Remove the O
2
supply tube (6) by opening the two ground-in clamps (5).
Top view furnace
The following picture shows a top view of the furnace pulled out:
Legend:
1 Post combustion tube plug
2 Post combustion tube
3 Combustion tube connection
4 Combustion tube
5 Plug of Reductor
6 Reductor
Phase 3: Removing the ball valve
Proceed as follows:
Open the ground-in ball-and-socket joints of the tube (1) leading to the ball valve.
Push the right side door open from inside (magnetic lock).
From the right, unscrew the ball valve (3) locking screws using an 8mm open jawed wrench.
Pull the ball valve out of the instrument to the front.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Dismantled ball valve
The following picture shows the disassembled ball valve:
Legend:
1 Wheel flange of the half shells
2 Top and bottom half shell
3 Ball
4 Screws
5 Drive bearing
6 Holder plate
7 O-ring
8 Bayonet catch
200
Phase 4: Dismantling the ball valve
Please observe the following instruction:
Caution Cutting sealing elements apart/out (o-rings, quad rings, half shells, ferrules).
When cutting sealing elements apart/out with a knife you may damage sealing surfaces.
Never remove sealing elements with a knife but rather with tweezers.
Proceed as follows:
Unscrew and remove the wheel flange of the half shells using the hook wrench.
Unscrew the screws of the holder plate and remove the holder plate.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Remove the drive bearing.
Remove the ball and top half shell by means of the "knock-out".
201
Loosen and remove the bayonet catch.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Press the lower half shells out of the ball valve casing by means of the "knock-out".
202
Cleaning, assembling and installing the ball valve.
Note
The following section is a continuation of Removing and dismantling the ball valve. All steps described there must already have been performed.
Process
The section is divided into the following phases:
Cleaning the half shells and ball
Assembling the ball valve
Mounting the ball balve
Preparing the Instrument for measurements
Requirements
Before starting work, the following requirements must be met:
Keep the following tools ready:
Hook wrench
Phillips screwdriver / Allen wrench 3 mm
8 mm open jaw wrench.
Keep acetone ready to clean components.
The ball valve must have been removed.
The instrument must have cooled down and be disconnected from the mains when you install the ball valve again. See step 1 in Removing and dismantling the ball valve.
Safety instruction
Strictly observe the safety instruction "Hot instrument parts" under
Warning notes during operation
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Dismantled ball valve
The following picture shows the disassembled ball valve:
Legend:
1 Wheel flange of the half shells
2 Top and bottom half shell
3 Ball
4 Screws
5 Drive bearing
6 Holder plate
7 O-ring
8 Bayonet catch
203
Phase 1: Cleaning the half shells and ball
Proceed as follows:
Clean the half shells (2) and the ball (3) with acetone.
Check the half shells (2) for grooves. If there are any grooves, replace the half shells.
Check the ball (3) for grooves. If there are any grooves, replace the ball.
Phase 2: Assembling the ball valve
Proceed as follows:
Slighly grease the sealing surface of the half shells and the surface of the ball (contact surface of the ball).
Insert the bottom half shell (2) and observe the recess for the drive bearing. Insert the ball (3) and observe the position of the recess for the drive bearing.
Insert the drive bearing (6). Observe the following
the fit of the o-ring (9)
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
and that the cylinder pin snaps into the blind hole bore of the ball.
204
Insert the top half shell (2) and observe the recess for the drive bearing.
Screw the holder plate (7) onto the ball valve.
Also grease the surface of the wheel flange facing the half shells. Insert the wheel flange into the half shells (1) and tighten it by means of the hook wrench (to the stop).
Turn the ball at the drive shaft twice for a better dispersion of the grease.
Position the ball in such a way that the ball valve is open.
Remove excessive grease with a cloth by pulling the cloth through the bore.
Step 3: Installing the ball valve
For installation of the ball valve proceed in reversed sequence as it is described for its removal.
Furnace area
The following picture shows the details of the furnace area:
Legend:
1 Bayonet catch
2 Handle
3 Connection Reductor
4 Ball valve fastening
5 Ground-in clamp
6 O
2
supply tube
7 Post combustion tube connection
Phase 4: Bringing the instrument to a "ready to measure" state
Proceed as follows:
Close the right side door (magnetic lock).
Replace the carousel.
Push the furnace back:
Lift the bayonet catch (1) slightly so as not to damage the seal on the combustion tube connection.
Close the bayonet catch by turning the bayonet catch handle (2) to the left.
Close the ground-in clamp (5,3) on the Reductor again.
Connect the O
2
supply tube with a ground-in clamp (5).
Close the front door.
Switch on the furnace by means System > Furnace .
Wait for the tubes to reach the correct temperature.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 205
Once the furnaces are stable, perform a leak test. See Performing a leak test.
The instrument is only ready to measure when the leak test is successful.
To be observed after maintenance
If you have performed maintenance work that has a defined maintenance interval, you must manually reset the "Status" field to zero on the "Maintenance intervals" dialog (accessible via
Options >
Maintenance > Intervals . See Defining maintenance intervals in the software.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Maintaining the Ni flap and the O2 lance
Target group
Personnel authorized by BÜCHI Labortechnik AG and having undergone training.
Purpose
This section enables you to maintain the Ni flap and the O
2
lance.
In this section
206
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 207
Purpose and frequency of maintaining the Ni flap and O2 lance
Why maintain the Ni flap and the O
2
lance?
Maintaining the Ni flap is necessary because the side facing to the combustion chamber will soil which can result in an unsafe working of the Ni flap.
The O
2
lance will also be slightly soiled by soot which should be removed.
When to maintain the Ni flap and the O
2
lance?
It is recommended to check Ni flap and O
2 them if necessary.
lance with each replacement of the ash crucible and clean
Automatic Ni flap monitoring
Moreover, the automatic Ni flap monitoring can be enabled/disabled by the control software. As soon as the program detects a possible contamination of the Ni flap, the analysis will be aborted and a corresponding error message will be displayed. Further information about this topic:
Error handling
Removing and cleaning the Ni flap
Note
The following section describes the first part of the maintenance of the Ni flap. The topic is continued in Installing the Ni flap.
Process
The section is divided into the following phases:
Preparing the instrument, gas pressure
Removing the Ni flap
Cleaning the Ni flap and the Ni flap flange
Safety instruction
Strictly observe the safety instruction "Hot instrument parts" under
Warning notes during operation
Requirements
Before starting work, the following requirements must be met:
Keep a tube rack ready to hold hot components.
Phase 1: Preparing the instrument, gas pressure
Safety instruction
Strictly observe the safety instruction "Gas pressure" under
Warning notes during operation
(on
To prepare the instrument for maintenance work follow the instructions in "Preparing the instrument:
Cool down the furnace, gas pressure" in Preparing and following up maintenance work.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 208
Furnace area
The following picture shows the details of the furnace area:
Legend:
1 Bayonet catch
2 Handle
3 Connection Reductor
4 Ball valve fastening
5 Ground-in clamp
6 O
2
supply tube
7 Post combustion tube connection
Phase 2: Removing the Ni flap
Proceed as follows:
Open the front door.
Unscrew the combustion tube connector. To do so, turn the bayonet catch handle (2) to the right.
Remove the ground-in clamp (5) on the reductor (3).
Remove the ground-in clamp (5) on the post combustion tube (7).
Remove the O
2
supply tube (6) by opening the two ground-in clamps (5).
Top view furnace
The following picture shows a top view of the furnace pulled out:
Legend:
1 Post combustion tube plug
2 Post combustion tube
3 Combustion tube connection
4 Combustion tube
5 Plug of Reductor
6 Reductor
Phase 2: Removing the Ni flap (continued)
Proceed as follows:
Press the reductor plug (5), the combustion tube connection (3) and the post combustion tube connector (1) down lightly and pull the furnace out of the instrument to the front.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 209
Caution:
Tilting and jamming the combustion tube connection can damage the combustion tube.
Pull the combustion tube connection (3) out of the combustion tube with careful jiggling motions.
Place the combustion tube connection with Ni flap (3) on the tube rack.
Allow the flange to cool down to room temperature.
Phase 3: Cleaning the Ni flap
Proceed as follows:
Slowly pull out the O
2
lance.
Remove sooty particles from the metal surface by means of a wire brush. For cleaning the Ni flap itself use a soft brush (e.g. toothbrush).
In case of heavy contamination, both sides must be cleaned. For this purpose remove the o-rings and the O
2
lance.
Place the complete combustion tube connection with the Ni flap in ethyl alcohol or in a laboratory cleaner (duration approx. 15 min).
Brush again the metal surface and the flap itself as described above.
Remove possible residues of ethyl alcohol with water and allow the combustion tube connection to dry.
Insert the o-rings again.
Slightly grease the o-rings.
Insert the O
2
lance again.
Installing the Ni flap
Note
The following section is a continuation of "Removing the Ni flap". All steps described in "Removing the
Ni flap" must already have been performed. See: Removing and cleaning the Ni flap.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Process
The section is divided into the following phases:
Preparing the instrument, gas pressure
Installing the Ni flap
Follow-up instrument preparation, gas pressure / gas-tightness
210
Safety instruction
Strictly observe the safety instruction "Hot instrument parts" under
Warning notes during operation
Phase 1: Preparing the instrument, gas pressure
Safety instruction
Strictly observe the safety instruction "Gas pressure" under
Warning notes during operation
(on
To prepare the instrument for maintenance work follow the instructions in "Preparing the instrument:
Cool down the furnace, gas pressure" in Preparing and following up maintenance work.
Top view furnace
The following picture shows a top view of the furnace pulled out:
Legend:
1 Post combustion tube plug
2 Post combustion tube
3 Combustion tube connection
4 Combustion tube
5 Plug of Reductor
6 Reductor
Phase 2: Installing the Ni flap
Proceed as follows:
Place the combustion tube connection (3) onto the combustion tube (4). The lance must extend into the ash crucible approx. 5 - 10 mm.
Place the ungreased seal on the combustion tube connection (3) at the top.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Furnace area
The following picture shows the details of the furnace area:
Legend:
1 Bayonet catch
2 Handle
3 Connection Reductor
4 Ball valve fastening
5 Ground-in clamp
6 O
2
supply tube
7 Post combustion tube connection
Phase 2: Installing the Ni flap (continued)
Proceed as follows:
Push the furnace back:
Lift the bayonet catch (1) slightly so as not to damage the seal on the combustion tube connection.
Close the bayonet catch by turning the bayonet catch handle (2) to the left.
Close the ground-in clamp (5,3) on the Reductor again.
Connect the post combustion tube (7) with the ground-in clamp (5) again.
Connect the O
2
supply tube with a ground-in clamp (5).
Close the front door.
211
Step 3:Follow-up instrument preparation, gas pressure / gas-tightness
After completing all maintenance work, put the instrument back into a state ready for measurement.
See "Follow-up preparation of the instrument: Gas pressure / tightness" in Preparing and following up maintenance work.
To be observed after maintenance
If you have performed maintenance work that has a defined maintenance interval, you must manually reset the "Status" field to zero on the "Maintenance intervals" dialog (accessible via
Options >
Maintenance > Intervals
. See Defining maintenance intervals in the software.
Removing, cleaning and re-installing the O2 lance
Note
The following section describes the maintenance of the O
2
lance.
Process
This maintenance work is always carried out together with the maintenance of the Ni flap. The steps in Removing and cleaning the Ni flap are presumed for maintenance and removal of the O
2
lance.
Safety instruction
Strictly observe the safety instruction "Hot instrument parts" under
Warning notes during operation
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Removing the O
2
lance
Proceed as follows:
Place the combustion tube connection upside-down on the tube rack.
212
Carefully pull the O
2
lance with circular rotations out of the combustion tube connection.
Cleaning the O
2
lance
Proceed as follows:
Wipe any soot with a dry cloth.
Replace the seal made of sealing hose.
Check the lance for patency.
Installing the O
2
lance
Proceed as follows:
Pull on the lance connector (2) at the end of the O
2
lance (3). Insert the O breakage of the lance by slight rotary motions while inserting.
2
lance with the connector into the 3 mm bore (1) located across from the flap with hinge up to the stop. Avoid
After insertion the sealing hose must be set in completely into the bore and must not stick out.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 213
Removing, cleaning and installing the quartz glass bridge
Target group
Personnel authorized by BÜCHI Labortechnik AG and having undergone training.
Purpose
This section enables you to remove, clean and install the quartz glass bridge.
In this section
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Removing the quartz glass bridge
Process
The section is divided into the following phases:
Preparing the instrument, gas pressure
Removing the quartz glass bridge
Furnace area
The following picture shows the furnace area in detail:
Legend:
1 Quartz glass bridge
214
Phase 1, Preparing the instrument, gas pressure
Safety instruction
Strictly observe the safety instruction "Gas pressure" under
Warning notes during operation
(on
To prepare the instrument for maintenance work follow the instructions in Preparing and following up maintenance work.
Phase 2: Removing the quartz glass bridge
Proceed as follows:
Open the front door.
Remove the ground-in clamps from both the combustion and post combustion tube (bottom side) while holding the quartz glass bridge.
Detach the quartz glass bridge and place it on a non-combustible surface.
Protect the hot quartz glass bridge from unauthorized access.
Cleaning and installing the quartz glass bridge
What contaminations are possible?
Black residue (tar) indicate poor combustion and incorrect O
2
dosing.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
When to clean the quartz glass bridge
The quartz glass bridge must be checked for soiling after every tube change and, if necessary, cleaned.
Process
The section is divided into the following phases:
Cleaning the quartz glass bridge
Reinstalling the quartz glass bridge
Follow-up instrument preparation, gas pressure / gas-tightness
Performing the necessary follow-up work
Requirements
Before starting work, the following requirements must be met:
Remove the quartz glass bridge. Cf. Removing the quartz glass bridge.
Allow the quartz glass bridge to cool down.
Keep the following ready:
Pipe cleaner
Detergent
Distilled water
215
Safety instruction
Strictly observe the safety instruction "Installing/removing and cleaning the quartz glass bridge" under
Warning notes during operation
Phase 1: Cleaning the quartz glass bridge
Proceed as follows:
Remove the o-rings from the ground-in connection of the quartz glass bridge. Check whether the o-rings need to be replaced. See Replacing sealing elements.
Clean the quartz glass bridge. Put it...
... either into an ultrasonic bath filled with a commercial laboratory rinsing agent for 20 minutes...
... or in a commercial laboratory rinsing agent overnight.
Remove heavy contaminations with a pipe cleaner.
Then rinse the quartz glass bridge thoroughly with distilled water.
Dry the quartz glass bridge.
Insert the o-rings in the ground-in connections. Use new o-rings if necessary.
Phase 2: Re-installing the quartz glass bridge
Before starting work, the following requirements must be met:
The instrument must be in "Replace part" status. See Replacing part
The front door has to be opened.
Proceed as follows:
Connect the combustion and reduction tube with the quartz glass bridge by means of two ground-in clamps.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 216
Note:
When you close a ground-in ball-and-socket joint, you must be able to feel an elastic resistance when you press-in the o-ring, otherwise you must replace the o-ring.
Close the front door.
Phase 3: Follow-up work, gas pressure/ tightness
After completing all maintenance work, put the instrument back into a state ready for measurement. See Start-up.
Phase 4: Performing the necessary follow-up work
Proceed as follows:
Perform blank value determinations to test complete combustion. See
Determining blank values
(on page 141). Allocate an oxygen dosing time of 90 s to the sample.
Only stop the measurements once you have reached low, stable blank values. See "Measure of gas-tightness (N blan value)" in Types of blank value determination and their settings.
To be observed after maintenance
If you have performed maintenance work that has a defined maintenance interval, you must manually reset the "Status" field to zero on the "Maintenance intervals" dialog (accessible via
Options >
Maintenance > Intervals
. See Defining maintenance intervals in the software.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Removing, cleaning and installing the carousel
Target group
Personnel authorized by BÜCHI Labortechnik AG and having undergone training.
Purpose
This section enables you to remove, clean and install the carousel.
In this section
217
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Removing, cleaning and installing the carousel
Purpose of cleaning
Dust accumulations or damaged sample packings may soil the carousel in the course of time.
Cleaning the carousel prevents these foreign substances from entering the apparatus when you introduce the sample and cause errors.
Requirements:
Keep the following ready:
a soft cloth or bottle brush.
some water with a mild laboratory cleaner.
Cleaning the carousel
218
Safety instruction
Strictly observe the safety instruction "Damaged base panel" under
Warning notes during operation
Proceed as follows:
Ensure that all samples have been removed from the carousel.
Perform a reference run in order to move the carousel to the correct position.
Press both handles down and lift the carousel with the protruding handles toward the top.
Dismantle the carousel into its two component parts:
the metal ring and
the plastic top section with the ring holder magnets.
Remove the four hexagon head screws (1) with a wrench.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Lift off the ring at the pilots.
219
Clean the plastic top section and ring with
a soft cloth or bottle brush and
some water with a mild laboratory cleaner.
Allow the carousel to dry. If necessary, remove the last traces of moisture with warm air.
Replace the ring on the plastic top section and use a wrench to turn the hexagon head screws so the tips of the screws prevent you from lifting off the ring (tighten the screws only slightly). The metal ring will be held with the plastic top section by means of a magnet.
Move the plastic section until the reference hole (bore in the plastic section without number indicated by a white ring) matches the bore in the metal ring.
Insert the carousel into the holder and observe that the ejector openings of the ring must be above the ball valve.
Subsequently, perform a reference run.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Emptying and filling reaction tubes
Target group
Personnel authorized by BÜCHI Labortechnik AG and having undergone training.
Purpose
This section enables you to empty and refill reaction tubes.
In this section
220
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Emptying reaction tubes
Requirements:
Before starting work, the following requirements must be met:
The reaction tubes have been removed from the furnace.
The reaction tubes have cooled down.
Keep a tube extractor ready.
221
Safety instruction
Strictly observe the safety instruction "Emptying the reaction tubes" under
Warning notes during operation
Emptying the combustion tube
Proceed as follows:
Insert the tube extractor into the combustion tube. After clamping the crucible tongs in the ash crucible, pull the ash crucible out.
Empty the ash crucible.
Empty the copper oxide out of the combustion tube.
Remove the wire mesh ronde and the spacer out of the combustion tube.
Remove the CuO dust out of the combustion tube by means of a damp cloth.
Dispose of the chemicals according to the relevant disposal categories.
Emptying the post combustion tube
Proceed as follows:
Remove the brass wool out of the post combustion tube plug. Usually, the brass wool has turned to discolored and is used-up.
Remove the Regainer.
Remove the corundum balls.
Remove the CuO and the Pt catalyst.
Remove the corundum balls.
Remove the wire mesh ronde and the spacer.
Remove the CuO dust and, if applicable, the crust of salt by means of a damp cloth.
Dispose of the chemicals according to the relevant disposal categories.
Dispose of the Reductor
Proceed as follows:
Dispose of the Reductor to the relevant disposal categories.
Filling the combustion tube
Note
Note the following rules:
Observe the filling heights indicated as exactly as possible.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 222
The tube filling must not have any cavities. Therefore, tap the tube wall with a piece of wood or cork when filling the tubes.
Filling the combustion tube requires the use of the provided plastic tube with dimension data.
To avoid some residues of the filling material sticking to the tube walls, filling should be carried out through the plasic tube.
Correct positioning of the catalyst (CuO) and the ash crucible in the combustion tube is decisive for optimum sample combustion.
Safety instruction
Strictly observe the safety instruction "Filling reaction tubes" under
Warning notes during operation
Combustion tube filling
The following picture shows the fillings and filling heights of the combustion tube:
Legend:
1 Ash crucible
2 Corundum balls (10 mm)
3 80 g CuO + 20 g Corundum balls (87 mm)
4 Corundum balls (26 mm)
5 Wire mesh ronde
6 Spacer
Filling the combustion tube
Proceed as follows:
Place the tube in the tube rack.
Insert the spacer.
Insert the wire mesh ronde.
Fill the chemicals through the plastic tube into the combustion tube:
Fill in the corundum balls.
Pour the recommended amounts of copper oxide (CuO) and corundum balls into two small beakers; then simultaneously pour from the two beakers into the combustion tube, so that a good mixture is developed.
Fill in the corundum balls.
Insert the ash crucible.
Apply the cleaned Ni flap flange with O
2
lance.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Filling the post combustion tube
Note
Note the following rules:
Observe the filling heights indicated as exactly as possible.
The tube filling must not have any cavities. Therefore, tap the tube wall with a piece of wood or cork when filling the tubes.
For filling use the furnished plastic tube with measuring marks to avoid sticking of residues of filling material at the tube walls.
223
Safety instruction
Strictly observe the safety instruction "Filling reaction tubes" under
Warning notes during operation
Filling the post combustion tube
The following picture shows the fillings and filling heights of the post combustion tube:
Legend:
1 Plug with embedded 3.3g brass wool
2 53g Regainer (126 mm)
3 Quartz wool (10 mm)
4,180 g CuO + 15 g Pt catalyst (167 mm)
5 Corundum balls (28 mm)
6 Wire mesh ronde
7 Spacer
Filling the post combustion tube
Proceed as follows:
Place the tube in the tube rack.
Insert the spacer.
Insert the wire mesh ronde.
Fill the chemicals through the plastic tube into the post combustion tube:
Fill in the corundum balls.
Pour the copper oxide (CuO) and Pt catalyst into two separate beakers - simultaneously pour from the two beakers, so that a good mixture is developed.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 224
Fill in the quartz wool.
Fill in the Regainer.
Insert the plug at the top (filled with brass wool).
Reductor replacing
Note
The top and bottom plug of the Reductor are no consumables and therefore have to be reused.
Use both plugs for the new Reductor.
The Reductor is a consumable and should be replaced.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Removing/installing and conditioning the reaction tubes
In this section
225
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Removing the reaction tubes from the furnace
Process
The section is divided into the following phases:
Preparing the instrument, gas pressure
Removing reaction tubes
226
Safety instruction
Strictly observe the safety instruction "Removing reaction tubes" under
Warning notes during operation
Requirements
Before starting work, the following requirements must be met:
Keep a tube rack ready to hold hot components.
Phase 1, Preparing the instrument, gas pressure
In order to be able to prepare the instrument for maintenance works follow the instructions
"Preparing the instrument: Gas pressure" in Preparing and following up maintenance work.
Furnace area
The following picture shows the details of the furnace area:
Legend:
1 Bayonet catch
2 Handle
3 Connection Reductor
4 Ball valve fastening
5 Ground-in clamp
6 O
2
supply tube
7 Post combustion tube connection
Phase 2: Removing reaction tubes
Proceed as follows:
Open the front door.
Unscrew the combustion tube connector. To do so, turn the bayonet catch handle (2) to the right.
Remove the ground-in clamp (5) on the reductor (3).
Remove the ground-in clamp (5) on the plug of the post combustion tube (7).
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Top view furnace
The following picture shows a top view of the furnace pulled out:
Legend:
1 Post combustion tube plug
2 Post combustion tube
3 Combustion tube connection
4 Combustion tube
5 Plug of Reductor
6 Reductor
227
Phase 2: Removing reaction tubes, continued
Proceed as follows:
Press the reductor plug (5), the combustion tube connection (3) and the post combustion tube connector (1) down lightly and pull the furnace out of the instrument to the front.
Caution:
Tilting and jamming the combustion tube connection can damage the combustion tube.
Pull the combustion tube connection (3) out of the combustion tube with careful jiggling motions.
Place the combustion tube connection (3) on the tube rack.
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8 - Maintaining the instrument 228
Remove the quartz glass bridge. Hold the quartz glass bridge and detach the ground-in clamps.
Pull the combustion tube (4) and the post combustion tube (2) out of the furnace and place them in the tube rack. After cooling down, remove the plug of the post combustion tube.
Pull the reductor (6) out of the furnace towards the top and place it in the tube rack. Lever out the
Reductor from the lower holder by means of a screwdriver. After cooling down of the Reductor remove the top and bottom plug.
Place the tube rack on a level, non-combustible surface. Protect the hot parts from unauthorized access.
Installing reaction tubes in the furnace and conditioning
Note
The following section is a continuation of Removing reaction tubes from the furnace. All steps described there must already have been performed.
Process
The section is divided into the following phases:
Installing reaction tubes
Conditioning reaction tubes, getting the instrument ready to measure
Safety instruction
Strictly observe the safety instruction "Installing and conditioning the reaction tubes" under
Warning notes during operation
Requirements
Before starting work, the following requirements must be met:
The instrument must be in "Replace part" status. See instructions "Preparing the instrument: Gas pressure" in Preparing and following up maintenance work.
The front door must be open and the furnace must be moved out.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Clean off all fingerprints on quartz parts before installing them. This prevents premature ageing of quartz parts. Use acetone, for example, for cleaning.
Top view furnace
The following picture shows a top view of the furnace pulled out:
Legend:
1 Post combustion tube plug
2 Post combustion tube
3 Combustion tube connection
4 Combustion tube
5 Plug of Reductor
6 Reductor
229
Phase 1: Installing reaction tubes
Proceed as follows:
Close the Reductor (6) with the plug (5) and well as with the bottom plug.
Close the combustion tube (4) with the combustion tube connector (3).
Close the post combustion tube (2) with the plug (1).
Insert the reaction tubes into the furnace:
Insert the combustion tube (4) in the middle, as seen from the front; the combustion tube fixing pin (5) must snap into the holder (6).
Insert the Reductor (6) on the right, as seen from the front.
Insert the post combustion tube (2) on the left, as seen from the front.
Check that the reaction tube comes to rest on the bottom of the holder. The holders are height-adjustable so as to allow for reaction tube length tolerances.
Install the quartz glass bridge between the combustion tube outlet and the post combustion tube inlet.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Note:
When you close the ground-in ball-and-socket joints, you must be able to feel an elastic resistance when you press the o-rings into the pans, otherwise you must replace the o-rings.
230
Place the ungreased seal on the combustion tube connection (3) at the top.
Check whether the seals are in the pans of the plugs of combustion and post combustion tube.
Furnace area
The following picture shows the details of the furnace area:
Legend:
1 Bayonet catch
2 Handle
3 Connection Reductor
4 Ball valve fastening
5 Ground-in clamp
6 O
2
supply tube
7 Post combustion tube connection
Phase 1: Installing the reaction tubes, continued
Proceed as follows:
Push the furnace back:
Lift the bayonet catch (2) slightly so as not to damage the seal on the combustion tube connection.
Close the bayonet catch by turning the bayonet catch handle (1) to the left.
Leave the end of the post combustion tube open.
Close the front door.
Phase 2: Conditioning the combustion tube, post combustion tube and Reductor
Proceed as follows:
Close the "Replace part" dialog in the operating software. To do so, click
Finish
in the "Replace part" dialog. By doing so, the gas will be automatically turned on. and the atmospheric nitrogen is removed by flushing with CO
2
for five minutes.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 231
Reduce CO
2
pressure at the delivery point until the CO screen at approx. 400 ml/min.
2
flow meter displays "Flow CO2" on
Wait the required conditioning time. See table of "conditioning rules" in Conditioning newly installed tubes.
Close the ground-in clamp on the reductor outlet.
Set CO
2
intake pressure on the cylinder manometer so that...
... the "Pressure" display shows 1300 - 1350 mbar on screen.
... the measuring gas flow meter "MFC-TCD" displays 700 ml/min on screen.
... the CO
2
flow meter "Flow CO2" displays approx. 700 ml/min. on screen.
Decide:
If approximately the same flow and pressure values as prior to maintenance work are displayed: The instrument is ready to measure again.
If distinctly different flow and pressure values to those displayed prior to maintenance work are displayed: Perform a leak test. See Performing a leak test. The instrument is only ready for further conditioning when the leak test is successful.
To be observed after maintenance
If you have performed maintenance work that has a defined maintenance interval, you must manually reset the "Status" field to zero on the "Maintenance intervals" dialog (accessible via
Options >
Maintenance > Intervals
. See Defining maintenance intervals in the software.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 232
Filling, removing and installing the absorption and drying tubes
Target group
Personnel authorized by BÜCHI Labortechnik AG and having undergone training.
Purpose
This section enables you to fill, remove and install the drying tubes.
In this section
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 233
Filling the drying tubes
Note
Note the following rules:
Observe the filling heights indicated as exactly as possible.
The tube filling must not have any cavities. Therefore, tap the tube wall with a piece of wood or cork when filling the tubes.
If the Sicapent® cannot be tapped properly, also a glass rod for slight compacting can be used.
Since the life time depends on the amount of Sicapent®, it is recommended to achieve a mean density as high as possible. In doing so, make sure that the carrier gas flow will not be impaired.
Drying tube filling (small)
The following picture shows the fillings of the drying tube:
Legend:
1 Empty space
2 Cotton (10 mm)
3 Sicapent® (116 mm)
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument
Drying tube filling (large)
The following picture shows the fillings of the drying tube:
Legend:
1 Empty space
2 Cotton (10 mm)
3 Sicapent® (314 mm)
234
Safety instruction
Strictly observe the safety instruction "Filling the drying tube" under
Warning notes during operation
Filling the drying tubes
Proceed as follows:
Disconnect both tubes.
Remove the glass tube.
Detach the screw-on caps.
Leave approx. 5 mm space (1) at the end of the tube.
Plug approx. 10 mm of cotton (2) into the tube so that it comes to rest above the empty space
(3).
Fill in enough Sicapent® (3) to leave approx. 15 mm space at the top of the tube. To do so, tap the tube wall with a piece of wood or cork so as to prevent cavities. If the Sicapent® cannot be tapped properly, also a glass rod for slight compacting can be used.
Clean any Sicapent® off the end of the tube.
Plug approx. 10 mm of cotton over the Sicapent®.
Replace the screw-on caps and tighten them on the glass tube by hand.
Push the glass tube between the clamps and close the tubes.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 235
Notes regarding further operation
The drying tube fillings must be replaced regularly in order to ensure correct readings. The drying agent is charged with an indicator which shows the used up zones of the tube. If ¾ of the desiccant is discolored, the filling must be replaced.
Removing and installing the drying tubes
Function of the drying tubes
The drying tubes bind traces of water that would impair both the detector signal and the lifetime of the
IR detector.
Location of the drying tubes
The following picture shows the location of the drying tubes (1, 2) with the front door open:
Process
The section is divided into the following phases:
Preparing the instrument, gas pressure
Removing the drying tubes
Installing the drying tubes, getting the instrument ready to measure
Safety instruction
Strictly observe the safety instruction "Installing/removing the drying tube" under
Warning notes during operation
Phase 1, Preparing the instrument, gas pressure
Safety instruction
Strictly observe the safety instruction "Gas pressure" under
Warning notes during operation
(on
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
8 - Maintaining the instrument 236
To prepare the instrument for maintenance work follow the instructions in Preparing and following up maintenance work.
Phase 2: Removing the drying tubes
Proceed as follows:
Open the front door.
Loosen the ground-in clamps at the small dryting tube (1).
Remove the small drying tube (1) from the instrument and unscrew the red caps.
Unscrew the large drying tube (2) from the top. Loosen the red cap.
Lossen the ground-in clamp on the bottom of the large drying tube (2).
Remove the large drying tube (2) from the instrument and unscrew the red cap.
Phase 3: Installing drying tubes, getting the instrument ready to measure
Proceed as follows:
Screw on the red caps onto the drying tubes.
Fasten the small drying tube again by means of the ground-in clamps.
Install the large drying tube.
Screw the large drying tube (2) tightly on top with the red cap.
Close the front door.
Close the "Replace part" dialog in the operating software. To do so, click
Finish
in the "Replace part" dialog. By doing so, the gas will be automatically turned on. and the atmospheric nitrogen is removed by flushing with CO
2
for five minutes.
Decide:
If...
... approximately the same flow and pressure values as prior to maintenance work are displayed: The instrument is ready to measure again.
... distinctly different flow and pressure values to those displayed prior to maintenance work are displayed: Perform a leak test. See Performing a leak test. The instrument is only ready to measure when the leak test is successful.
To be observed after maintenance
If you have performed maintenance work that has a defined maintenance interval, you must manually reset the "Status" field to zero on the "Maintenance intervals" dialog (accessible via Options >
Maintenance > Intervals
. See Defining maintenance intervals in the software.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
C H A P T E R 9
Repairing the instrument
Target group
Personnel authorized by BÜCHI Labortechnik AG and having undergone training.
Purpose
This section is designed to restore proper working order of the instrument.
In this chapter
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
9 - Repairing the instrument 238
Interpreting PC error messages
Software reaction to errors
When an error is detected, the software displays its error code on screen and saves it to the "error buffer".
If the error is a critical error, the instrument is stopped immediately.
If the error is a non-critical error, the instrument is only stopped:
if you have defined a maximum number of permissible errors in the Options Settings
Error Handling menu
and
the maximum number has been exceeded defined in
Options > Settings > Error
Handling
.
On-screen error message
When an error is detected the "Error information window" is displayed on screen. Here, the name of the module which has detected the error as well as the error number is displayed.
Interpreting error code
Proceed as follows:
Open the "Error buffer" dialog by selecting
Options > Diagnostics > Error Buffer
.
Double-click on the error code you want to interpret in the "Event" column.
This displays the "Error display" dialog that is automatically open at the appropriate tab. The causes of the error are indicated by a red dot.
The error texts have different colors.
red: Critical error. Requires immediate correction.
blue: Warning. Requires no activity for now. If occuring repeatedly with succeeding analyses, look for the cause and find a remedy.
green: Hint. Informs about an unusual behaviour, however, under normal circumstances no activities are necessary.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
9 - Repairing the instrument 239
Interpreting combustion module error messages and troubleshooting
The following table lists combustion module error messages, explaining the causes of the errors and giving tips for troubleshooting:
Possible causes Measures for troubleshooting* Combustion module error messages
Ambient temperature too high
Fan failure.
Front door of the instrument was open too long.
Release the thermoclick (1) above the furnace again. (Press pin)
Then restart the instrument and the software.
Cf. last step in Replacing fuses. If unsuccessful, please contact the service department.
*Illustrations may vary in instrument type and model.
Performing a system test
What does the system test check?
The system test checks the following components of the analyzer for proper functioning:
Furnaces
Fan
Ball valve
Ni flap
MFCs
Valves
Performing a system test
Perform the system test in consultation with the service department. The service department will give you the necessary instructions to perform the system test.
You can contact the service under: www.buchi.com
Further information
Further information can be found in:
System test.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
9 - Repairing the instrument
Performing a leak test
Purpose of the leak test
The leak test checks the instrument for leaks.
Performing a leak test
The leak test consists of a total leakage test and a subsequent leak test stages.
The leak test stages checks the gas-tightness of the system by using severer criteria and, in case a leak has been detected, supports you during the leak search procedure.
Proceed as follows:
Click
Options > Diagnosis > Leak test
. A message window appears which requests you to confirm the execution of the leak test once more.
Click
Yes
to start the leak test. The program opens the "Leak test: Whole device" dialog. The tubing diagram of the analysis system is displayed.
Click
Start
to begin "Whole System" leak test. The "Leak test: Whole device" dialog appears.
The leak test begins. On the left, the arrow indicates the current stage of the leak test.
The result of the leak test is displayed at the bottom:
240
If the leak test has passed the symbol becomes visible.
If the leak test has failed the symbol becomes visible.
Print out the result if you wish. Click
to do so.
Click
Close
to close the dialog again.
If the test for the whole system has not been passed, click now
Next
. This will activate the next test stage. Here you will be informed how to proceed. Click
Start
to continue with the corresponding test stage. The "Test Phases" dialog will open again showing the status of the currently running test stage.
Note:
Switching to the next test stage is only possible during performing a fine leak test!
Continue with the stages described above until the result "Leak test not passed" is displayed.
The leak is then probably located at the blue indicated gas ways.
Further information
Leak test.
Leak test: Test phases
Leak test procedure
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
9 - Repairing the instrument 241
Leak test procedure
Process
The execution of the leak test takes place in several steps. The leak test always starts with testing of the whole system (Whole leak test). If the program detects a leak during the whole leak test, it will provide additional test stages. The purpose of these test stages is to test only a certain section of the system in sequence. As long as no leak can be detected the next section will be added to the test.
However, after a leak has been detected, the location of the leak must be inside the section added last. In the "Leak test" dialog the tubing diagram of the analyzer is displayed. The gas ways are colored differently depending on the test stage carried out currently:
No coloring: Whole leak test and/or gas ways not tested yet,
Blue coloring: Gas way currently under test,
Green coloring: Gas ways already tested.
By means of this coloring a detected leak can be localized easily: It must be in the blue colored section.
A test stage is started by clicking the
Start
button. The "Leak test" dialog will open. Here, the test run can be observed.
Each leak test stage takes place in the following phases::
Pressure build-up
Stabilization
Test
Pressure build-up
During this stage, the valves are switched to positions allowing pressure build-up in a certain section of the system.
Stabilization
During this stage, first the gas inlet valve is closed. The system waits for a set time to allow stable pressure conditions in the subsequent test stage. If system pressure does not reach a defined minimum pressure after this stage has ended, the leak test is regarded as having failed. If minimum pressure is reached, the system moves on to the next stage.
Test
During this stage, first the system maintains the initial pressure of the instrument. During this stage of the test, the system constantly compares current pressure with the initial pressure previously measured and calculates the current drop in pressure. If the drop in pressure exceeds a certain threshold during this stage of the test, the leak test is regarded as having failed. If the drop in pressure stays below the threshold, the system moves on to the next stage.
Replacing fuses
The fuses
The following table lists the different fuses.
Fuse holder label
F1
F2
F3
F5 + F6
Responsible for...
Heater 1
Heater 2
Heater 3
Power supply
Fuse specifications
25 A
10 A
10 A
10 A
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
9 - Repairing the instrument
F7 + F8
Process
Furnace transformer
The section is divided into the following phases:
Allow instrument to cool down and disconnect from the mains
Remove and check fuse
Insert fuses
Switch the instrument on again
Note
15 A
242
Please note:
If the fuses trip, please always notify your service office as there may be serious reasons for this.
Only use fuses matching the indicated type and the indicated voltage on the fuse holder. No fuses with a higher amperage (A) may be used.
Safety instruction
Strictly observe the safety instruction "Replacing fuses" under
Warning notes during operation
(on
Phase 1: Allow instrument to cool down and disconnect from the mains
Proceed as follows:
Set the furnace off by
System > Ofen
.
Wait 2-3 hours until the instrument has cooled down to at least 55 °C.
Quit the operating software. Execute the following command:
File > Exit
.
Switch off the analyzer and its peripherals.
Disconnect the analyzer from the mains. Disconnect the power supply plug.
The instrument is now ready for removal of the fuses.
Fuse holder
The following picture shows a fuse holder from the side:
Phase 2: Remove and check fuse
Proceed as follows:
If a part of the instrument is no longer working, consult the above table to find out which fuse is resposible for the component.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
9 - Repairing the instrument
First remove the rear wall. To do that, unscrew the rear wall retaining screws and pull the protective earth conductor connector out of the rear wall. The following picture shows the protective earth conductor connector:
243
Then remove the rear wall.
Loosen the knurled screw (1) of the semiconductor relay holding plate (2) and fold out the semiconductor relay holding plate.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
9 - Repairing the instrument
The electrical section is now visible.
244
Pull out the fuse holder of the appropriate fuse.
Press the fuse out.
Check the fuse:
If the fuse wire...
... is visible: Check whether the wire is broken or not.
... is not visible: Measure fuse continuity.
Make a decision for the further proceeding:
If...
... the fuse wire is broken: Insert a new fuse of the same type.
... no continuity was measured on the fuse: Insert a new fuse of the same type.
... the fuse wire is OK: Insert the old fuse again.
... continuity was measured on the fuse: Insert the old fuse again.
Phase 3: Insert fuses
Proceed as follows:
Make sure that the fuse specifications match the label on the fuse holder.
Insert the fuse into the appropriate fuse holder and tighten the semiconductor relay holding plate again.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
9 - Repairing the instrument
Plug the protective earth conductor back into the rear wall.
245
Attach the rear wall again.
Phase 4: Switch the instrument on again
Proceed as follows:
Plug the power supply plug of the analyzer into the socket.
Switch
PC,
monitor
and printer on.
Wait until the boot process is completed.
Launch the operating software. See
Starting the operating software
Set the normal temperatures as the setpoint temperature of the furnaces under System >
Furnace
.
Once the setpoint temperatures have been reached the instrument is ready to measure again.
What to do after a computer crash
After a computer crash
Because open documents are saved to a temporary file every 3 minutes, large-scale loss of data is not usual. After a computer crash, restart the operating software and the software automatically loads the most recent temporary file.
Reacting to a power failure
Open document
An open document is not lost in the event of a power failure. The temporary document file is automatically loaded when the operating software is restarted.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
9 - Repairing the instrument
What to do after a power failure
Depending on when the power failure occurred, proceed as follows:
Case
When the power failure occurred while you were performing an analysis and there was a sample in the analyzer.
Although you were performing an analysis when the power failure occurred, there was no sample in the analyzer.
The analyzer was in standby mode when the power failure occurred. The power failure lasted longer than 15 minutes.
The analyzer was in standby mode when the power failure occurred. The power failure lasted less than 15 minutes.
Procedure
Follow the instructions in "Reacting to a power failure during analysis".
Follow the instructions in "Reacting to a power failure".
Follow the instructions in "Checking the gastightness of the instrument".
No special measures required.
246
Reacting to a power failure during analysis
Please observe the following instruction:
Caution
Inserting multiple samples into the ball valve (only for solid operation)
If there are samples in the carousel while you are changing the position of the carousel via
System > Carousel position
, multiple samples may fall into the ball valve at the same time. In this case, a service technician is required.
Before changing the position of the carousel, always remove all samples from the carousel.
Proceed as follows:
If the analyzer is still switched on, switch it off and wait for a moment.
Switch the analyzer on again.
If the ball valve...
... audibly does perform a reference run: Go to the next step.
... ...does not perform a reference run: Disconnect the instrument from the mains, check the fuses and replace them if necessary. See Replacing fuses. After replacing the fuse repeat this step.
Restart the operating software. The temporary file of the most recent document is loaded.
All measuring results exist except for the most recent sample. A message appears which informs that the sample position is not definied and a reference run has to be carried out.
Confirm this message by clicking
OK
. This displays the "Adjusting the carousel position dialog.
without removing the carousel, remove all remaining samples from the carousel. Confirm this in the dialog by checking "All samples removed from carousel". Then move the empty carousel to zero position ("Reference run" radio button). Cf.
Changing the position of the carousel
(on
Create a backup of the current document via
File > Save as
.
Perform a leak test by selecting
Options > Diagnostics > Leak Test
.See Performing a leak test.
If a leak is identified, replace the sealing elements in the furnace area. See Replacing sealing elements.
There may still be some residue of the last sample in the combustion section. Perform blank value determinations to remove the residues. See Determining blank values
Correct the number of the current sample via
Edit > Current sample
. See Adjusting the current sample.
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9 - Repairing the instrument 247
Insert additional sample lines at the top of the sample view for a daily factor determination via
Edit > Insert Line
.
Prepare daily factor samples and place them on the carousel. Put the other samples behind this.
Restart the measurement via
System > Continuous
.
Reacting to a power failure
Please observe the following instruction:
Caution
Inserting multiple samples into the ball valve (only for solid operation)
If there are samples in the carousel while you are changing the position of the carousel via
System > Carousel position
, multiple samples may fall into the ball valve at the same time. In this case, a service technician is required.
Before changing the position of the carousel, always remove all samples from the carousel.
Proceed as follows:
If the analyzer is still switched on, switch it off and wait for a moment.
Switch the analyzer on again.
If the ball valve...
... audibly does perform a reference run: Go to the next step.
... ...does not perform a reference run: Disconnect the instrument from the mains, check the fuses and replace them if necessary. See Replacing fuses. After replacing the fuse repeat this step.
Restart the operating software. The temporary file of the most recent document is loaded.
All measuring results exist except for the most recent sample. A message appears which informs that the sample position is not definied and a reference run has to be carried out.
Confirm this message by clicking
OK
. This displays the "Adjusting the carousel position dialog.
without removing the carousel, remove all remaining samples from the carousel. Confirm this in the dialog by checking "All samples removed from carousel". Then move the empty carousel to zero position ("Reference run" radio button). Cf.
Changing the position of the carousel
(on
Create a backup of the current document via
File > Save as
.
Perform a leak test by selecting Options > Diagnostics > Leak Test .See Performing a leak test.
If a leak is identified, replace the sealing elements in the furnace area. See Replacing sealing elements.
Correct the number of the current sample via
Edit > Current sample
. See Adjusting the current sample.
Insert additional sample lines at the top of the sample view for a daily factor determination via
Edit > Insert Line
.
Prepare daily factor samples and place them on the carousel. Put the other samples behind this.
Restart the measurement via
System > Continuous
.
Checking air-tightness of instrument
Proceed as follows:
Perform a leak test to check the air-tightness of the instrument. See Performing a leak test.
If any leaks are detected, replace all sealing elements in the furnace area. See Replacing sealing elements.
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9 - Repairing the instrument 248
Stopping continuous analysis
When do I stop continuous analysis?
It makes sense to stop a continuous analysis in the following cases:
If the result of the blank value indicates that the instrument is leaky.
If the results of the conditioning sample indicate that parts of the instrument are defective or that gas pressure and flow behaviors are not OK.
If results of the daily factor deviate substantially from the last results.
Stopping a continuous analysis spontaneously
Proceed as follows:
Execute the command System > Single run in the operating software.
This stops the analysis after measuring the current sample.
Moving a stop marker
The program automatically moves the stop marker to the last sample position during sample data input. It is therefore only necessary to move the stop marker in special cases.
Nevertheless, if for any reason you have to move the stop marker proceed as follows:
Open the "Set stop marker" dialog by selecting
Edit > Stop tag
.
Use the arrow buttons to set the sample number at which to set a stop marker.
Click
OK
. This closes the dialog and moves the stop marker to the desired position.
Re-weighing after sample loss
Sample loss
If you drop a sample on the floor when loading the carousel, for example, the sample is contaminated and should not be analyzed. You have to prepare and weigh a new sample.
Re-weighing after sample loss
Proceed as follows:
Prepare the sample again.
Open the "Set current weight" dialog by selecting
Edit > Current weight
.
Use the arrows to specify the sample to re-weigh.
Click
OK
. This closes the dialog and the cursor moves to the "Weight" column of the selected sample number.
If 21 CFR Part 11 functionality is enabled, the "Comment change" dialog is displayed. Enter a justification in the "Comment modification" dialog and click
Close
.
Weigh the sample If the weight is not transmitted online, enter the weight by hand in the sample view on the PC.
Insert the new sample on the carousel.
Open the "Set current weigt" dialog again by selecting
Edit > Current weight
.
Use the arrows to set the number following the number of the last sample.
Click
OK
. This closes the dialog and the cursor moves to the "Weight" column of the selected sample number.
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9 - Repairing the instrument 249
If 21 CFR Part 11 functionality is enabled, the "Comment change" dialog is displayed. Enter a justification in the "Comment modification" dialog and click
Close
.
Changing the position of the carousel
When is this necessary?
It is necessary to change the position of the carousel in the following cases:
If the analyzer was switched off, the carousel is no longer in zero position. Before you can start an analysis, you must move the carousel back to zero position.
If you lose samples, it may be necessary to move the carousel to a different position.
Changing the position
Please observe the following instruction:
Caution
Inserting multiple samples into the ball valve (only for solid operation)
If there are samples in the carousel while you are changing the position of the carousel via System > Carousel position , multiple samples may fall into the ball valve at the same time. In this case, a service technician is required.
Before changing the position of the carousel, always remove all samples from the carousel.
Proceed as follows:
Remove all samples from the carousel.
Open the "Set carousel position" dialog via
System > Sample Position
.
Once you have removed all samples from the carousel, check the checkbox next to "All samples removed from carousel".
Decide:
If you want to...
... move the carousel to a position other than zero position, select the radio button next to
"Position" and use the arrows to set the position in the box next to it.
... move the carousel to the zero position, select the radiobutton next to "Reference run".
Click
OK
. This closes the dialog and moves the carousel to the desired position.
Export analysis data for support
Export for support
The service department can draw conclusions about the condition of the analyzer from the analysis data, particularly the graphical information. Therefore, analysis data must be exported in sqlite format for support, as this also contains graphical data.
Exporting analysis data
Proceed as follows:
Open the "Export document" dialog in the operating software by selecting File > Export/Import >
Export
.
Select the desired document file and click
OK
. This displays the "Save file as" dialog.
Select the directory to export the document to from the "Save" dropdown listbox.
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9 - Repairing the instrument 250
Select the "SQLite Files (*.sqlite) file type from the "File type" dropdown listbox and click
Save
.
The document is exported and saved under the corresponding name.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
C H A P T E R 1 0
Menu and dialog descriptions
Target group
Personnel involved with the instrument.
Purpose
This section describes the dialogs and commands in the various menus in the software.
Note
The order of the menu commands in this document corresponds to the menu structure of the instrument software.
If the invokation of a menu command opens a dialog the corresponding dialog wil be described directly instead of describing the menu command.
In this chapter
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Dialog descriptions key
Element types
The following list provides pictures of element types that feature in the dialog descriptions:
Element type
Label
Example picture
Dropdown listbox
Checkbox
Listbox
Radiobutton
Button
Sliding controller
Listbox column
252
Textbox
Textbox/label
Textbox with checkbox
Textbox with buttons
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
File menu
Purpose
This section describes commands and dialogs for this menu.
In this section
253
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
File > New (Command)
What is the command used for?
This command creates a new document.
Short cuts
254
Invocation via the toolbar:
Invocation via hot key: CTRL + N
Select document name (Dialog)
Function
The function of this dialog differs depending on how you open it:
If it was opened via File > Export/Import > Export , you can select a document to be exported.
If it was opened via
File > Open
you can select a file to load from the database into sample memory.
If it was opened via
File > Save
or
File > Save as
you can select a file to save from the sample memory into the database.
Open
Open the dialog via:
Menu command
Datei > Export/Import >
Export
File > Open
Button
---
Hot key
CTRL + E
CTRL + O
File > Save
CTRL + S
File > Save As.
--- ---
Elements
The following describes the elements of the dialog.
Label
---
Name / Date /
Time / Author /
Mode / Previous versions /
Signatures
Selection
Element type
Textbox/label
Listboxes
Checkbox
Meaning
Field to input a document name, that is automatically completed if necessary.
Field displaying a document name if a document is selected in the listbox below.
Fields listing all documents in the database if the filter function is not enabled.
If activated the filter elements "Mode", "From", "To",
"Name" and "Author" will appear.
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10 - Menu and dialog descriptions 255
Label
Mode from to
Name
Author
OK
Previous versions
Cancel
Signatures
Element type
Dropdown listbox
Textbox with checkbox
Textbox with checkbox
Textbox
Textbox
Button
Button
Button
Button
Meaning
Field in which you can select the operating mode as the filter criterion. Only documents in the selected operating mode are displayed.
Field in which you can select a date as the filter criterion.
Only documents as from the selected date are displayed if the checkbox next to the date display is checked.
In connection with the "To" textbox you can limit the display to documents in a certain period.
Field in which you can select a date as the filter criterion.
Only documents up to the selected date are displayed if the checkbox next to the date display is checked.
In connection with the "From" textbox you can limit the display to documents in a certain period.
Field in which you can select a document name as the filter criterion. Only documents with the selected name are displayed. Wildcards such as ? and * are also allowed.
Field in which you can select an author as the filter criterion. Only documents from the selected author are displayed. Wildcards such as ? and * are also allowed.
Depending on how the dialog was opened:
Loads the selected document in the current version
(
File > Open
)
or saves data under the selected name in the database. (
File > Export/Import > Export
;
File >
Save
;
File > Save as
)
Opens the "Select version" dialog in which you can select a version of the document. When you select a previous version you cannot edit it but only view or print it out.
Previous versions are read-only.
Opens the "Verify digital signatures" dialog in which you can verify a document's digital signatures.
Aborts the process.
Depending on how the dialog was opened, some elements may not be enabled.
Listbox columns
The following describes the columns of the listbox.
Label
Name
Date/Time
Author
Element type Meaning
Listbox column Document name
Listbox column Date and time when the document was last saved.
Listbox column Name of the user who was logged in at the time of last saving.
Mode Listbox column Analysis mode in which the document was created. The document can only be loaded in the mode in which it was created, otherwise a message is displayed.
Previous versions Listbox column A figure in parentheses indicates how many previous versions of the document exist.
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Label
Signatures
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Data backup and printing
Exporting analysis data to MS Excel and viewing
Finding documents
Creating new documents
Export analysis data for support.
Select version (Dialog)
Function
Element type Meaning
Listbox column Column displaying for what purpose the document was already signed.
If the document is unsigned, the column is empty.
For the first signature the column displays "created".
For the second signature the column displays "checked".
For the third signature the column displays "released".
Documents with a signature cannot be edited after loading but rather only viewed or given another signature for monitoring purposes.
In this dialog you can select a version of a document and load it from the database into sample memory. This dialog is only relevant if 21 CFR Part 11 functionality is enabled.
Open
Open the dialog by clicking the
Previous versions
button in the "Select document name" dialog.
Elements
The following describes the elements of the dialog.
Label
---
---
OK
Cancel
Element type
Label
Listbox
Button
Button
Meaning
This field displays the document to load if you selected a document in the listbox below.
This field lists all versions of document in the database along with the index number, creation date, and user name:
The current version is prefixed with index number 0.
Previous versions are prefixed with index numbers -1,
-2, etc.
Loads the selected version into sample memory.
If you load a previous version, you cannot edit it but only view or print it out. Previous versions are read-only.
Aborts the process.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Finding documents
Versioning
21 CFR Part 11 functionality
Consequences of modifying analysis data
Select document name
Save file as (Dialog)
257
Function
In this dialog you can specify the following for the file to export:
Directory in which to save the export file,
File name of the export file,
File type of the export file.
Open
Open the dialog by selecting
File > Export/Import > Export
. First the "Select document name" is displayed in which you select the export file before the "File saves as" dialog is displayed.
Elements
The following describes the elements of the dialog.
Label
Save
---
File name
File type
Save
Cancel
Element type
Dropdown listbox
Listbox
Textbox/label
Dropdown listbox
Button
Button
Meaning
Field in which you select the directory to save in.
Field displaying all files in the selected directory that match the file type specified below.
Field displaying the name of the file selected in the previous "Select file name" dialog. You can still edit this name.
Field in which you select the file type for the document export.
MS Excel format (export without graphical information)
MS Access database file (export with graphical information)
Exports the file according to the settings.
Aborts the process.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Exporting analysis data to MS Excel and viewing
Export analysis data for support.
Overview of export and import file formats.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
File > Delete (Command)
258
What is the command used for?
This command allows you to remove the current open document from the database. Before deleting, the program displays a dialog in which you must confirm that you want to delete the document.
Note
If 21 CFR Part 11 functionality is enabled, the "Comment change" dialog is displayed after deleting the document from the database. The user must justify deletion of the document in this dialog.
Comment modification (Dialog)
Function
In this dialog the user must justify certain actions with a comment. The comment input in this dialog is stored in the logbook together with information on the action. This allows you to track actions performed by various users.
Open
The dialog opens automatically,
if the user makes any changes that have to be commented
and if 21CFR functionality is enabled.
Elements
The following describes the elements of the dialog.
Label
---
Close
Element type
Textbox
Button
Meaning
Field to input a comment.
The comment must be at least 10 characters long.
Closes the dialog.
The button is only enabled if the comment contains 10 characters or more.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Granting authorizations
Reorganize database
Defining logon timeout
Creating new sections
Defining the analyzer / PC interface
Defining the autoexport directory
21 CFR Part 11 functionality
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Sign (Dialog)
259
Function
In the dialog:
the user is warned about signing documents that may still need to be edited. After signing, the document is read-only.
you can sign a document with an electronic signature. A document may be signed up to three times.
Open
You can open this dialog, if 21CFR11 functionality is enabled, via File > Sign :
Elements
The following describes the elements of the dialog.
Label created checked released
Name
Password
Signing
Cancel
Element type
Radiobutton
Radiobutton
Radiobutton
Textbox
Textbox
Button
Button
Meaning
The "created" signature is assigned to the document.
This is the first signature a document may receive.
The "checked" signature is assigned to the document.
A document may only be given the "checked" signature if it has already been given the "created" signature.
The "released" signature is assigned to the document.
A document may only be given the "released" signature if it has already been given the "created" and "checked" signatures.
Field to input the user's name defined in the signature program.
Field to input the password defined in the signature program.
Creates the signature. The program checks whether the signature is valid on the basis of a key. The result of the signature authenticity check is displayed in another dialog.
Aborts the process.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Signing documents
21 CFR Part 11 functionality
Verify digital signature (Dialog)
Function
In this dialog you can verify the authenticity of a document's digital signatures. This dialog is only relevant if 21 CFR Part 11 functionality is enabled.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Open
You can open this dialog, if 21 CFR Part 11 functionality is enabled, via:
File > Verify
or via
the
Signatures
button in the "Select document name" dialog.
Elements
The following describes the elements of the dialog.
Label created checked released
Verify
Cancel
Element type
Radiobutton
Radiobutton
Radiobutton
Button
Button
Meaning verify "created" signature.
If the radio button is locked, the signature does not yet exist.
verify "checked" signature.
If the radio button is locked, the signature does not yet exist.
verify "released" signature.
If the radio button is locked, the signature does not yet exist.
Starts verification of the selected signature.
Opens a dialog displaying the results of verification.
Aborts the process.
260
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Checking documents for authenticity
21 CFR Part 11 functionality
Database
Export to LIMS (Dialog)
Function
In this dialog you can specify how to perform manual transfer to a higher-level LIM system before the transfer is started.
Open
Open the dialog by selecting File > Export/Import > Export to LIMS .
Elements
The following describes the elements of the dialog.
Label Element type export all samples Radiobutton export only selected samples
Radiobutton
OK
Button
Meaning
Exports all samples in sample memory.
Exports selected samples in sample memory only.
You can only select this radio button if at least one sample is selected.
Starts the export according to the settings.
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Label
Cancel
Element type
Button
Meaning
Aborts the process and discards settings not yet saved.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Exporting LIMS data
Laboratory information and management system (LIMS)
LIMS export settings
Conditions for operating the LIMS.
LIMS settings
Export peak graphics (Dialog)
Function
In this dialog you can define settings for exporting graphic data. For each sample for which a graphic shall be exported a text file will be created. The names of these files have the following format: buchigraph.xxx
, where xxx represents the serial number of the corresponding sample (e.g. "buchigraph.001" for sample no. 1 etc.). If a file with the same name already exists, the content of this file will be overwritten with the new graphic information.
Open
Open the dialog by selecting
File > Export/Import > Export graphics
.
Elements
The following describes the elements of the dialog.
Label Element type export all samples Radiobutton export only selected samples
Directory
...
OK
Cancel
Radiobutton
Textbox
Button
Button
Button
Meaning
The graphic data of all samples listed in the sample view will be exported. For each sample a new file will be generated.
The graphic data of the samples marked in the sample view will be exported. For each sample a new file will be generated.
Defines the name of the directory where the graphic files shall be filed.
Allows the selection of the directory via the dialog "Browse for folder".
Starts the export according to the settings.
Aborts the process and discards settings not yet saved.
Configure report (Dialog)
Function
In this dialog you can define up to three headers to appear on every page of the log printout and the type of printout.
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Open
Open the dialog via:
Menu command
File > Print
Button Hot key
CTRL + P
File > Report configuration
File > Print preview
--- ---
CTRL + S
File > Report configuration --- ---
Elements
The following describes the elements of the dialog.
In section "Title":
Label
Line 1
Line 2
Line 3
Element type
Textbox
Textbox
Textbox
Meaning
Field to input a header.
Field to input a header.
Field to input a header.
In section "Report options":
Label Element type
Print parameters Checkbox
Print coefficients
Print tagged samples only
Print colors
Print selected columns only
---
Checkbox
Checkbox
Checkbox
Checkbox
Dropdown listbox
Meaning
The analysis log is preceded by a list of the currently valid parameters.
The analysis log is preceded by a list of the currently valid calibration coefficients.
Only samples that are highlighted in the text field will be printed.
The printout is in color.
If you are using a black/white printer and the gray values corresponding to the colors are unsatisfactory, do not check this box.
By activating this option, only columns are printed which were selected in the dialog "Select print columns".
This allows the selection which screen shall be printed: text, graphics, statistics, calibration. This option is not accessible if the dialog was invoked via File > Report configuration
.
Remaining elements:
Label
OK
Cancel
Element type
Button
Button
Meaning
Saves new settings
Discards settings not yet saved.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Data backup and printing
Configure report
Display print preview
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Optimizing data evaluation
Print (Dialog)
Function
In this dialog you can define print settings. The appearance of this dialog depends on the type of printer installed / activated. It is usually used to define the following:
the number of copies to print,
the print format, and
print quality.
Open
Open the dialog via:
Menu command
File > Print
Button Hot key
CTRL + P
First the "Configure report" dialog is displayed, in which you can select the headers and type of printing, before the "Print" dialog is displayed.
Elements
The following describes the elements of the dialog.
In section "Printer":
Label
Name
Properties
Status
Type
Location
Comment
Print to file
Element type
Dropdown listbox
Button
Label
Label
Label
Label
Checkbox
Meaning
Field displaying a list of printers connected to the computer.
Opens a dialog in which you can define the properties of the printer selected on the left in the "Name" field.
Displays the status of the selected printer.
Displays the type of the selected printer.
Displays the location of the selected printer.
Displays a comment on the printer.
The print output is sent to a file instead of to a printer.
Note:
Use the Windows control panel to install printers and configure printer connections.
In section "Print range":
Label
All
Element type
Radiobutton
Pages from ... to Radiobutton
Selection Radiobutton
Meaning
Prints all pages.
Prints a certain range. You can define the start and end pages in the textbox next to this button.
Prints the selection only.
In section "Copies":
Label Element type Meaning
Number of copies Textbox with buttons Field to input the number of copies to print.
Sort Checkbox Prints multiple complete copies of a document successively.
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Remaining elements:
Label
OK
Cancel
Element type
Button
Button
Meaning
Starts the printing process according to the settings.
Discards settings not yet saved.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Data backup and printing
Configure report
Display print preview
Optimizing data evaluation
Print preview (Dialog)
Function
This dialog displays the active document as it will print out.
Open
Open the dialog via:
Menu command
File > Print preview
Button Hot key
---
First the "Configure report" dialog is displayed, in which you can select the headers and type of printing, before the "Print preview" dialog is displayed.
Elements
The following describes the elements of the dialog.
Label
Next
Previous
Element type
Button
Button
Button
Button One Pages/Two
Pages
Zoom in
Zoom out
Close
Button
Button
Button
Meaning
Opens the "Print" dialog in which you can start a print job.
Displays the next page to print.
Displays the previous page to print.
Determines whether you want one or two pages to be visible.
Zooms in on the page.
Zooms out of the page.
Closes the dialog.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Display print preview
Optimizing data evaluation
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Printer setup (Dialog)
265
Function
In this dialog you can specify the printer and its connection. The appearance of this dialog depends on the type of printer installed / activated.
Open
Open the dialog by selecting
File > Printer Setup
.
Elements
The following describes the elements of the dialog.
In section "Printer":
Label
Name
Properties
Status
Type
Location
Comment
Element type
Dropdown listbox
Button
Label
Label
Label
Label
Meaning
Field displaying a list of printers connected to the computer.
Opens a dialog in which you can define the properties of the printer selected on the left in the "Name" field.
Displays the status of the selected printer.
Displays the type of the selected printer.
Displays the location of the selected printer.
Displays a comment on the printer.
Note:
Use the Windows control panel to install printers and configure printer connections.
In section "Paper":
Label
Size
Source
Element type
Dropdown listbox
Dropdown listbox
Meaning
Field in which you can select the size of the paper to print on.
Field to select the paper tray.
In section "Alignment":
Label
Portrait
Element type
Radiobutton
Landscape format Radiobutton
Remaining elements:
Label
Network
OK
Cancel
Element type
Button
Button
Button
Meaning
The page is in portrait format.
The page is in landscape format.
Meaning
Connects to a shared network.
Saves new settings
Discards settings not yet saved.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Printer setup
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Open (Dialog)
266
Function
In this dialog you can specify the following for the file to import:
Directory containing the file to import,
File name of the import file,
File type of the import file.
Note
You can only import files:
created with the operating software via File > Export/Import > Export .
generated by the "Balance" weighing data capture program.
Imported data are stored in sample memory. When you import weighing data (Balance files), the data can be deposited in sample memory in different ways.
Open
Open the dialog by selecting File > Export/Import > Import .
Elements
The following describes the elements of the dialog.
Label
Search in
---
File name
File type
Open
Cancel
Element type
Dropdown listbox
Listbox
Textbox/label
Dropdown listbox
Button
Button
Meaning
In this field you can select the directory containing the import file.
This field displays files in the selected directory that match the specified file type.
If you have selected a file in the listbox above, the name of the selected file is displayed here. You can still edit this name.
In this field you can select the file type of the document to import.
MS Excel format (export without graphical information)
MS Access format (export with graphical information)
Balance format (weighing data)
Imports the file according to the settings.
Aborts the process.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Importing documents
Administrative work on the database
Overview of export and import file formats.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Load balance file (Dialog)
267
Function
Open
Open the dialog by selecting
File > Export/Import > Import
. First the "Open" dialog is displayed in which you can select and open the weighing data. Then the "Import balance file" dialog is displayed.
Elements
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Importing documents
Configure backup (Dialog)
Function
The following describes the elements of the dialog.
Label
Append samples as from the current weighed sample
Create new document
OK
Cancel
Element type
Radiobutton
Radiobutton
Button
Button
Meaning
Appends the weighing data after the current weighed sample in the open document.
Creates a new document and inserts the weighing data.
Inserts the weighing data in the selected document.
Aborts the process.
In this dialog you can define settings for creating backups of the database. Backup copies the complete existing database file to a certain directory under a different name, thereby "capturing" a certain state.
In this dialog you specify
what directory to save the backup file to,
how many backup files to keep at the same time,
when the backup starts.
Open
In this dialog you can select whether to insert the weighing data to be imported in an open document or in a new empty document.
Open the dialog by selecting
File > Backup/Restore > Backup
.
Elements
The following describes the elements of the dialog.
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In section "Backup":
Label
Select
---
Keep max. last n backup files
Element type
Button
Label
Meaning
Opens the "Find directory" dialog in which you can select the directory to save to.
The operating software must have write access to the directory in order to be able to save the backup correctly.
Field displaying the selected directory.
Textbox with buttons Field to input the number of backup files to keep at the same time.
If you input 7, for example, and if the backup is performed once a day, you can track the database file back in intervals of one day up to one week. However, avoid keeping too many backup files for reasons of memory. If the number of backup files already equals the maximum number, the oldest file is deleted when you create a new backup copy.
In section "Start backup":
Label
Never
Daily
Element type
Radiobutton
Radiobutton
Every
Once
Radiobutton
Radiobutton
Meaning
The backup is never started automatically.
The backup is started automatically once a day. You can set the time in the textbox next to the button.
The backup is started automatically several times a day.
In the textboxes next to the button you can specify the intervals in minutes, hours or days.
In the following textboxes you can set the date and time as of when to start backing up several times a day.
Too frequent backups can disrupt the analysis and the operating software once the database file has reached a certain size.
The backup is started automatically once. In the textboxes next to the button you can define the date and time to start the backup.
Starts manually the backup immediately. Backup now Button
Remaining elements:
Label
Next backup
Element type
Label
OK
Cancel
Button
Button
Meaning
Field displaying when the next backup will start according to the settings.
Saves new settings
Discards settings not yet saved.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Backup der Datenbank starten
Administrative work on the database
Database backup.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Clean database (Dialog)
Function
269
In the dialog:
the user is warned about reorganizing the database without backing up first.
you can start a backup,
you can start reorganizing the database.
Caution
Data loss!
Reorganizing the database irrevocably deletes all sample data and the contents of the database logbook.
Always backup your data before reorganizing the database.
What does "Clean" mean?
The size of the database is limited to 2 gigabytes, so it is necessary to reorganize the database from time to time. The software displays a warning if the size of the database exceeds 1 gigabyte or if available disk space is less than 1 gigabyte.
Reorganization removes all sample data and the contents of the logbook from the database file, but retains the other data such as settings, coefficients, etc.
Open
Open the dialog by selecting
File > Backup/Restore > Clean
.
Elements
The following describes the elements of the dialog.
Label
Backup now
Reorganize
Cancel
Element type
Button
Button
Button
Meaning
Opens the "File save as" dialog in which you can save the database.
Starts reorganization of the database. The button is only enabled if you have previously created a backup.
Aborts the process.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Reorganize database
Database
Administrative work on the database
Restore database (Dialog)
Function
In the dialog:
the user is warned that importing an old database file irrevocably deletes all the current data,
you can start a backup of the current database file before importing the old database file,
you can reimport an old database file.
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Caution
Data loss!
Restoring the database via
Restore
irrevocably overwrites all sample data, the contents of the logbook and the database configfuration parameters.
Always backup your data before restoring the database via
Restore
.
Open
Open the dialog by selecting
File > Backup/Restore > Restore
.
Elements
The following describes the elements of the dialog.
Label
Backup now
Restore
Cancel
Element type
Button
Button
Button
Meaning
Opens the "Save file as" dialog in which you can backup the current database file under any name.
Opens the "Open file" dialog in which you can select an old database file to reimport. The button is only enabled if you have previously created a backup.
Aborts the process.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Reloading an old database file
Administrative work on the database
Log in as (Dialog)
Function
This dialog is used to input user data.
Open
Open the dialog:
automatically when you start the operating software or
automatically if the operating software is already running and you have not input any data for a long time or
automatically if you call a menu command which requires a higher access permisson than the current one or
via
File > User logon
if another user shall take over the operation of the system.
Elements
The following describes the elements of the dialog.
Label
User
Password
Domain
OK
Element type
Textbox
Textbox
Textbox
Button
Meaning
Field to input the user name.
Field to input the password.
Field to input the domain for company networks.
Launches the operating software or applies the changed user data if the operating software is already running.
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Label
Cancel
Element type
Button
Meaning
Aborts the process or discards the new user data if the operating software is already running.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Starting the operating software
User administration.
File > Logoff (Command)
What is the command used for?
The current user will be logged off. This allows a log-on of a different user while the program is running. The logon dialog appears in which the log-on of a different user can be performed.
File > Exit (Command)
What is the command used for?
This command closes the operating software. If a document is open, the program prompts the user to save it.
Short cuts
Invocation via the Windows symbol:
Invocation via hot key: ALT + F4
File > Export/Import > Create Excel sheet (Command)
What is the command used for?
This command saves the content of the sample view to an Excel file.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Edit menu
Purpose
This section describes commands and dialogs for this menu.
In this section
272
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Edit > Undo (Command)
What is the command used for?
This command undoes a previous action.
Short cuts
Invocation via the toolbar:
Invocation via hot key: CTRL + Z
Note
You can undo up to five previous actions. You can no longer undo an action if you have loaded a document or if the analysis system has received data during an analysis run in the meantime.
The undo function only applies to actions immediately connected with editing sample data.
Edit > Redo (Command)
What is the command used for?
This command restores an action that you have previously undone.
Short cuts
273
Invocation via the toolbar:
Invocation via hot key: CTRL + Y
Edit > Cut (Command)
What is the command used for?
This command removes selected cells and copies them to the clipboard.
Short cuts
Invocation via hot key: CTRL + X
Note
You cannot execute this command if no data are selected.
Cutting and copying data to the clipboard overwrites the data previously stored in the clipboard.
Edit > Copy (Command)
What is the command used for?
This command copies selected cells and/or selected rows to the clipboard.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Short cuts
Invocation via the toolbar:
Invocation via hot key: CTRL + C
Note
You cannot execute this command if no data are selected.
Copying data to the clipboard replaces the data previously stored in the clipboard.
Edit > Paste (Command)
What is the command used for?
This command inserts a copy of the clipboard contents at the cursor position.
Short cuts
Invocation via the toolbar:
Invocation via hot key: CTRL + V
Note
This command is not available if the clipboard is empty.
Edit > Insert line (Command)
What is the command used for?
This command inserts a line at a certain position in sample memory.
Short cuts
Invocation via the toolbar:
Note
The line at which to insert the new line must be selected. Executing this command inserts the new line at the desired position.
The inserted line is an "empty" line, i.e. every column is filled with its default value.
Edit > Delete line (Command)
What is the command used for?
This command deletes a line at a certain position in sample memory.
274
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Short cuts
275
Invocation via the toolbar:
Note
The line to delete must be selected. Executing this command deletes the line and all subsequent lines move up one line.
Swap samples (Dialog)
Function
In this dialog you can swap unprocessed samples in sample memory, e.g. if you want to prioritze urgent samples.
Note
The samples are only swapped in sample memory. After displaying the dialog, you must swap the appropriate samples on the carousel by hand.
Open
Open the dialog by selecting
Edit > Swap
.
Elements
The following describes the elements of the dialog.
Label
Swap sample No. with sample No.
OK
Cancel
Element type
Textbox
Textbox
Button
Button
Meaning
Field to input the number of the sample to swap.
Field to input the number of the sample to swap.
Swaps samples in sample memory.
If the input is incorrect, i.e. if you specify samples that are already finished, you can quit the dialog by clicking
OK
.
Aborts the process.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Prioritizing urgent samples
Optimizing sample data editing
Edit > Modify (Command)
What is the command used for?
This command allows you to edit a finished (analyzed) sample.
Note
The field you want to change must be selected. After executing this command you can edit the contents of the field.
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If 21 CFR Part 11 functionality is enabled, a new version of the document is created the next time it is saved.
Set stop tag (Dialog)
Function
In this dialog you can specify the sample at which to set the stop marker. Usually, the program automatically moves the stop marker while you input sample data. Therefore it is only necessary to move the stop marker manually in special cases.
Open
Open the dialog:
via the menu command
Edit > Stop tag
or
by clicking the right mouse key to the corresponding sample cell. Select
Set stop tag...
from the popping-up context menu.
Elements
The following describes the elements of the dialog.
Label
Stop marker at:
OK
Cancel
Element type
Textbox with buttons
Button
Button
Meaning
Field to input the sample number at which to set the stop marker.
You can also set the sample number in the textbox using the arrows.
Saves the setting.
Aborts the process.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Stopping continuous analysis
Right mouse button function
Select current sample (Dialog)
Function
You set the number of the current sample in the dialog. The current sample is the sample that is currently being analyzed (analysis mode) or that will be analyzed next (idle mode). It is only necessary to set the current sample after breakdowns (power failure, etc.), for example if the carousel position no longer matches the serial sample number.
Note
The current sample is only set in sample memory. Therefore, it is necessary to check that the data of the current sample in sample memory match the data of the sample on the carousel that will actually be analyzed next. Otherwise, measurements will be incorrect.
Open
Open the dialog:
via the menu command
Edit > Current sample
or
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by clicking the right mouse key to the corresponding sample cell. Select
Set current sample...
from the popping-up context menu.
Elements
The following describes the elements of the dialog.
Label
Current sample at:
OK
Cancel
Element type
Textbox with buttons
Button
Button
Meaning
Field to input a sample number
You can also set the sample number in the textbox using the arrows.
Saves the setting.
Aborts the process.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Reacting to a power failure
Right mouse button function
Set current weighed sample (Dialog)
Function
You set the number of the current weighed sample in the dialog. The current weighed sample is the sample that receives a weighing value next. It is only necessary to set the current weighed sample after breakdowns, for example if you lose a sample already when you put it on the carousel and therefore need to weigh in another sample.
Open
Open the dialog:
via the menu command
Edit > Current weight
or
by clicking the right mouse key to the corresponding sample cell. Select
Set current weight...
from the popping-up context menu.
Elements
The following describes the elements of the dialog.
Label
Current weighed sample at:
OK
Cancel
Element type
Textbox with buttons
Button
Button
Meaning
Field to input a sample number
You can also set the sample number in the textbox using the arrows.
Saves the setting.
Aborts the process.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
View menu
Purpose
This section describes commands and dialogs for this menu.
In this section
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View > Toggle (Command)
What is the command used for?
This command changes the field in the combi view.
Note
Execute this command several times to switch to the desired view. The sequence is: Calibration view
- progression graph - statistics view - calibration view, etc.
Also by clicking on the caption bar of the combi view you can change to the reqested view.
Zoom in/out (Dialog)
Function
In this dialog you can zoom in/out details of the graphical progression of an analysis or the calibration graph.
Open
Open the dialog via:
Menu command
View > Zoom in/out
Button Hot key
---
Elements
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Setting the size of the graph
Configure sample view (Dialog)
Function
The following describes the elements of the dialog.
Label
Zoom factor
OK
Cancel
Element type
Dropdown listbox
Button
Button
Meaning
Field to select the zoom factor. You can choose between zoom factors of 1; 2, 5; 10; 20; 50 and 100. At factor > 1 the graph view is enclosed by scrollbars so that you can select a specific area.
Zoom in/out of the graph.
Aborts the process.
This dialog is used to configure the sample view. It is possible to show/hide every column and to change the display sequence.
Open
Open the dialog via View > Gridview > Configure.
The sample view must be active in order to open the dialog.
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Elements
280
The following describes the elements of the dialog.
Label
Display column
Hide column
^
<<<
>>> v
Reset
OK
Cancel
Element type Meaning
Label
Label
Button
Button
Button
Button
Button
Button
Button
All sample data listed in this column are displayed.
All sample data listed in this column are not displayed.
Changes the display sequence of the sample data.
Moves selected samples one position to the left in the sample view (text view).
Moves the sample data from the "Hide" section into the
"Display" section.
Moves the sample data from the "Display" section into the "Hide" section.
Changes the display sequence of the sample data.
Moves selected samples one position to the right in the sample view (text view).
Shows all columns and resets the display sequence to the default setting.
Saves new settings
Discards settings not yet saved.
Number of decimal places
You can specify the number of decimal places used in columns in the "Column properties" dialog.
Open this dialog from the "Configure sample pane" dialog with the aid of the context menu. See
Column properties.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Specifying the number of decimal places
Configuring the sample pane
Save sample pane (Dialog)
Function
In this dialog you can save the current sample view that the user has configured according to his own requirements.
Open
Open the dialog via
View > Sample pane > Save configuration
. The sample pane must be active in order to open the dialog.
Elements
The following describes the elements of the dialog.
Label
---
Element type
Textbox/label
Meaning
Field to input a name under which to save the view.
If you have selected a file in the listbox, the name of the file is displayed here and you can overwrite the file.
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Label
---
OK
Cancel
Element type
Listbox
Button
Button
Meaning
Field listing the saved views.
Saves the view under the selected name.
Aborts the process.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Saving the sample view
Optimizing data evaluation
Load sample pane (Dialog)
Function
In this dialog you can reload saved sample views. However, you can only load a view if the view was saved in the same operating mode as the current mode in which the analyzer is running.
Open
Open the dialog via
View > Gridview > Load configuration
.
Elements
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Loading a sample view
Delete sample pane (Dialog)
Function
The following describes the elements of the dialog.
Label
---
---
Load
Cancel
Element type
Textbox/label
Listbox
Button
Button
Meaning
Field displaying the name of the selected view.
Field listing the available views.
Loads the selected view.
Aborts the process.
In this dialog you can delete saved sample views.
Open
Open the dialog via
View > Gridview > Delete configuration
. The sample pane must be active in order to open the dialog.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Elements
The following describes the elements of the dialog.
Label
---
---
Delete
Cancel
Element type
Textbox/label
Listbox
Button
Button
Meaning
Field displaying the name of the selected view.
Field listing the available views.
Deletes the selected view.
Aborts the process.
View > Gridview > Auto align (Command)
282
What is the command used for?
This command optimizes the sample view:
The individual columns are automatically widened or narrowed to make the headers and entries completely visible.
Configure graph view (Dialog)
Function
In this dialog you can define the appearance of the graph view.
Open
Open the dialog via
View > Graphic > Configure
. Progression view (graph view) must be enabled in order to open the dialog.
Elements
The following describes the elements of the dialog.
In section "Y axis configuration":
Label
{Graph type}
Element type
Checkbox
Meaning
Displays the appropriate progression graph. You can set the scale range of the progression graph in the adjacent textbox.
Note:
The number of progression graphs you can display at the same time is limited to four for the sake of clarity.
In section "Zero line":
Label
At height
Element type Meaning
Textbox with buttons In this field you specify which of the horizontal grid lines in the graph view is assumed to be the zero line. A value of 0 means that the zero line is at the bottom edge of the graph view.
In section "X axis configuration":
Label
Time axis
Element type
Textbox
Meaning
In this field you can define the division of the time axis (X axis).
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Remaining elements:
Label
During analysis run display current sample only
OK
Cancel
Element type
Checkbox
Button
Button
Meaning
During an ongoing analysis you cannot view a progression graph of a previously analyzed sample.
Saves new settings
Discards settings not yet saved.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Data backup and printing
Configuring the graph view
Right mouse button function
View > Graphic > Auto align (Command)
What is the command used for?
This command optimizes the graph view:
The graph is scaled so that it is completely visible.
Configure statistics view (Dialog)
Function
In this dialog you can define the appearance of the statistics view.
Open
Open the dialog via View > Statistic > Configure . The statistics view must be active in order to open the dialog.
Elements
The following describes the elements of the dialog.
In section "Show":
Label
{Element name}
Element type
Checkbox
Meaning
Only display statistical data for the corresponding element if this box is checked.
In section "show/hide":
Label
Std. dev. absolute
Element type
Checkbox
Std. dev. relative
Delta
Checkbox
Checkbox
Meaning
Only displays absolute standard deviation of the individual groups if this box is checked.
Only displays relative standard deviation of the individual groups if this box is checked.
Only displays the delta value of the individual groups if this box is checked.
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Note:
The percentage contents and the computed mean value are always displayed and cannot be hidden.
Remaining elements:
Label
OK
Cancel
Element type
Button
Button
Meaning
Saves new settings
Discards settings not yet saved.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Configure statistics view
Right mouse button function
View > Statistic > Auto align (Command)
What is the command used for?
This command optimizes the statistics view:
The individual columns are automatically widened or narrowed to make the headers and entries completely visible.
Select columns (Dialog)
Function
The dialog allows selection of the elements for the enhanced display of the sample analyzed most recently.
Open
Open the dialog via
View > Recent sample
.
Elements
The following describes the elements of the dialog.
Label
{Column name}
Element type
Checkbox
Meaning
Displays the corresponding column only if this box is checked.
Remaining elements:
Label
OK
Cancel
Element type
Button
Button
Meaning
Saves new settings
Discards settings not yet saved.
Column properties (Dialog)
Function
In this dialog you specify the number of decimal places.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Open
285
Proceed as follows:
Activate the sample view.
Open the "Configure sample pane" dialog in the operating software by selecting View > Sample pane > Configure
.
Select the column in the "Show" section whose decimal places you want to set and click the right mouse button.
Open the "Column properties" dialog by selecting the
Properties...
menu item.
Elements
The following describes the elements of the dialog.
Label
Column
Decimal places
OK
Cancel
Element type
Label
Textbox
Button
Button
Meaning
This field displays the column for which to set the number of decimal places.
Field to input the desired number of decimal places. 0 to 7 decimal places are possible.
Saves new settings
Discards settings not yet saved.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Specifying the number of decimal places
Right mouse button function
Configuring the sample pane
Weighing window (Dialog)
Function
The dialog displays the last five sample weights input and the names of the associated samples. The current weighed sample is displayed in a larger font. The weight window makes it easier for you to check whether the values were correctly transferred, particularly when automatically transferring weighing data.
Open
Open or close the dialog by selecting
View > Weight window
.
Elements
The following describes the elements of the dialog.
Label
No.
Wt. [mg]
Name
Element type
Label
Label
Label
Meaning
Displays the number of the weighed-in sample. The number of the current weighed sample is displayed in a larger font.
Displays the weight of the weighed-in sample. The weight of the current weighted sample is displayed in a larger font.
Displays the name of the weighed-in sample. The name of the current weighed sample is displayed in a larger font.
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Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
System menu
Purpose
This section describes commands and dialogs for this menu.
In this section
287
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10 - Menu and dialog descriptions
System > Auto run (Command)
What is the command used for?
This command starts continuous analysis, i.e. the system processes all samples in sample memory up to the stop marker. Once the system reaches the stop marker, it either goes into idle mode or sleep mode, depending on settings.
Short cuts
288
Invocation via the toolbar:
Note
You can only start the system if the following system conditions exist:
System pressure is at least 800 mbar.
Furnace temperatures are at most 50 °C below their setpoints.
The system has detected that the base line is stable.
Working temperature of the thermal conductivity detector is at least 59 °C.
If one of these conditions is not met, the system does not start and a message is displayed.
System > Single run (Command)
What is the command used for?
This command starts a single analysis, i.e. the next sample in sample memory (= current sample) is processed. After processing the single sample, the system goes into idle mode again, regardless of sleep settings.
Short cuts
Invocation via the toolbar:
Note
If you execute this command while continuous analysis is running, continuous analysis stops after finishing the current sample and the system goes into idle mode.
You can only start the system if the following system conditions exist:
System pressure is at least 800 mbar.
Furnace temperatures are at most 50 °C below their setpoints.
The system has detected that the base line is stable.
Working temperature of the thermal conductivity detector is at least 59 °C.
If one of these conditions is not met, the system does not start and a message is displayed.
System > Stop (Command)
What is the command used for?
This command aborts a running analysis. The system goes into idle mode again, regardless of sleep settings.
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Note
The "Abort analysis" dialog appears.
Observe the notes listed therein. Abort analysis only if either the sample has not been thrown in yet or has been already completely combusted. In the latter case, make sure that the column does not retain any element components, i.e. the desorption procedure has been completed. Otherwise, an abortion leads to system contaminations combined with significant damages.
To abort a running analysis, you have to confirm the note displayed in the dialog first. Only after the confirmation the
Abort analysis
button becomes accessible, thus allowing the abortion.
System > Auto zero (Command)
What is the command used for?
This command causes to set the current output values of the dectors to zero. The purpose is to reset the signals to zero if they have drifted over time.
Furnace switch off/on (Dialog)
Function
In this dialog the furnace will be switched off and on.
Open
Open the dialog via
System > Furnace
.
Elements
The following describes the elements of the dialog.
Label
Yes
No
Element type
Button
Button
Meaning
Confirm the action.
Aborts the process.
Initialize the instrument (Dialog)
Function
In this dialog the instrument will be initialized. It will be set all parameters to default values.
Open
Open the dialog via
System > Initialise
.
Elements
The following describes the elements of the dialog.
Label
Yes
No
Element type
Button
Button
Meaning
Confirm the action.
Aborts the process.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
System > Wake up (Command)
What is the command used for?
This command wakes up the "sleeping" system. The carrier gas is reactivated and the furnaces are heated back up to their working temperatures. This command is used to manually wake up the system if you need to start up the system prematurely, i.e. earlier than the chosen wake-up time.
Short cuts
290
Invocation via the toolbar:
Note
If you have defined a wake-up time that is in the past, you must wake up the sleeping system again with this command.
Feeding (Dialog)
Function
In this dialog you specify the size of the sample carousel. Make sure that the setting here matches to the actual size of the sample carousel.
Open
Open the dialog by selecting
System > Feeding
.
Elements
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Stopping continuous analysis
Right mouse button function
Adjust carousel position (Dialog)
Note
The following describes the elements of the dialog.
Label
Carousel with {n} positions
OK
Cancel
Element type
Radiobutton
Button
Button
Meaning
The feeding system is switched to a carousel size of {n} positions.
Saves the setting.
Aborts the process.
This function is only available in the solids modes.
Function
After a power failure or if you repeat initial startup and remove the carousel, it is necessary to readjust the position of the carousel.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
In the dialog:
you are warned about adjusting the carousel position if the carousel contains samples,
you can move the carousel to zero position or any other position.
Please observe the following instruction:
Caution
Inserting multiple samples into the ball valve (only for solid operation)
If there are samples in the carousel while you are changing the position of the carousel via
System > Carousel position
, multiple samples may fall into the ball valve at the same time. In this case, a service technician is required.
Before changing the position of the carousel, always remove all samples from the carousel.
291
Note
Observe the following when adjusting the position of the carousel:
The carousel is moved so that the selected position is above the insertion opening. When the next analysis starts, the carousel moves the next sample position above the insertion opening and drops the sample. Therefore, it makes sense to select the previous position when moving the carousel.
Example: You want to move the carousel so as to analyze the sample at position 26 in the next analysis. Therefore, select position 25. The carousel moves so far that position 25 is above the insertion opening. When the next analysis starts, the carousel moves one position on during the insertion process and thus drops the samples at position 26.
Open
Open the dialog via
System > Sample Position
.
Elements
The following describes the elements of the dialog.
Label
All samples removed from the carousel
Position
Reference run
OK
Cancel
Element type
Checkbox
Radiobutton
Radiobutton
Button
Button
Meaning
If you have removed all samples from the carousel, you must check this box. Otherwise the carousel will not move.
Moves the carousel to the desired position. You can set the position number in the textbox to the right. You must input the desired position number minus 1.
The carousel performs reference run, i.e. the carousel first moves to a defined reference position and then to position
0 which has almost the same location.
Adjusts the position of the carousel, if confirmed above that all samples have been removed from the carousel.
Aborts the process.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Performing measurement work
Reacting to a power failure
Performing calibration.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Math menu
Purpose
This section describes commands and dialogs for this menu.
In this section
292
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Math > Blank values > Calculate (Command)
What is the command used for?
This command starts a calculation of blank values. The results are entered in the appropriate columns in text view.
Note
Blank value calculation is only performed if sample memory contains blank samples.
Blank values (Dialog)
Function
The function of this dialog differs depending on how you open it:
If it is opened via
Math > Blank Value > Input
, the dialog displays and allows you to edit the blank values for each element. It is useful to input a blank value manually when the blank value is known. This allows you to dispense with the relatively time-consuming blank value determination.
If it was opened via
Math > Blank Value > Compute
, the dialog displays and allows you to apply the blank values just computed.
Open
Open the dialog either
via
Math > Blank Value > Input
. You can only open the dialog if you have set the "total" blank value calculation method.
or via Math > Blank Value > Calculate . However, blank value determination is only performed if sample memory contains blank samples.
Elements
The following describes the elements of the dialog.
Label
{Element name}
Element type
Textbox/label
Meaning
Field to input the blank value of the corresponding element.
(
Math > Blank Value > Input
)
Field displaying the computed blank value of the corresponding element.
(
Math > Blank Value > Compute
)
Remaining elements:
Label
OK
Cancel
Element type
Button
Button
Meaning
Saves new settings
Discards settings not yet saved.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Determining blank values
Specifying the computation method for blank value and daily factor
Performing routine measuring work
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Routine measuring work
Types of blank value determination and their settings
Formulae for blank value determination and compensation
Math. > Factor (Command)
What is the command used for?
This command computes the daily factor of a series of analyses.
Define type of peak (Dialog)
Function
In this dialog the behavior of the manual peak integration will be defined.
Open
Open the dialog by selecting
Math. > Manual Peak Integration > Type
. The dialog can only be opened when the graphic view is activated and display is set to a single detector signal.
Elements
The following describes the elements of the dialog.
Label single peak
Element type
Radiobutton
Superimposed peak Radiobutton straight baseline
OK
Cancel
Checkbox
Button
Button
Meaning
Sets the behavior in such a way that single peaks can be edited in the manual integration process. An integration process is executed by setting a start and end tag each.
Sets the behavior in such a way that superimposed peaks can be edited in the manual integration process. An integration process is executed by setting a start and end tag each for the socket and the "superimposed" peak.
If activated, a baseline is used which runs parallel to the xaxis (time axis).
If deactivated, a baseline is used which start height is at the start tag and which end height is at the end tag.
Saves the new settings.
Discards settings not yet saved.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Manual peak integration
Define peak start / end (Dialog)
Function
The dialog serves for the definition of the peak start and end tags and the height of the baseline during the manual peak integration.
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The dialog
The appearance of the dialog depends on the selected peak type.
Open
Open the dialog by selecting
Math. > Manual Peak Integration > Integrate
.
Elements
The following describes the elements of the dialog.
Label Element type
Button
and/or
and/or
Button
Button
Button
Meaning
Allows the setting of the start tag of the single and/or total peak.
Allows the setting of the end tag of the single and/or total peak.
Allows the vertical movement of the baseline. This button is only accessible if the option "straight baseline" is activated.
Allows the setting of the start tag of the superimposed peak.
Allows the setting of the end tag of the superimposed peak. Button
Assignment
Close
Button
Button
Button
Allows the setting of an intermediate point for a better adjustment to the socket course.
Allows the assignment of the manually integrated peak areas to one element component.
Closes the dialog.
Clicking a symbol button results in an activation of the corresponding function. Reclicking the same symbol button deactivates the function. Clicking a different symbol button results in its acitvation as well as in the deacitivation of the previously activated function. Which function is currently activated can be seen from the green bar above the corresponding symbol button.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Manual peak integration
Area assignment (Dialog)
Function
In the dialog it is defined to which element the manually integrated peak area(s) shall be assigned.
The dialog
The appearance of the dialog depends on the selected peak type.
Open
Open the "Define peak start/end" dialog via
Math. > Manual Peak Integration > Integrate
. Then, after you have performed the manual integration, open the "Area assignment" dialog by clicking the
Assign button.
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Elements
The following describes the elements of the dialog.
Label
Total
Element type
Radiobutton
"Superimposed" peak Radiobutton
Socket
{Element name}
OK
Cancel
Radiobutton
Option fields
Button
Button
Meaning
Defines that the total area shall be used for the assignment.
Defines that the area of the superimposed peak (ligh red color) shall be used for the assignment. (Not available for single peak integration)
Defines that the area of the socket (light blue color) shall be used for the assignment. The area value of the socket is the difference between the total area and the area of the superimposed peak. (Not available for single peak integration)
Define the element to which the selected peak area shall be assigned. The number of option fields and their labeling depend on the set analysis mode.
Executes the assignment and closes the dialog. After the assignment the assigned area and the resulting new element content are displayed in the sample view.
Closes the dialog without assignment.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Manual peak integration
Standard samples display (Dialog)
Function
In this dialog, you select how the standard samples are displayed in the sample field.
Open
Open the dialog via
Math > Standard samples
.
Elements
The following describes the elements of the dialog.
Label
Show as standard sample
(theoretical concentration)
Show as factor/monitor sample (measured concentration)
OK
Cancel
Element type
Radiobutton
Radiobutton
Button
Button
Meaning
The sample field displays the theoretical element concentrations of the standard samples in the corresponding columns.
The sample field displays the measured (calculated) element concentrations of the standard samples in the corresponding columns.
Saves new settings
Discards settings not yet saved.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Math. > Recalculate (Command)
297
What is the command used for?
This command recomputes the results of all samples in sample memory.
This makes sense, for example, if you have analyzed a calibration series and then a measuring series immediately afterwards (e.g. overnight). If you compute the coefficients the next day, you must recompute the appended measuring samples with the newly computed coefficients.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Statistics menu
Purpose
This section describes commands and dialogs for this menu.
In this section
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10 - Menu and dialog descriptions
Statistics > Via names (Command)
What is the command used for?
This command combines samples of the same sample name into a statistical group. The statistical groups are then displayed in the combi view statistics view together with the appropriate results.
Statistics > Group (Command)
What is the command used for?
This command combines two or more selected samples into a statistical group.
Short cuts
299
Invocation via the toolbar:
Note
This command is only available if at least two samples are selected. When you execute this command, the statitsical group and its results are displayed in the combi view statistics view.
Statistics > Sort group (Command)
What is the command used for?
This command sorts statistical groups so that the groups are listed in ascending order, starting from the serial number of the first member of the group.
Note
The command is only available if the statistics view is active.
Statistics > Delete group (Command)
What is the command used for?
This command deletes a selected statistical group in the statistics view.
Note
The command is only available if the statistics view is active.
Statistics > Clear statistic (Command)
What is the command used for?
This command deletes the entire statistics memory.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Statistics > Include/Exclude sample (Command)
What is the command used for?
This command either includes a sample in the calculation or excludes it.
Short cuts
300
Invocation via the toolbar:
Invocation via hot key: CTRL + T
Note
You can execute this command in the following cases:
In the statistics view: The selected sample of a statistical group is displayed crossed-out
(disabled) and the statistics calculation is performed without this sample. If you execute the command again, the sample is displayed as "enabled" again and the statistical calculation is performed with this sample again. If only two samples are enabled in a statistical group, you cannot disable either of these samples.
In the calibration view: The selected sample of a calibration series is displayed as a full circle
(eliminated) and is excluded from the calibration calculation. Executing this command again displays the sample as "uneliminated" and includes it in the calibration calculation again.
Statistics > Include/Exclude value (Command)
What is the command used for?
This command either includes the value of a sample in the calculation or excludes it.
Note
You can execute this command in the following cases:
In the statistics view: The selected value of a sample of a statistical group is displayed crossedout (disabled) and the statistics calculation is performed without this value. If you execute the command again, the value is displayed as "enabled" again and the statistical calculation is performed with this value again. If only two values are enabled in a statistical group, you cannot disable either of these values.
Statistics > Create Excel sheet (Command)
What is the command used for?
This command saves the content of the statistic field to an Excel file.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Calibration menu
Purpose
This section describes commands and dialogs for this menu.
In this section
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Calibration coefficients (Dialog)
Function
This dialog displays the calibration coefficients on a tab. With suitable permission, you can also manually input the coefficients.
Note the following for manual input
Observe the following when manually inputting calibration coefficients.
Sample memory must be empty, otherwise manual input is not possible.
The program interprets the comma as a decimal separator and the * sign as an exponent. If, for example, you want to input a coefficient of -2.345320e-004, input the following string of characters on the number pad. When the press the tab key, the program automatically converts the string into -2.345320e-004.
If only one calibration coefficient set is displayed an element in the dialog although you want to manually input calibration coefficients for two ranges, you can click the "upper range" checkbox to display the second calibration coefficient set.
Open
Open the dialog via Calibration > Coefficients .
Elements
The following describes the elements of the dialog.
On the respective tab:
Label
Coefficient {x}
Min.
Max. upper range
Date
(Copy)
Element type
Textbox
Textbox
Textbox
Checkbox
Label
Button
Meaning
The respective field displays for the selected coefficients set the corresponding calibration coefficient and allows you to edit it if you have the right permission.
This field displays for the selected coefficients set the lower limit of the work range and allows you to edit it if you have the right permission.
This field displays for the selected coefficients set the upper limit of the work range and allows you to edit it if you have the right permission.
If activated, fields for a second coefficients set are displayed. This allows the definition of a lower and an upper calibration range.
Displays the creation date of the corresponding coefficients set.
Copies the coefficients of the currently active tab to the clipboard.
(Paste)
Button Copies the coefficients from the clipboard to the currently active tab.
Button Undoes the copy action performed recently.
(Undo)
Remaining elements:
Label
OK
Element type
Button
Meaning
Applies calibration coefficients that have just been computed or input.
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Label
Cancel
Element type
Button
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Viewing calibration coefficients
Defining standard substances as calibration samples
Performing calibration.
Background knowledge required for calibration
Configure calibration (Dialog)
Function
Meaning
Discards calibration coefficients that have just been computed or input.
In this dialog you can specify the calibration curve calculation methods. It is not possible to perform the calibration computation without this information.
Open
Open the dialog via
Calibration > Calibrate
. In order to open the dialog, sample memory must contain a sufficient number of valid calibration samples.
Elements
The following describes the elements of the dialog.
On the respective tab:
Label Element type
One calibration range Radiobutton
Polynomial degree
Two calibration ranges
Polynomial degree, lower range
Polynomial degree, upper range
Textbox
Radiobutton
Textbox
Textbox
Meaning
Only one calibration curve is computed over the entire measuring range for the respective element.
Field to input the polynomial degree for the calibration curve calculation over the entire measuring range. May be set from 1 to 4.
For each element, the whole measuring range is divided into an upper and lower calibration range. A separate calibration curve is computed for each calibration range.
Field to input the polynomial degree for the calibration curve calculation in the lower range. May be set from 1 to
4.
Field to input the polynomial degree for the calibration curve calculation in the upper range. May be set from 1 to
4.
Remaining elements:
Label
OK
Cancel
Element type
Button
Button
Meaning
Continues with the calibration calculation. If the option
"Two calibration ranges" has been checked for at least for one element, then the "Specify lower and upper calibration range" dialog will open. Here, the split-up of both calibration ranges can be carried out.
Aborts the process.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Defining standard substances as calibration samples
Background knowledge required for calibration
Calibration formulae
Specify lower and upper calibration range (Dialog)
304
Function
In this dialog you specify for a two-range calibration at what point to divide between the upper and lower calibration range. The dialog displays all samples on the basis of a virtual line. This shows you whether it makes sense to split the ranges with a dividing line.
Open
Open the dialog via
Calibration > Calibrate
. First the "Configure calibration" dialog is displayed in which you specify the calculation methods. Only then the "Specify lower and upper calibration range" dialog is displayed if you have specified a two-range calibration.
Elements
The following describes the elements of the dialog.
Label
<<<
<
>
>>>
Zoom +
Zoom -
Zoom
Dividing line at
OK
Cancel
Element type
Button
Button
Button
Button
Button
Button
Label
Label
Button
Button
Meaning
Moves the dividing line between the upper and lower calibration range to the left in larger intervals.
Moves the dividing line between the upper and lower calibration range to the left in smaller intervals.
Moves the dividing line between the upper and lower calibration range to the right in smaller intervals.
Moves the dividing line between the upper and lower calibration range to the right in larger intervals.
Increases the scale of the view.
Decreases the scale of the view.
Displays the current zoom setting.
Displays in figures where the dividing line is currently set between the upper and lower calibration range.
Saves new settings
Aborts the process.
Note:
The dividing line can also be set directly: To do so, place the mouse cursor at the point where you want to place the dividing line and then click the right mouse button.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Performing calibration.
Background knowledge required for calibration
Right mouse button function
Calibration formulae
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Calibration > Next sample (Command)
What is the command used for?
This command moves the sample marker to the next sample in the calibration graph.
Short cuts
Invocation via the toolbar:
Invocation via hot key: CTRL + "+"
Calibration > Previous sample (Command)
What is the command used for?
This command moves the sample marker to the previous sample in the calibration graph.
Short cuts
Invocation via the toolbar:
Invocation via hot key: CTRL + "-"
Calibration > Next (Command)
What is the command used for?
This command displays the next calibration curve in the calibration view or calls up the end of the calibration.
Short cuts
305
Invocation via the toolbar:
Calibration > Previous (Command)
What is the command used for?
This command displays the previous calibration curve in the calibration view or calls up the "Configure calibration" dialog.
Short cuts
Invocation via the toolbar:
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Options menu
Purpose
This section describes commands and dialogs for this menu.
In this section
306
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10 - Menu and dialog descriptions 307
Maintenance intervals (Dialog)
Function
In this dialog, any number of maintenance events can be defined and viewed.
Open
Open the dialog via
Options > Maintenance > Intervals
.
Elements
The following describes the elements of the dialog.
Label
---
Total:
Event: {n}
Interval
Status
Mode assignment
Information only
Information and stop continuous analysis
New
Delete
Save
Close
Element type
Listbox
Label
Textbox/label
Textbox/label
Textbox/label
List box with checkboxes
Radiobutton
Radiobutton
Button
Button
Button
Button
Meaning
In this field the texts of all currently defined events are displayed. Each text has a highlighted bar which displays the urgency of the maintenance:
Green bar: There is still time for maintenance.
Yellow bar: The maintenance must be performed soon.
Red bar: The maintenance is overdue.
Displays the number of all analyses performed so far.
Field to enter the text of a new event. or
The field displays the text of the event selected in the adjacent list box.
Field to input the number of analyzed samples after which the maintenance must be performed. or
The field displays the interval of the event selected in the adjacent list box.
Field to input the number of samples already analyzed, e.g. when you install a used tube. You must enter 0 as the status after performing maintenance. or
This field displays the number of samples already analyzed for the adjacent event.
Allows assignment of the corresponding event to the different analysis modes. Incrementing of the corresponding counter will be suppressed if analysis modes are not checked here.
When a maintenance event falls due, the system only displays a message in the status view. See Defining maintenance intervals in the software.
When a maintenance event falls due, the system displays a message in the status view and continuous analysis is stopped.
Allows the definition of a new event.
Removes the selected event from the list.
Saves the settings made.
Closes the dialog.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Defining maintenance intervals in the software.
Viewing the status of maintenance intervals
Installing used tubes
Maintenance work to be performed by the customer.
Replace part (Dialog)
Function
308
If you need to replace parts of the instrument, it is necessary to take certain precautions on the instrument beforehand. It is necessary to depressurize the analyzer.
Via the dialog:
you can stop gas supply,
reduce pressure,
and the user receives further instructions.
After replacing the part, you can get the instrument ready for operation again via this dialog. I.e. gas supply is reactivated and any atmospheric nitrogen is flushed out with carrier gas.
Safety instruction
Strictly observe the safety instruction "Gas pressure" under
Warning notes during operation
(on
Open
Open the dialog via:
Options > Maintenance > Replace parts
.
Elements
The following describes the elements of the dialog.
Label
Please wait a moment
You can now replace the part. Click "Finish" to continue after replacing.
Done
Element type
Label
Label
Button
Meaning
This field displays an instruction to wait for pressure drop without pressing any buttons until the next instruction is displayed.
If this instruction is displayed in the dialog and the displays "Flow" and "Pressure" show 0 on screen, you may replace the part.
Automatically switches the gas back on after replacing the part.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Installing reaction tubes in the furnace and conditioning.
Preparing and following up maintenance work.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Adjust carousel (Dialog)
Note
This function is only available in the solids modes.
Function
309
After a power failure or if you repeat initial startup and remove the carousel, it is necessary to readjust the position of the carousel.
In the dialog:
you are warned about adjusting the carousel position if the carousel contains samples,
you can move the carousel to zero position or any other position.
Please observe the following instruction:
Caution Inserting multiple samples into the ball valve (only for solid operation)
If there are samples in the carousel while you are changing the position of the carousel via
System > Carousel position
, multiple samples may fall into the ball valve at the same time. In this case, a service technician is required.
Before changing the position of the carousel, always remove all samples from the carousel.
Note
Observe the following when adjusting the position of the carousel:
The carousel is moved so that the selected position is above the insertion opening. When the next analysis starts, the carousel moves the next sample position above the insertion opening and drops the sample. Therefore, it makes sense to select the previous position when moving the carousel.
Example: You want to move the carousel so as to analyze the sample at position 26 in the next analysis. Therefore, select position 25. The carousel moves so far that position 25 is above the insertion opening. When the next analysis starts, the carousel moves one position on during the insertion process and thus drops the samples at position 26.
Open
Open the dialog via Options > Maintenance > Carousel adjustment .
Elements
The following describes the elements of the dialog.
Label
All samples removed from the carousel
Position
Reference run
OK
Cancel
Element type
Checkbox
Radiobutton
Radiobutton
Button
Button
Meaning
If you have removed all samples from the carousel, you must check this box. Otherwise the carousel will not move.
Moves the carousel to the desired position. You can set the position number in the textbox to the right. You must input the desired position number minus 1.
The carousel performs reference run, i.e. the carousel first moves to a defined reference position and then to position
0 which has almost the same location.
Adjusts the position of the carousel, if confirmed above that all samples have been removed from the carousel.
Aborts the process.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Performing measurement work
Reacting to a power failure
Performing calibration.
Leak test (Dialog)
310
Function
This dialog is used to perform a leak test and the leak search:
In the display window the tubing diagram of the analysis system is shown. Depending on the currently performed leak test stage, the appearance of the tubing diagram may vary.
If there are certain tasks to be performed during the leak test, they are displayed in the form of colored numbers in the tubing diagram. By positioning the mouse pointer over these numbers a particular window will pop up showing the task in detail.
Below the diagram there is a field which will show information about the actions to be performed during the certain test stages, e.g. which gas ways have to be closed etc.
At the right edge of the dialog box there are the buttons for selection and/or execution of the certain test stages.
Open
Open the dialog by selecting
Options > Diagnostics > Leak test
. First a dialog is displayed in which you must confirm that you want to perform a leak test. The "Leak test: Complete instrument" dialog is displayed once you confirm.
Elements
The following describes the elements of the dialog.
Label
(Graphic field)
Info field (below the graphic field)
Start
Leak search set
Close
Element type
Label
Label
Button
Button
Button
Meaning
Shows the tubing diagram of the analysis system.
Gives information to the user, which actions have to be performed for the execution of a test stage (e.g. sealing of certain gas ways etc.).
Starts execution of the currently active leak test stage. The
"Test Phases" dialog will open. Here, the test run can be observed.
Opens a dialog in which all components of the leak test kit are displayed.
Closes the dialog. The user will be requested to turn on again the gas supply. Afterwards, a re-initialization of the system takes place.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Performing a leak test.
Installing reaction tubes in the furnace and conditioning.
Preparing and following up maintenance work.
Start-up.
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Reacting to a power failure
Maintenance work to be performed by the customer.
Leak test: Test phases (Dialog)
Function
This dialog displays the current status while performing a leak test.
The left half of the dialog displays the individual stages of the test. The current stage of the test is marked with an arrow.
The right half of the dialog displays the remaining time of the respective stage of the test and system pressure.
The result is displayed at the bottom of the dialog once the test is finished.
Open
Open the dialog by clicking
Start
in the "Leak test" dialog.
Elements
The following describes the elements of the dialog.
In the left area:
Label
Pressure build-up
Stabilization
Test
Element type
Label
Label
Label
Meaning
The valves are switched to positions allowing pressure build-up in a certain section of the system (first stage of the test).
The gas inlet valve is closed. The system waits for a set time to allow stable pressure conditions in the subsequent test stage. If system pressure does not reach a defined minimum pressure after this stage has ended, the leak test is regarded as having failed. If minimum pressure is reached, the system moves on to the next stage.
The initial pressure of the instrument is recorded at the beginning. During this stage of the test, the system constantly compares current pressure with the initial pressure previously measured and calculates the current drop in pressure. If the drop in pressure exceeds a certain threshold during this stage of the test, the leak test is regarded as having failed. If the drop in pressure stays below the threshold, the system moves on to the next stage.
In the right area:
Label
0 ... x Sec.
Pressure, current
Element type
Label
Label
Meaning
This field displays the remaining time of the respective stage of the test.
This field displays instrument pressure.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
In the lower area:
Label
Result
Element type
Label
312
Meaning
This field displays whether the leak test was successful or not. The following symbols highlight the leak test result:
..... Leak test successful.
Cancel
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Performing a leak test.
Installing reaction tubes in the furnace and conditioning.
Preparing and following up maintenance work.
Optimizing instrument condition for calibration.
Start-up.
Reacting to a power failure
Maintenance work to be performed by the customer.
System test (Dialog)
Function
Button
Button
..... Leak test failed.
Prints the result after the leak test finishes.
Aborts the leak test.
In this dialog you can test the system components of the analyzer for proper working order. The dialog contains the following two tabs:
On the "Outputs" tab you can test the valves for proper working order.
On the "Flows" tab you can test the MFCs (Mass Flow Controllers) for proper working order.
On the "Ball valve" tab you can test the ball valve for proper working order.
Open
Open the dialog by selecting
Options > Diagnostics > System Test
.
Elements
The following describes the elements of the dialog.
In section "Outputs":
Label
Ni flap
Oxygen valve
Water drain
Element type
Buttons
Buttons
Buttons
Meaning
0 Opens the Ni flap.
I Closes the Ni flap.
0 removes the current from the valve.
I applies current to the valve.
0 removes the current from the valve.
I applies current to the valve.
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Label
CO2 inlet
Fan
Leak test
Oven transformer
Element type
Buttons
Buttons
Buttons
Buttons
Meaning
0 removes the current from the valve.
I applies current to the valve.
0 removes the current from the valve.
I applies current to the valve.
0 removes the current from the valve.
I applies current to the valve.
0 removes the current from the valve.
I applies current to the valve.
The light bulb behind the buttons displays the following:
If the light bulb behind the button goes off, the component has been correctly switched off and current has been removed.
If the light bulb behind the button lights up yellow, the component has been correctly switched on and current has been applied.
In section "Flow":
Label
MFC CO2
MFC O2
Apply
Element type
Textbox/label
Textbox/label
Button
Meaning
This field displays the current flow of the carrier gas. Field to input a target flow value. This field displays the flow progression of the carrier gas towards setpoint flow.
This field displays the current flow of the oxygen. Field to input a target flow value. This field displays the flow progression of the oxygen towards setpoint flow.
Brings the CO
2
and/or O
2
flow to a previously set value.
The two fields display the current flows. Placing the cursor in one of these fields "freezes" the flow value displayed there. You can now input a setpoint flow value. Click Update to set the respective
MFC to the setpoint flow value. The two fields now display the current flow values again and you can observe whether and how flows approaches the setpoint flow values.
In section "Ball valve":
Label
Reference position
Inlet position
Move to
Element type
Label
Label
Button
Meaning
Moves to reference position if you click the button to the right.
Moves to inlet position if you click the button to the right.
Moves to a selected position.
Remaining elements:
Label
Close
Help
Element type
Button
Button
Meaning
Closes the dialog.
Opens the description of the dialog in the help.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Performing a system test.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Error buffer (Dialog)
314
Function
This dialog displays a chronological list of all errors and events detected by the system. Every event detected is accompanied by the following information for tracking purposes:
Date and time in the "Date/Time" column.
Error code in the "Event" column.
Open
Open the dialog by selecting
Options > Diagnostics > Error buffer
.
Elements
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Interpreting PC error messages
Error display (Dialog)
Function
The following describes the elements of the dialog.
Label
Date/time; event
Number of events show deleted items
Delete
Close
Element type
Listbox
Label
Checkbox
Button
Button
Button
Meaning
Field listing every event with the date, time and its error code.
Field displaying the total number of events currently in the error buffer.
If activated, all events which have been deleted previously will be displayed again. This element is not enabled at the lowest access level.
Deletes selected events.
Prints the content of the error buffer.
Closes the dialog.
This dialog decodes the various error codes and displays the results. The error types are divided into different categories and each category is allocated to a separate tab.
Open
Open the dialog via:
Options > Diagnostics > Error display
or
by double-clicking the appropriate event line in the "Error buffer" dialog. See
Error buffer
(on
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Elements
The following describes the elements of the dialog.
Label
Input error code
Close
Element type
Textbox
Button
Meaning
Field to input the appropriate error code. Once the input box contains a code number, the program displays the decoded result green in the section above it.
Closes the dialog.
315
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Interpreting PC error messages
Options > Diagnostics > Baseline recording (Command)
What is the command used for?
This command displays the detector baseline in graph view. For better distinction the frame of the graphic field appears in red color. The baseline recording is used for troubleshooting, for example if a measurement deviates too strongly.
Select this command again to hide the base line.
Input options (Dialog)
Function
In this dialog you can define what the program should do when you input the same name. This allows you to optmize sample data input and minimize keystrokes.
Open
Open the dialog via
Options > Settings > Input
.
Elements
The following describes the elements of the dialog.
Label
Normal sample name input
Element type
Radiobutton
Apply sample name Radiobutton autom. Autoincrement the number in the sample name
Radiobutton
Meaning
The sample name is entered in the appropriate column as it is input.
After entering the sample name and pressing Enter, the input name is applied to the next line.
If a sample name ends with a number (e.g. "Name001"), this figure is automatically incremented by a certain amount and suggested for the next sample (e.g. "Name002").
Exceptions:
If the number of characters is completely used up (e.g.
"Name999"), it is not incremented and the same name is suggested for the next sample.
If the figure is not at the end of the sample name (e.g.
"Name001xyz"), it is not incremented.
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10 - Menu and dialog descriptions 316
Label autom. Autodecrement the number in the sample name
Element type
Radiobutton
Increment/decrement interval
Textbox with
Buttons
Fill method names to stop marker
Fill daily factors to last sample
Fill blank values to last sample
OK
Cancel
Checkbox
Checkbox
Checkbox
Button
Button
Meaning
Works the same way as auto-increment, only the figure in the name is decremented.
Exception:
The figure "zero" is not decremented.
In this field you can input the interval at which to increment/decrement the figure in the name. This figure can be between 1 and 99. The number must, however, fit in the displayable number of digits, otherwise the number is not changed.
If, for example, you have input/copied 10 successive sample names with the sample memory empty, the stop marker is now at the tenth sample. If you have input a method name for the first sample, this name is entered for all ten samples.
The daily factor input for the first sample is entered for all subsequent samples.
The blank value input for the first sample is entered for all subsequent samples.
Saves new settings
Discards settings not yet saved.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Settings for sample input
Optimizing sample data editing
Standard samples (Dialog)
Function
In this dialog you can create, delete, view, copy and change standard samples.
Open
Open the dialog by selecting
Options > Settings > Standards
.
Elements
The following describes the elements of the dialog.
Label
---
Name
{Element} conc. [%]
(or {Element} conc.
[ppm])
{Element} tolerance
[%]
Element type
Listbox
Textbox/label
Textbox/label
Textbox/label
Meaning
This field lists all standard samples already defined.
Field to input the name of the standard sample.
Field to input the theoretical percentage content of the corresponding element in the respective sample.
Field to input the tolerance limit of the corresponding element. The tolerance limit is required if standard tolerance monitoring is enabled.
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Label
New
Delete
Save/Create
Close
Element type
Button
Button
Button
Button
Meaning
Allows the definition of a new standard sample. This function empties the input boxes, thus data for a new standard sample can be entered.
Deletes a standard sample previously selected in the listbox.
Saves changes of an existing standard sample or creates and saves the settings of a newly defined standard sample.
Closes the dialog.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Defining standard substances as factor and monitor samples
Defining standard substances as calibration samples
Viewing list of defined factor, monitor and standard samples
Keywords (Dialog)
Function
In this dialog you specify keywords for conditioning samples and blank value samples. A key word is a reserved sample name that the software recognizes and interprets in a special way.
Note
Keywords are already defined for conditioning samples and blank value samples. You can change keywords, but you must observe the following:
The names must be distinguishable.
The program does not distinguish between uppercase and lowercase, so "BLANK" has the same meaning as "blank", for example.
Open
Open the dialog via
Options > Settings > Keywords
.
Elements
The following describes the elements of the dialog.
Label
Conditioning sample name
Name blank value
OK
Cancel
Element type
Textbox
Textbox
Button
Button
Meaning
Field to input the key word for conditioning samples.
Field for input of the keyword for blank samples
Saves the keywords.
Discards keywords not yet saved.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Defining keywords for blank and conditioning samples
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Acoustic signals (Dialog)
318
Function
In the dialog you can enable and disable acoustic signals to be output when certain events occur. The individual signals vary in pitch for easier distinction.
Open
Open the dialog by selecting
Options > Settings > Acoustic Signals
.
Elements
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Enabling/disabling acoustic signals
Configure Calculations (Dialog)
Function
The following describes the elements of the dialog.
Label
Maintenance event sound
Error sound
Analysis start sound Checkbox
Weighing data transmission sound
OK
Cancel
Element type
Checkbox
Checkbox
Checkbox
Button
Button
Meaning
If a maintenance interval is exceeded or if the interval can be expected to expire while processing a series of analyses, a warning signal is output every 2 seconds.
If the analysis system reports an error, a warning sound is output every two seconds.
A sound is output whenever a measurement starts in continuous operation.
A sound is output whenever a connected balance transmits a weighing value to the PC.
Saves new settings
Discards settings not yet saved.
In this dialog you can set the calculation method for determining the daily factor and blank value.
There are two calculation methods:
Sequential calculation. This means that a separate factor or blank value is computed for each group of standard or blank value samples; this is then used to correct the measuring samples until the next group of standard or blank value samples arrives. This calculation method allows you to compensate for fluctuations in measuring over a certain period.
Total calculation method. This means that the calculation is performed for all of the standard or blank value samples in a document. An average factor is computed.
Open
Open the dialog via
Options > Settings > Calculation
.
Elements
The following describes the elements of the dialog.
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In section "Factor determination":
Label sequentially total manual input
Element type
Radiobutton
Radiobutton
Radiobutton autom. factor calculation separate upper/lower calibration range
Checkbox
Checkbox
In section "Blank value determination":
Label sequentially total manual input
Element type
Radiobutton
Radiobutton
Radiobutton
Meaning
The blank value is computed sequentially.
The blank value is computed as a total.
The blank value can be entered manually, there will be no calculation of the blank value. calculation of the blank value starts automatically after the end of every analysis. autom. blank value calculation
Checkbox
Remaining elements:
Label
OK
Cancel
Element type
Button
Button
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Determining the daily factor
Determining blank values
Specifying the computation method for blank value and daily factor
LIMS settings (Dialog)
Function
Meaning
Saves new settings
Discards settings not yet saved.
This dialog is used to make various adjustments to a laboratory information and management system
(LIMS). The dialog has the following tabs:
On the "LIMS data" tab you select which data to send to the LIMS and whether they should be sent automatically after every analysis.
On the "Communication" tab you specify whether and how to transfer data.
If you are using multiple analyzers with one PC, you must specify one instrument identifier on the
"Identifier" tab so that the LIMS data can be allocated to the correct instrument. You can also define user names.
Note
Meaning
The daily factor is computed sequentially.
The daily factor is computed as a total.
The daily factor can be entered manually, there will be no calculation of the daily factor. calculation of the daily factor starts automatically after the end of every analysis.
Determines whether valid factors shall be computed for both calibration ranges or separate ones for each range.
Note that the LIMS port name must not be identical to the port name between the PC and the analyzer. This could lead to a system crash.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
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Open
Open the dialog via
Options > Settings > LIMS
.
Elements
The following describes the elements of the dialog.
"LIMS data" tab
In section "Data to send":
Label
{Data member}
Send data automatically after every analysis
Send weighing data on input/transfer
Element type
Checkbox
Checkbox
Checkbox
Meaning
Sends the corresponding data member.
Automatically send the data to LIMS after every analysis.
After entering or transferring the sample weight, it will be sent automatically to the LIMS.
Note:
Sends every element with a check mark. The order corresponds to the list from top to bottom. If you change the selection of elements to send, you must edit the LIMS software, otherwise the data may be misinterpreted.
"Communication" tab:
In section "Data transfer":
Label none via serial port via network
Element type
Radiobutton
Radiobutton
Radiobutton
Meaning
No data are sent to LIMS.
Data are transferred via the serial port.
The data to send to the LIMS are written to a file.
The file can be accessed from the LIMS and from the instrument operating software.
In section "Serial":
Label
Port name
Baud rate
Databits
Stopbits
Parity
Element type
Textbox
Textbox
Textbox
Textbox
Textbox
Meaning
Field to input the name of the interface.
The port name must not be the same as the port for communication between the PC and analyzer. Otherwise, operation of the analysis system will be disrupted.
Field to input transfer parameters.
Field to input transfer parameters.
Field to input transfer parameters.
Field to input transfer parameters.
Note:
The textboxes in the "Serial" section only have to be filled in if you have selected the "via serial port" radio button in the "Data transfer" section. The settings here must match those of the LIMS interface.
In section "Network":
Label
Path name
Element type
Textbox
Meaning
This field displays the path to store the data.
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Label
Browse samples
File extension
Element type
Button
Textbox
Meaning
Opens the "Find folder" dialog in which you can search the file structure and select a directory.
The path must already exist, it cannot be created from the instrument operating software.
Field to input the file extension. The file name is automatically generated by the program as follows: dddsssss.xxx
. where:
ddd
= Days since January 1.
sssss
= Seconds since midnight.
xxx
= defined file extension
Thus, the file 12837894.abc was created at the following date:
128
: File was created on the 128th day of the year, i.e. on May 9.
37894
: File was created 37894 seconds after midnight, i.e. at 10:31:34.
abc
: Defined file extension.
As described above. File extensions weights
Create extra PDF
Textbox
Checkbox The data sent to LIMS will be saved to an additional PDF file.
Note:
You only need to edit the "Network" section if you have selected the "via network" radio button in the "Data transfer" section.
"Identifier" tab:
On this tab:
Label Element type
Instrument identifier Textbox
User's name
Balance ID
Balance operator
Textbox
Textbox
Textbox
Meaning
Field to input an instrument identifier. If there are several analyzers connected to the PC, you must define an instrument identifier for each instrument so that the LIMS data are assigned to the correct instrument. The instrument identifier precedes the actual data and can be interpreted by the LIMS.
Field for display of the user's name. The user's name is similar to the name of the user who is currently logged on.
The name precedes the actual data and can be interpreted by the LIMS.
Field to enter the ID of the balance. The balance identifier precedes the actual data and can be interpreted by the
LIMS.
Field to input the name of the balance operator. The name precedes the actual data and can be interpreted by the
LIMS.
Valid for all tabs:
Remaining elements:
Label
OK
Element type
Button
Meaning
Saves new settings
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Label
Cancel
Element type
Button
Meaning
Discards settings not yet saved.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Exporting LIMS data
Defining the LIMS / PC interface
Laboratory information and management system (LIMS)
LIMS export settings
Method (Dialog)
Function
In this dialog you can create, delete, view, copy and change methods.
Note
The method parameters can not only be defined via a method but also via the "Device parameters" dialog. If not otherwise defined by a method, the settings in the "Device parameters" dialog apply. If a parameter is defined differently in the method and in the "Device parameters" dialog, the method takes priority if it is used for the measurement.
Open
Open the dialog by selecting
Options > Settings > Methods
.
Elements
The following describes the elements of the dialog.
Label
---
Identifier
Description
O2 dosing time
O2 dosing flow
O2 cut off threshold
Autozero delay
Element type
Listbox
Textbox
Textbox
Textbox
Textbox
Textbox
Textbox
Meaning
This field lists all methods already defined.
Field to input the name of the method. When you enter the name in the sample view, this method is allocated to the appropriate sample.
Field to input the purpose of the method. For easier selection of a method.
Field to input the duration of O
2
dosing during the combustion phase. The O2 dosing can be gradually filled in by adjusting the O2 dosing time 1.
Field to input the duration of oxygen flow during the combustion phase. The O2 flow can be gradually filled in by adjusting the O2 dosing flow 1.
Field to input a value which delimits the oxygen excess. If during the oxygen dosing the measured oxygen concentration exceeds this value, then the oxygen supply will be turned off.
Field to input a time. Defines the time to wait after introduction until the system performs autozero alignment.
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Label
Peak anticipation
Integrator reset delay Textbox
Kjeldahl factor
New
Delete
Default method
Element type
Textbox
Textbox
Button
Button
Button
Meaning
Field to input a time. Defines the time the system waits for the occurrence of the nitrogen peak. If the system has not detected a peak start after expiration of this peak expectation time, it assumes that the sample does not contain nitrogen.
Field to input a time. Defines the time after which the integrator is reset to zero before beginning actual integration.
Field to input a factor which is used to normalize the nitrogen results measured by the rapid N to their Kjeldahl equivalent values.
Allows the definition of a new method. This function empties the input boxes, thus data for a new method can be entered.
Deletes a method previously selected in the listbox.
Defines the method selected in the list box as the default method. If during input of sample data no method has been specified then the program suggests the name of the default method.
Saves changes of an existing method or creates and saves the settings of a newly defined method.
Save/
Create
Close
Button
Button Closes the dialog.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Viewing method settings
Defining custom methods
Copy methods
Optimizing basic instrument settings
Monthly logbook (Dialog)
Function
This dialog contains records of the actions performed by various users in chronological order. You can search for and print out certain information via the dialog menus. The following information is stored for each action:
Date and time of the action,
Name of the person who performed the action,
Type of action,
Description of changes, e.g. of parameters,
User's justification if the action needed to be justified.
Note:
The period displayed in the logbook covers a maximum of one month, usually the current month.
However, it is possible to display actions preceding this period.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Open
Open the dialog by selecting
Options > Logbook
. This dialog is only accessible if 21 CFR Part 11 functionality is enabled.
324
Elements
The following describes the elements of the dialog.
In the "File" menu:
Label
File > Load
File > Save As
File > Print
File > Close
Element type Meaning
Menu command Opens the "Select period" dialog in which you select the desired period. Allows you to load actions further in the past. If no file is found for the selected period, a message is displayed.
Menu command Opens the "Save logbook as" dialog in which you can save the current records to a file outside of the database.
Menu command Outputs the records currently being displayed to a printer.
Menu command Closes the dialog.
In the "Edit" menu:
Label
Edit > Copy
Edit > Select All
Edit > Search
Element type Meaning
Menu command Copies the selected text to the clipboard. You can then insert this text in a text documennt, for example.
Menu command Selects the whole text. You can then copy the selected contents via Edit > Copy.
Menu command Opens the "Search" dialog in which you can search for certain phrases.
Remaining elements:
Label Element type
Button
...
Meaning
Reverse the chronological order; either the oldest or the most recent entry is displayed first.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Viewing the logbook
21 CFR Part 11 functionality
Select period (Dialog)
Function
In this dialog you select the period for which to display the logbook.
Open
Open the "Logbook for month..." dialog via
Options > Logbook
. Open the "Select period" dialog by selecting
File > Load
.
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10 - Menu and dialog descriptions 325
Elements
The following describes the elements of the dialog.
Label
Year
Month
OK
Cancel
Element type
Textbox with buttons
Textbox with buttons
Button
Button
Meaning
Field to input a year. You can also set the year in the textbox using the arrows.
Field to input a month. You can also set the month in the textbox using the arrows.
Saves new settings
Discards settings not yet saved.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Viewing the logbook
21 CFR Part 11 functionality
Device configuration (Dialog)
Function
In this dialog you can define initialization entries to adjust system behavior.
The individual tabs represent the respective initialization files. There are various sections in an initialization file. Each section contains entries whose values influence the behavior of the system.
During operation, the system stores certain information in the initialization files. It is usually not necessary to modify these values. The entries that may be changed are located on the following tabs:
DEVICE.INI
LEAKTEST.INI
Safety instruction
Strictly observe the safety instruction "Improper changes" under
Warning notes during operation
Note
This section only describes the sections of the tabs in which you can make changes via the "Device configuration" dialog only, as these sections do not have their own settings menu.
If 21 CFR Part 11 functionality is enabled, every change to the configuration must be justified in the
"Comment modification" dialog.
Open
Open the dialog by selecting
Options > Configuration
.
Elements
The following describes the elements of the dialog.
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10 - Menu and dialog descriptions 326
Valid for all tabs:
Label
Section
Entries
New Section
Edit
Delete
Paste
Import
Export
Delete all
OK
Element type Meaning
Dropdown listbox This field lists the available sections. Field to input a name for a new section.
Listbox This field lists the entries of a previously selected section.
Button
Button
Creates a new section under the name previously entered in the dropdown listbox.
Opens the "Configure key value" dialog. Allows you to edit a section entry previously selected from the list.
Button
Button
Button
Button
Button
Button
Deletes a section previously selected in the dropdown listbox.
Deletes a section entry previously selected in the listbox.
Opens the "Configure key value" dialog. Allows you to insert new entries in a section.
Opens the "Open" dialog. Allows you to import further sections.
Opens the "File save as" dialog. Allows you to export sections.
Deletes all entries which are included in the activated tab.
Saves new settings
"DEVICE.INI" tab
The following table describes the entries under the "AnalyzerPort" section:
Entry
Name
Baud
Data
Stop
Parity
Standard
COM1
9600
8
1
N
Description
Defines the serial interface between the PC and the analyzer.
Defines the transfer rate of the serial interface between the PC and the analyzer.
Defines the number of databits of the serial interface between the
PC and the analyzer.
Defines the number of stopbits of the serial interface between the
PC and the analyzer.
Defines the type of parity check of the serial interface between the
PC and the analyzer.
N= no parity check
E= even parity check
O= odd parity check.
The following table describes the entries under the "BalancePort" section:
Entry
Name
Baud
Data
Stop
Standard
----
300
7
1
Description
Defines the serial interface between the PC and the balance.
Defines the transfer rate of the serial interface between the PC and the balance.
Defines the number of databits of the serial interface between the
PC and the balance.
Defines the number of stopbits of the serial interface between the
PC and the balance.
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10 - Menu and dialog descriptions 327
Entry
Parity
Standard
O
Description
Defines the type of parity check of the serial interface between the
PC and the balance.
N= no parity check
E= even parity check
O= odd parity check.
The following table describes the entries under the "BalanceInit" section:
Entry
StartString
EndString
WeightFactor
Standard
----
----
1
Description
Defines the character with which a weighing datum starts. This is used for correct interpretation of the characters received.
Defines the character with which a weighing datum ends. This is used for correct interpretation of the characters received.
The WeightFactor allows correction of the weighing data sent by the balance. The program expects weighing data milligram format.
For example, if the balance sends data in gram format, you must set WeightFactor to 1000.
The following table describes the entries under the "PGP" section:
Entry
ExecutablePath
Sign Parameters
Standard
---
---
Verify Parameters ---
Description
Defines what signature program to use for signing and verifying documents.
Defines what parameters must be sent to the signature program when signing.
Defines what parameters must be sent to the signature program when verifying.
The following table describes the entries under the "Menu" section:
Entry xxx
Standard
1,2,3
Description
The text in this entry describes the respective menu command.
The value to the right of the equals sign defines the access level with which the user may access this command. 1 means the lowest, 3 is the highest level.
The following table describes the entries under the "System" section:
Entry
Logon Timeout
User1
User2
User3
Standard
60
---
Description
Defines the time that must expire before the program displays the login dialog again.
Specifies the name of the user group which the instrument software regards as level 1 users.
Specifies the name of the user group which the instrument software regards as level 2 users.
Specifies the name of the user group which the instrument software regards as level 3 users.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Defining the analyzer / PC interface
Creating new sections
Granting authorizations
Defining the autoexport directory
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10 - Menu and dialog descriptions 328
Configure key value
Optimizing basic instrument settings
What can you modify in the configuration?
Error handling (Dialog)
Function
In this dialog you can define how you want the operating software to react to detected errors.
Open
Open the dialog via
Options > Settings > Error handling
.
Elements
The following describes the elements of the dialog.
Label
Standard tolerance monitoring
Ni flap monitoring
Element type
Checkbox
Checkbox
Blank value threshold Textbox
Number of errors
OK
Cancel
Textbox
Button
Button
Meaning
Every finished standard sample is checked as to whether the computed percentage contents are inside the defined tolerance range for theoretical percentage contents. If the tolerance limit is exceeded, continuous analysis is aborted and "Tol" is entered in the info column of the appropriate sample. The defined tolerance limits can be seen in the
"Standard samples" dialog. See
Standard samples
(on
Every finished sample, which is not a blank sample, is checked for its peak area. If its value does not exceed a minimum threshold, the program assumes that the sample has not been thrown in which is in the most cases the result of a blocked Ni flap. The minimum threshold can be defined in the "Blank value threshold" field.
Allows to input of a minimum threshold for the Ni flap monitoring (see description above).
Field to input a number between 0 and 10. This figure defines how many successive analyzed samples may display non-critical errors before aborting continuous operation. Input 0 to disable this stop mechanism. If a critical error occurs, the analysis is immediately stopped regardles of the figure you input.
Saves new settings
Discards settings not yet saved.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Configuring error handling
Interpreting PC error messages
Determining the daily factor
Optimizing basic instrument settings
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Sleep / wake-up function (Dialog)
Function
In this dialog you define the sleep and wake-up options for the analyzer.
Note:
329
Observe the following when entering the date in the "Wake-up" section: The program accepts numbers between 1 and 31 for day input, but it does not check whether the date is permissible (e.g.
09/31).
Open
Open the dialog by selecting
Options > Settings > Sleep/Wake-up
.
Elements
The following describes the elements of the dialog.
In section "Sleep":
Label
Sleep disabled
Element type
Radiobutton
Sleep after end of sample
Radiobutton
Sleep at sample No. Option field / textbox
Shut off carrier gas Checkbox
Meaning
The sleep/wake-up function is disabled.
The analyzer goes into sleep mode after finishing the last sample (indicated by the stop marker).
The analyzer goes into sleep mode when it reaches the specified sample.
You can enter the sample number in the adjacent textbox.
Shuts off the carrier gas when the analyzer goes into sleep mode.
The heater of the combustion tube will be turned off. Switch of combustion tube
Switch of post combustion tube
Switch off the
Reductor
Sleep now
Checkbox
Checkbox
Checkbox
Button
The heater of the combustion tube will be turned off.
The heater of the Reductor will be turned off.
Causes the analyzer to go into sleep mode immediately.
In section "Wake-up":
Label
Time
Element type
Textbox
Date
One-time wake-up at above time/date
Daily wake-up at above time/date, except
Mon. Tues. Wed.
Thurs. Fri. Sat. Sun.
Continue after wakeup if there are samples
Wake up now
Textbox
Radiobutton
Radiobutton
Checkbox
Checkbox
Button
Meaning
Fields to input the time in hours and minutes at which to wake up the analyzer.
Fields to input the date on which to wake up the analyzer.
Wakes up the sleeping analyzer at the date and time specified above.
Wakes up the analyzer every day at the time specified above.
Defines on which days not to wake up the instrument, e.g. on weekends.
If there are any unprocessed samples in sample memory, analysis is automatically resumed after "wake-up".
Wakes up the analyzer immediately.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Remaining elements:
Label
OK
Cancel
Element type
Button
Button
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Shutting the instrument down for short measuring breaks (standby).
Optimizing sleep and wake-up behavior
Optimizing basic instrument settings
Configure key value (Dialog)
Function
Meaning
Saves new settings
Discards settings not yet saved.
This dialog is used to configure the system. In this dialog you allocated values to the system that influence the system's behavior.
330
Safety instruction
Strictly observe the safety instruction "Improper changes" under
Warning notes during operation
Open
Open the "Configure instrument" dialog by selecting View > Configuration . Click:
Edit
to edit a selected entry in a section.
Insert
to create a new entry in a section.
Elements
The following describes the elements of the dialog.
Label
Key
Value
OK
Cancel
Element type
Textbox/label
Textbox/label
Button
Button
Meaning
Field to input the key. This field displays the key of an entry previously selected in the "Device configuration" dialog and allows you to edit this key. The field is only enabled if the dialog was opened via the Insert button.
Field to input the value. This field displays the value of an entry previously selected in the "Device configuration" dialog and allows you to edit this key.
Saves new settings
Discards settings not yet saved.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Granting authorizations
Defining logon timeout
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Creating new sections
Defining the analyzer / PC interface
Defining the autoexport directory
Device configuration
331
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10 - Menu and dialog descriptions
Windows menu
Purpose
This section describes commands and dialogs for this menu.
In this section
332
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10 - Menu and dialog descriptions
Windows > Toolbar / Run-Bar (Command)
What are these commands used for?
This command shows or hides the toolbar and the run bar. If the toolbar and/or the run bar is displayed, a check will appear next to the menu item. See
Toolbar
Toolbar
Toolbar
The individual buttons on the toolbar correspond to the following commands:
Icon Command
File > New
File > Open
File > Save
Edit > Copy
Edit > Paste
Edit > Insert Line
Edit > Delete Line
Edit > Undo
Edit > Restore
File > Print
File > Print preview
Statistics > Group
Statistics > Include/Exclude sample
View > Zoom in/out
Calibration > Previous
Calibration > Next
Calibration > Previous sample
333
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10 - Menu and dialog descriptions 334
Icon Command
Calibration > Next sample
System > Wake-up
Help > About ...
System > Auto run
System > Single run
System > Single run (when manual injection is selected)
Note
The number of the available symbols in the toolbar can be different depending on the instrument type.
Windows > Recent sample (Command)
What is the command used for?
This command shows or hides the enhanced display of the sample analyzed most recently. If the most recently sample is displayed, a check will appear next to the menu item.
Windows > Status view (Command)
What is the command used for?
This command shows or hides the status view. If the status view is displayed, a check will appear next to the menu item.
Windows > Default layout (Command)
What is the command used for?
This command switches the arrangement of the windows to its default settings:
Displayed are
Toolbar
Run bar
Recent sample
Status view
Setting of the balance windows will not be affected.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
10 - Menu and dialog descriptions
Help menu
Purpose
This section describes commands and dialogs for this menu.
In this section
335
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10 - Menu and dialog descriptions 336
Help > Content (Command)
What is the command used for?
This command opens the "Contents" tab of the help window in the foreground.
Short cuts
Invocation via hot key: F1
Help > Find (Command)
What is the command used for?
This command opens the "Search" tab of the help window in the foreground.
Help > BÜCHI Labortechnik AG on the WEB (Command)
What is the command used for?
This command creates an Internet link to the BÜCHI Labortechnik AG website, on condition that the
PC has an Internet connection.
Product registration (Dialog)
Function
In this dialog you can input your registration data to unlock the operating software.
Open
This dialog is automatically displayed when you launch the operating software for the first time, if you forgot any important details during registration. Open the dialog by selecting
Help > Registration
.
Elements
The following describes the elements of the dialog.
In section "User":
Label
Company/Dept.
Street
ZIP
City
Country
Tel. e-mail
Element type
Textbox
Textbox
Textbox
Textbox
Textbox
Textbox
Textbox
Meaning
Field to input user data.
Field to input user data.
Field to input user data.
Field to input user data.
Field to input user data.
Field to input user data.
Field to input user data.
Note:
These data are not mandatory. However, these data make it easier for BÜCHI's service department to identitfy customers if you have a problem and contact BÜCHI.
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In section "Analyzer":
Label
Type
Serial number
Element type Meaning
Dropdown listbox Field displaying the instrument type.
Textbox Field to input the serial number if it was not automatically sent to the program by the analyzer. The serial number is found on the type plate on the back of the analyzer. This number should match the serial number of the installation
DVD cover when installing for the first time.
In section "Software":
Label
Version
Software ID
Element type
Label
Textbox
Meaning
This field displays the software version number.
Field to input the identification code. If installing for the first time, this number is found on the installation DVD cover. If installing and upgrading, you must send the registration details in this dialog to BÜCHI. You will then receive an identification code to be entered here.
It is not possible to operate the system if the identification code is missing or incorrect.
Remaining elements:
Label
OK
Cancel
Element type
Button
Button
Meaning
Saves new settings
Discards settings not yet saved.
Further information
Further information includes instructions in which the dialog is used and knowledge articles concerning the dialog:
Modifying the registration.
Help > About... (Command)
What is the command used for?
This command displays the following:
The copyright note.
The software version number.
If the system is connected, the version numbers of the individual modules are also displayed. They provide valuable information about the status of the system and what to do in the event of updates.
Short cuts
Invocation via the toolbar:
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
C H A P T E R 1 1
Appendix
Target group
Personnel involved with the instrument.
In this chapter
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
11 - Appendix
Revision history
List of modifications in this document up to now
Date
29.09.2014
16.10.2014
Modification
Creation made small text correction in the section "Replacing fuses"
340
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11 - Appendix
Warranty
Target group
Personnel involved with the instrument.
In this section
341
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11 - Appendix 342
Warranty of the overall instrument
Warranty of the overall instrument
Please refer to your order for details on the warranty on the overall instrument.
Excluded from the warranty
Wear and tear parts and consumables are excluded from the warranty.
Warranty on the furnace
Warranty on the furnace
BÜCHI Labortechnik AG gives a 10-year warranty on the furnace. In the event of a manufacturing or material fault, you will receive a replacement furnace free of charge during the 10 years as of the date of delivery.
What is excluded from the warranty?
Damage due to improper use is excluded from the warranty. The following instructions have been compiled for correct operation of the furnace and must be observed in order to uphold the warranty.
Instructions for operating the furnace
Observe the following instructions for using the furnace so that the warranty is upheld.
The user must ensure that the furnace is operated according to the instructions.
The furnace must not be heated in excess of the maximum temperature indicated in the operating instructions.
The furnace must not be operated with a voltage higher than that indicated on the type plate.
In the event of breaks lasting several hours (e.g. overnight downtime) furnace 1 must be reduced to 800 °C.
In the event of longer breaks lasting several days (as of 5 days) the furnace must be shut down
(set temperature control to 0 °C).
The furnace must be protected against penetration of liquids.
Short-circuits in connection with the heating spirals and/or the thermocouples must be avoided.
Inner and outer damage to the heating spirals, thermocouples and supply lines must be avoided.
Only use original parts from BÜCHI for operation (e.g. combustion tubes / Reductor, fillings, seals, etc.).
In the event of furnace failure, the furnace must be sent at the following address for fault identification:
BÜCHI Labortechnik AG,
Meierseggstrasse 40,
9230 Flawil
Switzerland
If this analysis reveals that the furnace became defective due to improper use, all warranty claims shall be forfeited.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
11 - Appendix
Accessories, spare parts and consumables
Target group
Personnel involved with the instrument.
Purpose
This secton contains information about ordering accessories, spare parts and consumables.
In this section
343
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11 - Appendix 344
Smallest workable unit
Condition
You can only order the smallest workable unit if you already have all of the necessary accessories.
See Required accessories.
Smallest workable unit
D-480 basic instrument with initial set including Starter-KIT.
Computer with control and application software.
Component details
Basic instrument: Fully automatic elemental analyzer for quantitative determination nitrogen in solid or liquid samples.
Initial set for initial start-up and instruction.
Starter-KIT.
Computer with control and application software: The computer is suited for 230 V and 50/60 Hz, other voltages on request. Windows operating system, software available in German or English.
Basic instrument product numbers
Product numbers for the basic instrument with initial set, initial chemical set, replacement chemicals and consumables set are listed below:
Basic instrument product numbers
16.30-0000 (Basic unit)
Operating mode
N
16.02-5010 (Initial equipment) N
16.02-5052 (Starter-KIT) N
Product numbers for computer with control and application software
The product numbers for the computer with control and application software are listed below:
Language Product numbers for computer with control and application software
50 008 369
50 008 368
16.03-8000
Computer (operating system
German)
Computer (operating system
English)
Instrument software German/English
Instrument CD/DVD
The CD/DVD provided with the instrument contains the following information:
List of initial equipment
Various consumable sets
Catalog of spare parts
Operating instructions
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
11 - Appendix
Required accessories
345
Note
The following section describes what accessories you need in addition to the smallest working unit and the order numbers.
Computer
A computer is essential as the control and evaluation unit. The computer can be ordered together with the software. See Smallest working unit.
If you are using your own computer, please observe the following requirements:
PC with Pentium III processor 500 MHZ (or equivalent) or faster
PC with operating system Windows 7 Professional or a newer version of Windows Professional
Available disk space min. 2 GB
Serial interfaces
2 x RS 232 (instrument and balance) or
1 x USB (instrument) and 1 x RS 232 (balance)
DVD-ROM drive
Printer
Article no. 50 031 857
Printer with printer cable for 230 V, 50/60 Hz, other voltages on request.
Electronic microbalance
There are two different microbalances available:
Electronic microbalance 1:
Reading precision 0.1 mg
Weighing range up to 64 g
With V 24/ RS 232 interface
Prod. No. 12.01-0202
Pressure reducer O
2
Two-stage, 2nd stage 0-3 bar with stop valve
For gas quality 99.995 % or better
Article no. 04 278 800
Electronic microbalance 2:
Reading precision 0.01 mg
Weighing range up to 61 g
With V 24/ RS 232 interface
Prod. No. 25.00-0202
Pressure reducer CO
2
Two-stage, 2nd stage 0-3 bar with stop valve
For gas quality 99.995 % or better
Article no. 04 278 810
Note
If you want to use your own pressure reducer, it must be a two-stage precision pressure reducer of a higher quality category (Air Liquid or equivalent). Inferior reducing valves impair the results of analysis.
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
11 - Appendix
Optional accessories
346
Note
The following section lists the optional accessories. Please refer to the consumable material catalog for ordering procedure.
Consumables set for solid samples
Optional
Required when the material from the initial set is used up.
The following table lists consumables for solid samples:
Consumable material set product number
16.02-5051 (Reagent kit)
16.02-5050 (Convenience pack)
Number of analyses approx. 4000
Accessories for liquid samples / samples sensitive to air
The following accessories are required for liquid samples / samples sensitive to air:
Capsule press
For dosed filling and gas-tight closure of tin capsules for liquid and sensitive samples
Prod. No. 41.05-0000
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
11 - Appendix
Declaration of conformity
Purpose
This section includes the declaration of conformity of BÜCHI Labortechnik AG.
In this section
Declaration of conformity .............................................................................................................348
347
Operating instructions DuMaster D-480 ©BÜCHI Labortechnik AG
Index 349
Index
2
21 CFR Part 11 functionality - 71, 92, 257, 258, 259,
260, 324, 325
A
About this document - 14
Accessories, spare parts and consumables - 343
Acoustic signals (Dialog) - 318
Adjust carousel (Dialog) - 309
Adjust carousel position (Dialog) - 290
Administrative work on the database - 92, 266, 268,
269, 270
Analytical characteristics - 33
Analytical characteristics and technical specifications - 32
Appendix - 339
Area assignment (Dialog) - 295
Assessing the calibration curves - 176, 178, 179
B
Background knowledge required for calibration - 48,
51, 66, 176, 303, 304
Ball valve maintenance - 197
Basic facts about working with the instrument - 49
Basic functions of the operating software - 59
Basic security settings - 17
Blank values (Dialog) - 293
C
Calibration > Next (Command) - 305
Calibration > Next sample (Command) - 305
Calibration > Previous (Command) - 305
Calibration > Previous sample (Command) - 305
Calibration coefficients (Dialog) - 302
Calibration curve calculation method criteria - 51,
52, 177
Calibration formulae - 51, 54, 304
Calibration menu - 301
Calibration table for nitrogen calibration - 183
Calibration tables - 182
Changing the position of the carousel - 246, 247,
249
Checking documents for authenticity - 89, 164, 260
Checklist for blank value / conditioning and daily factor measurements - 139
Checklist for real sample measurement - 140
Clean database (Dialog) - 269
Cleaning and installing the quartz glass bridge - 214
Cleaning, assembling and installing the ball valve. -
202
Column properties (Dialog) - 284
Combi view - 63
Operating instructions DuMaster D-480
Comment modification (Dialog) - 258
Conditioning newly installed tubes - 170
Conditions for operating the LIMS - 70
Configure analyzer - 75, 76, 97
Configure backup (Dialog) - 94, 267
Configure Calculations (Dialog) - 318
Configure calibration (Dialog) - 303
Configure graph view (Dialog) - 282
Configure key value (Dialog) - 328, 330
Configure report - 99, 155, 262, 264
Configure report (Dialog) - 261
Configure sample view (Dialog) - 279
Configure statistics view - 99, 148, 284
Configure statistics view (Dialog) - 283
Configuring error handling - 122, 328
Configuring the graph view - 99, 154, 283
Configuring the sample view - 68, 99, 147, 280, 285
Connecting peripherals - 107, 108
Connecting supply lines and waste gas lines - 109
Consequences of modifying analysis data - 87, 257
Copy methods - 130, 323
Copying documents via the clipboard - 162
Creating new documents - 160, 256
Creating new sections - 77, 258, 327, 331
D
Data administration and data security - 69
Data backup and printing - 64, 137, 138, 156, 177,
256, 262, 264, 283
Database - 92, 260, 269
Database backup - 93
Declaration of conformity - 347, 348
Default instrument settings - 112
Define peak start / end (Dialog) - 294
Define type of peak (Dialog) - 294
Defining custom methods - 97, 129, 323
Defining custom standard substances - 119
Defining interfaces - 83
Defining keywords for blank and conditioning samples - 119, 317
Defining LIMS export settings - 78
Defining logon timeout - 76, 258, 330
Defining maintenance intervals in the software - 168
Defining standard substances - 174
Defining standard substances as calibration samples - 62, 120, 176, 303, 304, 317
Defining standard substances as factor and monitor samples - 62, 120, 176, 317
Defining the analyzer / PC interface - 84, 258, 327,
331
Defining the autoexport directory - 93, 258, 327, 331
Defining the balance / PC interface - 85
Defining the Kjeldahl factor - 130
Defining the LIMS / PC interface - 84, 322
©BÜCHI Labortechnik AG
Index
Delete sample pane (Dialog) - 281
Deleting documents - 161
Detection of measuring components and evaluation of the measuring signal - 45, 48
Determine measuring units and number of decimal places. - 99, 147, 280, 285
Determining blank values - 141, 171, 216, 246, 293,
319
Determining sample weight - 124
Determining the daily factor - 142, 319, 328
Device configuration (Dialog) - 84, 85, 325, 331
Dialog descriptions key - 252
Display conventions - 15
Display print preview - 155, 262, 264
E
Edit > Copy (Command) - 273
Edit > Cut (Command) - 273
Edit > Delete line (Command) - 274
Edit > Insert line (Command) - 274
Edit > Modify (Command) - 275
Edit > Paste (Command) - 274
Edit > Redo (Command) - 273
Edit > Undo (Command) - 273
Edit menu - 272
Editing analysis data - 86, 161
Editing documents - 160
Emptying and filling reaction tubes - 220
Emptying reaction tubes - 221
Enabling/disabling acoustic signals - 121, 318
Error buffer (Dialog) - 314
Error display (Dialog) - 314
Error handling (Dialog) - 97, 207, 328
Export analysis data for support - 249
Export peak graphics (Dialog) - 261
Export to LIMS (Dialog) - 260
Exporting analysis data to MS Excel and viewing -
157, 256, 257
Exporting LIMS data - 158, 261, 322
F
Feeding (Dialog) - 290
File > Delete (Command) - 258
File > Exit (Command) - 271
File > Export/Import > Create Excel sheet
(Command) - 271
File > Logoff (Command) - 271
File > New (Command) - 254
File menu - 253
Filling the combustion tube - 221
Filling the drying tubes - 107, 167, 175, 233
Filling the post combustion tube - 223
Filling, removing and installing the absorption and drying tubes - 232
Finding documents - 161, 256, 257
Formula for determining the daily factor - 57
Formulae for blank value determination and compensation - 56, 294
Formulae for generating statistical data - 149
Formulas for determining element concentration of analysis samples (Solids) - 48
Front view - 36
Functional units - 43
Furnace switch off/on (Dialog) - 289
Operating instructions DuMaster D-480
350
G
Gases and chemicals to be provided - 106
General - 13
General information on the operating instructions -
15
Generating statistical data - 148
Granting authorizations - 81, 258, 327, 330
H
Heating up the furnace - 108, 113
Help > About... (Command) - 337
Help > BÜCHI Labortechnik AG on the WEB
(Command) - 336
Help > Content (Command) - 336
Help > Find (Command) - 336
Help menu - 335
I
Important information about maintenance - 166
Importing documents - 163, 266, 267
Importing weighing data - 131
Initialize the instrument (Dialog) - 289
Input options (Dialog) - 97, 315
Installation site requirements - 105
Installing and updating the software - 74, 112
Installing reaction tubes in the furnace and conditioning - 228
Installing the ash crucible - 188
Installing the Ni flap - 209
Installing used tubes - 169, 308
Instructions for disposal of consumables - 18
Instructions for operating the furnace - 105
Instrument design - 35
Instrument equipment - 50
Intended use of the instrument - 19
Interpreting PC error messages - 63, 238, 314, 315,
328
K
Keywords (Dialog) - 317
L
Laboratory information and management system
(LIMS) - 70, 261, 322
Layout and mode of functioning - 42
Leak test: Test phases (Dialog) - 240, 311
Leak test (Dialog) - 310
Leak test procedure - 240, 241
Left side view - 38
Limits for modifying analysis data - 87
LIMS export settings - 79, 261, 322
LIMS settings (Dialog) - 70, 79, 84, 261, 319
Linking the analyzer and software - 72
Load balance file (Dialog) - 267
Load sample pane (Dialog) - 281
Loading a sample view - 148, 281
Log in as (Dialog) - 270
M
Maintaining the instrument - 165
Maintaining the Ni flap and the O2 lance - 206
Maintenance intervals (Dialog) - 307
©BÜCHI Labortechnik AG
Index
Maintenance work to be performed by the customer
- 167
Manual peak integration - 150, 294, 295, 296
Math > Blank values > Calculate (Command) - 293
Math menu - 292
Math. > Factor (Command) - 294
Math. > Recalculate (Command) - 297
Measurement settings - 108, 118
Menu and dialog descriptions - 60, 251
Method (Dialog) - 322
Modifying the registration - 101
Monthly logbook (Dialog) - 323
O
Open (Dialog) - 266
Optimizing basic instrument settings - 97, 323, 328,
330
Optimizing data evaluation - 99, 263, 264, 281
Optimizing instrument condition for calibration - 175
Optimizing sample data editing - 97, 275, 316
Optimizing sleep and wake-up behavior - 97, 132,
330
Optional accessories - 346
Options > Diagnostics > Baseline recording
(Command) - 315
Options menu - 306
Overview of export and import file formats - 157
P
Packing samples - 125
Performing a leak test - 240
Performing a system test - 239
Performing checks - 88
Performing measurement work - 108, 134, 291, 310
Performing measurements - 136
Performing other administrator tasks - 100
Performing routine measuring work - 138
Performing the calibration - 173, 175
Peripherals and their function - 40
Preparing and following up maintenance work - 169
Preparing measurement work - 127
Preparing measuring data for evaluation - 146
Preparing samples - 123, 176
Print (Dialog) - 99, 263
Print preview (Dialog) - 99, 264
Printer setup - 99, 101, 265
Printer setup (Dialog) - 265
Prioritizing urgent samples - 132, 275
Processes in the instrument during a measurement
- 46
Product description - 31
Product registration (Dialog) - 336
Purpose and frequency of crucible replacement -
185
Purpose and frequency of maintaining the Ni flap and O2 lance - 207
Purpose and frequency of refilling of the Regainer -
191
R
Reacting to a power failure - 245, 277, 291, 310,
311, 312
Rear view - 37
Operating instructions DuMaster D-480
351
Recommendations for user administration - 81
Reductor replacing - 224
Refill the Regainer - 190, 191
Reloading an old database file - 95, 270
Removing and cleaning the Ni flap - 207
Removing and dismantling the ball valve - 198
Removing and installing the drying tubes - 235
Removing sealing elements from grooves - 167, 196
Removing the ash crucible - 185
Removing the quartz glass bridge - 214
Removing the reaction tubes from the furnace - 226
Removing the transport protection - 110
Removing, cleaning and installing the carousel -
217, 218
Removing, cleaning and installing the quartz glass bridge - 213
Removing, cleaning and re-installing the O2 lance -
211
Removing/installing and conditioning the reaction tubes - 225
Reorganize database - 94, 258, 269
Repairing the instrument - 237
Replace part (Dialog) - 215, 308
Replacing fuses - 241
Replacing sealing elements - 194
Replacing the ash crucible - 184
Representation of safety instructions - 18
Required accessories - 345
Required personal safety equipment - 24
Required user knowledge and skills - 23
Restore database (Dialog) - 95, 269
Revision history - 340
Re-weighing after sample loss - 248
Right mouse button function - 67, 276, 277, 283,
284, 285, 290, 304
Right side view - 37
Routine measuring work - 55, 294
Rules for first-time start-up - 105
S
Safety devices in the analyzer - 20
Sample insertion and initiation of measurement - 44,
47
Sample preparation instructions - 124, 137, 138
Sample view - 61
Save file as (Dialog) - 257
Save sample pane (Dialog) - 280
Saving the sample view - 99, 148, 281
Select columns (Dialog) - 284
Select current sample (Dialog) - 276
Select document name (Dialog) - 254, 257
Select period (Dialog) - 324
Select version (Dialog) - 256
Set current weighed sample (Dialog) - 277
Set stop tag (Dialog) - 276
Setting the size of the graph - 99, 154, 279
Setting up and starting up the instrument - 104
Setting up user administration - 80
Settings for sample input - 131, 316
Showing or hiding the toolbar - 128
Showing or hiding the weight window - 125
Shutting down the instrument - 114
Shutting the instrument down for long measuring breaks (switching off) - 115
©BÜCHI Labortechnik AG
Index
Shutting the instrument down for short measuring breaks (standby) - 115
Sign (Dialog) - 259
Signing documents - 89, 163, 259
Sleep / wake-up function (Dialog) - 329
Smallest workable unit - 344
Software usage rules - 128
Software user interface - 60
Specify lower and upper calibration range (Dialog) -
304
Specifying the computation method for blank value and daily factor - 121, 293, 319
Standard samples (Dialog) - 316, 328
Standard samples display (Dialog) - 296
Starting the database backup - 94, 167, 268
Starting the operating software - 108, 128, 245, 271
Starting up and shutting down the instrument - 103
Start-up - 107
Statistics > Clear statistic (Command) - 299
Statistics > Create Excel sheet (Command) - 300
Statistics > Delete group (Command) - 299
Statistics > Group (Command) - 299
Statistics > Include/Exclude sample (Command) -
300
Statistics > Include/Exclude value (Command) - 300
Statistics > Sort group (Command) - 299
Statistics > Via names (Command) - 299
Statistics menu - 298
Status view - 66
Stopping continuous analysis - 144, 248, 276, 290
Substance digestion and preparation of the reaction gas mixture - 47
Swap samples (Dialog) - 98, 275
Switching on - 108, 112
System > Auto run (Command) - 288
System > Auto zero (Command) - 289
System > Single run (Command) - 288
System > Stop (Command) - 288
System > Wake up (Command) - 290
System menu - 287
System test (Dialog) - 312
T
Technical specifications - 33
The thermal conductivity detector (TCD) - 45, 48
Toolbar - 61, 333
Top view - 39
Types of blank value determination and their settings - 141
U
Understanding the instrument and planning its use -
41
Understanding the operating software - 58
User administration - 81
Using the instrument - 117
V
Values for oxygen dosing - 135
Verify digital signature (Dialog) - 259
Versioning - 71, 72, 257
View > Graphic > Auto align (Command) - 283
View > Gridview > Auto align (Command) - 282
Operating instructions DuMaster D-480
352
View > Statistic > Auto align (Command) - 284
View > Toggle (Command) - 279
View menu - 278
Viewing calibration coefficients - 175, 303
Viewing list of defined factor, monitor and standard samples - 119, 174, 317
Viewing method settings - 129, 135, 323
Viewing the logbook - 90, 324, 325
Viewing the status of maintenance intervals - 168,
308
W
Waking up the instrument - 128
Warning: changes to the instrument - 23; residual risks - 19; unsuitable spare parts and consumables - 23
Warning notes during operation - 24, 76, 77, 82, 84,
85, 93, 94, 95, 110, 169, 171, 185, 188, 191, 198,
202, 207, 210, 211, 214, 215, 218, 221, 222, 223,
226, 228, 234, 235, 242, 308, 325, 330
Warning signs on the analyzer - 22
Warranty - 341
Warranty of the overall instrument - 342
Warranty on the furnace - 342
Ways of optimizing the use of the analyzer - 96
Weighing window (Dialog) - 285
What can you modify in the configuration? - 76, 328
What to do after a computer crash - 245
When does it make sense to edit analysis data? - 87
When to replace sealing elements - 195
Windows > Default layout (Command) - 334
Windows > Recent sample (Command) - 334
Windows > Status view (Command) - 334
Windows > Toolbar / Run-Bar (Command) - 333
Windows menu - 332
Work performed by the system administrator - 73
Working with documents - 159
Working with the database - 91
Working with the operating instructions - 18
Z
Zoom in/out (Dialog) - 279
©BÜCHI Labortechnik AG
Quality in your hands
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