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TitraLab
840 and 845
pH/EP/IP Titration Workstations
D21T062
Reference Manual
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D21T062 • Printed by Radiometer Analytical SAS • 2008-02C
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TitraLab
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TitraLab 840 and 845 Reference Manual
Contents
Contents..................................................................................................................3
Introduction ..........................................................................................................13
General Information .............................................................................................14
Starting up instructions.......................................................................................15
Read me! ...............................................................................................................16
Practical examples ..............................................................................................19
Programming electrodes ...........................................................................................21
Programming reagents .............................................................................................23
Programming methods ..............................................................................................25
Programming sequences ...........................................................................................29
Programming tips ................................................................................................31
Glossary ...............................................................................................................33
0IP (result indicator) ...................................................................................................35
Acceptance criteria ....................................................................................................35
Acceptation .................................................................................................................35
Access routine mode .................................................................................................36
Add method menu ......................................................................................................36
Add. reagent = Titrant ................................................................................................36
Addition .......................................................................................................................37
Addition volume .........................................................................................................37
Address .......................................................................................................................38
Address conflict (between electrode IDs) ................................................................38
Alarm: Locked .............................................................................................................38
Alarm: Unlocked .........................................................................................................39
Alphanumeric characters ..........................................................................................39
Amount unit ................................................................................................................39
Applied signal (AC/DC) ..............................................................................................40
Archives data lost - Cal. Data lost - Methods kept ..................................................40
Autochaining ...............................................................................................................40
Auxiliary input .............................................................................................................41
Auxiliary output ..........................................................................................................42
Aux. action / Aux. on for ............................................................................................42
Back reagent = Titrant ................................................................................................43
Back reagent unknown ..............................................................................................43
Back titration ...............................................................................................................43
Back titration - ID ........................................................................................................43
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Back titration No/Manual/Automatic .........................................................................43
Balance cables - A95Z201, A95Z202 .........................................................................44
Balance cables - A95Z204, A95Z205 .........................................................................45
Balance cables - A95Z206, A95Z207 .........................................................................46
Balance cables - A95Z208 ..........................................................................................47
Balance connection ....................................................................................................48
Balance in use ............................................................................................................49
Bar code reader connection ......................................................................................49
Beaker detection .........................................................................................................50
Beaker detection minimum height ............................................................................51
Beaker menu ...............................................................................................................52
Beakers: [F;L] .............................................................................................................53
Beep .............................................................................................................................53
Blank (Yes/No) ............................................................................................................53
Blank not required ......................................................................................................53
Blank on inflection no. ...............................................................................................53
Blank required ............................................................................................................53
Blank volume ..............................................................................................................54
Burette functions menu .............................................................................................54
Burette speed ..............................................................................................................54
Burette volume ...........................................................................................................55
Calculate with EP no. .................................................................................................55
Calculate with IP no. ...................................................................................................55
Calibrate electrodes ...................................................................................................55
Calibrate reagents ......................................................................................................55
Calibration delay elapsed ..........................................................................................55
Calibration parameters ..............................................................................................56
Calibration request .....................................................................................................56
Calibration results parameters ..................................................................................56
Calibration sequence .................................................................................................56
Calibration stack .........................................................................................................56
Catalogue list ..............................................................................................................56
Cell grounding ............................................................................................................57
Cell window .................................................................................................................57
Change electrode name .............................................................................................57
Change method name ................................................................................................58
Change reagent name ................................................................................................58
Change sequence name ............................................................................................58
Check command .........................................................................................................59
Check electrodes ........................................................................................................59
Check reagents ...........................................................................................................59
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Communication failure (SAC error) ..........................................................................60
Concentration .............................................................................................................60
Concentration unit ......................................................................................................60
Configuration menu ...................................................................................................60
Connections ................................................................................................................61
Continuous IP method ...............................................................................................62
Contrast .......................................................................................................................63
Controlled by TTL IN ..................................................................................................63
Copy electrode ............................................................................................................63
Copy method ...............................................................................................................64
Copy reagent ...............................................................................................................64
Coupled method .........................................................................................................65
Create electrode .........................................................................................................66
Create method ............................................................................................................66
Create reagent ............................................................................................................67
Current value ..............................................................................................................67
Curve ...........................................................................................................................67
Curves data lost - Cal. Data kept - Methods kept ....................................................67
Customise ...................................................................................................................68
Date entry ....................................................................................................................68
Default parameters .....................................................................................................68
Delay after addition ....................................................................................................69
Delete electrode ..........................................................................................................69
Delete method .............................................................................................................69
Delete reagent .............................................................................................................69
Delete sequence .........................................................................................................70
Demand: Locked .........................................................................................................70
Demand: Unlocked .....................................................................................................70
Derivative ....................................................................................................................70
Detailed ........................................................................................................................71
Direction ......................................................................................................................72
Direct measurements .................................................................................................72
Display contrast ..........................................................................................................72
Display measurement ................................................................................................73
Dyn. rinse ....................................................................................................................74
Dynamic dose .............................................................................................................75
Dynamic IP method ....................................................................................................76
Dynamic rinses ...........................................................................................................77
Edit electrode menu ...................................................................................................78
Edit method menu ......................................................................................................79
Edit reagent menu ......................................................................................................80
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Edit sequence menu ...................................................................................................81
Electrode calibration ..................................................................................................82
Electrode calibration (SAC sequence) .....................................................................83
Electrode calibration not required ............................................................................84
Electrode calibration parameters ..............................................................................84
Electrode calibration stack ........................................................................................85
Electrode connection .................................................................................................86
Electrode function ......................................................................................................87
Electrode icons ...........................................................................................................87
Electrode ID .................................................................................................................87
Electrode identification ..............................................................................................88
Electrode library .........................................................................................................88
Electrode not calibrated .............................................................................................88
Electrode system ........................................................................................................88
Electrode type .............................................................................................................89
Electrode window .......................................................................................................90
Electrodes are different .............................................................................................90
Empty burette .............................................................................................................90
Empty sequence .........................................................................................................90
End point .....................................................................................................................91
End point delay ...........................................................................................................91
End point method .......................................................................................................91
Enter titre .....................................................................................................................92
Equation formula ........................................................................................................93
Equation formula ........................................................................................................94
Equation - ID ...............................................................................................................94
Equation - unit ............................................................................................................95
Equivalent point determination (IP methods) ..........................................................96
Equivalent point determination (IP methods) ..........................................................97
ERR#32 (SAC error) ....................................................................................................98
Error messages ..........................................................................................................99
Error in equation formula ........................................................................................100
Excess reagent ID .....................................................................................................100
Excess titre ...............................................................................................................100
Excess volume ..........................................................................................................100
Fill burette .................................................................................................................101
Flush burette .............................................................................................................101
Format (printouts) ....................................................................................................101
Function ....................................................................................................................102
Fuses .........................................................................................................................102
Global flush burettes ................................................................................................103
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GLP-Archives menu .................................................................................................104
Ground conflict .........................................................................................................104
Help ............................................................................................................................104
High (result indicator) ..............................................................................................104
Icons ..........................................................................................................................105
ID ................................................................................................................................105
Increment ..................................................................................................................106
Inflection Point (IP) ...................................................................................................106
Insert method menu .................................................................................................106
Install burette ............................................................................................................107
Install reagent ...........................................................................................................108
Install reagent (with replacement) ..........................................................................109
Insufficient number of beakers ...............................................................................109
IP filter .......................................................................................................................110
IP reject ......................................................................................................................110
IP>1 (result indicator) ...............................................................................................110
Iso pH .........................................................................................................................111
Keyboard connection ...............................................................................................112
Language ...................................................................................................................113
Low (result indicator) ...............................................................................................113
Main window .............................................................................................................113
Mains frequency .......................................................................................................113
Max. stab reached ....................................................................................................114
Max. stab time ...........................................................................................................114
Max. volume ..............................................................................................................114
Max. vol - Predose > Bur. vol ...................................................................................114
Max. volume reached ...............................................................................................115
Maximum dose ..........................................................................................................115
Measurement ............................................................................................................115
Method .......................................................................................................................116
Method ID ..................................................................................................................116
Method library ...........................................................................................................117
Method parameters menu ........................................................................................117
Method results menu ...............................................................................................118
Method wrong type ...................................................................................................118
Min. ordinate Max. ordinate .....................................................................................119
Min. ordinate Max. ordinate - Blank ........................................................................120
Min. pH0(25) - Max. pH0(25) .....................................................................................120
Min. sensitivity - Max. sensitivity ............................................................................120
Min. speed - Max. speed ..........................................................................................121
Min. Temp. - Max. Temp. ..........................................................................................121
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Missing beaker (SAC error) .....................................................................................122
Missing EP ................................................................................................................122
Missing IP ..................................................................................................................122
Mode ..........................................................................................................................122
Molar weight ..............................................................................................................123
Monotonic IP method ...............................................................................................123
Nb lines per page (printouts) ...................................................................................124
No active electrode defined in "method ID" ...........................................................124
Notification message ...............................................................................................124
Number of buffers ....................................................................................................124
Number of decimals .................................................................................................125
Number of digits .......................................................................................................125
Number of dynamic rinses ......................................................................................125
Number of EP ............................................................................................................125
Number of equations ................................................................................................126
Number of IP .............................................................................................................126
Number of results .....................................................................................................126
Number of static rinses ............................................................................................127
Number of tests ........................................................................................................127
OK (result indicator) .................................................................................................128
Others list ..................................................................................................................128
Parameters menu .....................................................................................................128
PC cable - A95X501 ..................................................................................................128
PC connection ..........................................................................................................128
PC keyboard ..............................................................................................................129
Periodicity .................................................................................................................129
pH0(25) ......................................................................................................................129
pH buffer ....................................................................................................................129
pH calibration results parameters ..........................................................................130
pH calibration solutions parameters ......................................................................130
pH int .........................................................................................................................130
Potential versus SHE ...............................................................................................131
Predose mode, Predose until ..................................................................................132
Preprogrammed list ..................................................................................................132
Printer ........................................................................................................................133
Printer = LIMS (XML) ................................................................................................133
Printer cables - A95P201, A95X506 .........................................................................134
Printer connection ....................................................................................................135
Print in table ..............................................................................................................135
Printouts ....................................................................................................................136
Printouts detailed .....................................................................................................137
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Printouts menu .........................................................................................................137
Printouts setup .........................................................................................................137
Printouts title ............................................................................................................138
Programming method ..............................................................................................138
Programming sequence ...........................................................................................139
Proportional band .....................................................................................................140
Reaction X Exc. + Y Titr ...........................................................................................141
Reaction X Smp + Y Titr ...........................................................................................142
Reaction X Smp + Y Exc ..........................................................................................143
Reaction X Std + Y Titr ............................................................................................144
Reagent addition ID .................................................................................................144
Reagent addition volume .........................................................................................145
Reagent calibration ..................................................................................................145
Reagent calibration (SAC sequence) ......................................................................146
Reagent calibration not required ............................................................................146
Reagent calibration parameters ..............................................................................147
Reagent calibration stack ........................................................................................148
Reagent icons ...........................................................................................................149
Reagent ID .................................................................................................................149
Reagent identification ..............................................................................................150
Reagent library .........................................................................................................150
Reagent not calibrated .............................................................................................150
Reagent system ........................................................................................................150
Reagent titre not entered .........................................................................................150
Reagent unit ..............................................................................................................151
Reagent window .......................................................................................................151
Recalculate results ...................................................................................................152
Remove burette ........................................................................................................153
Remove method from a sequence ..........................................................................153
Remove reagent ........................................................................................................154
Replace burette .........................................................................................................155
Replace reagent ........................................................................................................156
Reset memory ...........................................................................................................156
Reset to factory settings ..........................................................................................156
Result accepted (Yes/No) ........................................................................................156
Result ID ....................................................................................................................156
Result indicators ......................................................................................................157
Result unit .................................................................................................................157
Results .......................................................................................................................158
Results by difference/cumulate ..............................................................................158
Results factor (Yes/No) ............................................................................................159
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Results menu ............................................................................................................160
Rinse time .................................................................................................................160
Routine mode ............................................................................................................161
Run window ..............................................................................................................161
Running a method (preliminary steps) ...................................................................162
Running a method
(steps 6 to 9) 163
Running a method (steps 10 to 12) .........................................................................164
Running a method (last steps) ................................................................................165
Running a sequence with a sample changer .........................................................166
SAC arm obstructed (SAC error) ............................................................................166
SAC ext. cell GND .....................................................................................................167
SAC option missing (SAC error) .............................................................................167
SAC switch Off/On (SAC error) ...............................................................................167
SAC80/SAC850 .........................................................................................................167
Same buffer change buffer ......................................................................................168
Sample amount .........................................................................................................168
Sample changer ........................................................................................................169
Sample changer cable - A95A202 (SAC80) ............................................................170
Sample changer cable - A95X501 (SAC850) ..........................................................170
Sample ID ..................................................................................................................171
Sample menu ............................................................................................................171
Sample preparation no. ............................................................................................172
Sample Run Start/Run End (Standard/Shortcut) ...................................................173
Sample stack .............................................................................................................174
Sample unit ...............................................................................................................174
Sample unit conflict .................................................................................................174
Select electrode ........................................................................................................175
Select method ...........................................................................................................175
Select reagent ...........................................................................................................175
Select sequence .......................................................................................................175
Sensitivity ..................................................................................................................175
Sequence/SAC sequence ........................................................................................176
Sequence/Sample stack menu ................................................................................177
Sequence end in Park (Yes/No) ...............................................................................177
Sequence ID ..............................................................................................................177
Serial number (burette) ............................................................................................178
Setup menu ...............................................................................................................178
Skip empty position .................................................................................................179
Smoothing parameter ..............................................................................................180
Software version .......................................................................................................180
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Solution menu ...........................................................................................................181
Speed .........................................................................................................................182
Stability ......................................................................................................................182
Standard amount ......................................................................................................182
Standard ID ...............................................................................................................183
Standard menu .........................................................................................................183
Start timer ..................................................................................................................184
Static rinses ..............................................................................................................184
Static rinse time ........................................................................................................184
Statistics ....................................................................................................................184
Stirring .......................................................................................................................185
Stoichiometric coefficients ......................................................................................186
Stop after last IP .......................................................................................................186
Stop analysis ............................................................................................................186
Stop point ..................................................................................................................187
Supervisor code .......................................................................................................188
Supervisor mode ......................................................................................................189
Target titre .................................................................................................................189
Temperature Probe/ Fixed at 25°C/Entered ............................................................189
Temperature sensor ID ............................................................................................190
Test amount ..............................................................................................................190
The sequence is empty ............................................................................................190
TIM cell external Gnd ...............................................................................................191
Time max (result indicator) ......................................................................................191
Title ............................................................................................................................191
Titrant ID ....................................................................................................................191
Titre Enter/Calibrate .................................................................................................192
Tray missing (SAC error) .........................................................................................192
TTL 5 V OUT (sockets) ............................................................................................192
TTL IN (sockets) .......................................................................................................193
Turntable blocked (SAC error) ................................................................................193
Type of method .........................................................................................................193
User ID (Yes/No) .......................................................................................................194
User list .....................................................................................................................194
User’s rights ..............................................................................................................194
Volume .......................................................................................................................195
Wrong buffer .............................................................................................................195
Wrong type (SAC error) ...........................................................................................195
Zero pH ......................................................................................................................195
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Appendixes ........................................................................................................197
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Appendix 1: Preprogrammed methods ..................................................................199
Appendix 2: General information ............................................................................201
Appendix 3: Result calculations .............................................................................205
Appendix 4: Technical specifications ....................................................................211
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Introduction
The TitraLab 840 and 845 Titration Workstations are dedicated for routine use. They offer two
distinct user levels:
• Supervisor
Dedicated for operators who wish to edit their methods to fit their specific needs. They can
also assign a password to protect the programmed data from eventual changes.
•Routine
Dedicated for operators wishing to use the routine functions to guide them step by step
through the analyses.
The TIM840 and TIM845 can store up to 10 methods, 15 electrodes and 15 reagents.
Thanks to the preprogrammed applications, the Titration Manager is ready for use as soon as
it has been installed. Refer to "Appendix 1: Preprogrammed methods", page 199.
The TIM840 and TIM845 also allow you to automatically sequence and repeat measurements
- ideal for direct measurements followed by a titration.
The purpose of the TitraLab 840 and 845 Reference Manual is to give detailed information on
the Titration Workstation and the data displayed during operations. The information is listed in
alphabetical order for quick access and cross-references are listed in italics.
In addition to this handbook, a general User’s Guide (part no. D21T065) is available giving
descriptions and overviews of the workstation menus and operating concepts to guide you
through programming and running of the analyses.
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General Information
Safety Information
Please read this entire manual before unpacking, setting up, or operating this equipment.
Pay attention to all danger and caution statements. Failure to do so could result in serious injury
to the operator or damage to the equipment.
To ensure that the protection provided by this equipment is not impaired, do not use and do not
install this equipment in any manner other than that specified in this manual.
Precautionary Labels
Read all labels and tags attached to the instrument. Personal injury or damage to the
instrument could occur if not observed.
This symbol, if noted on the instrument, references the instruction manual
for operation and/or safety information.
Electrical and electronical equipment marked with this symbol may not be
disposed of in European public disposal systems after 13 August of 2005.
In conformity with European local and national regulations (EU Directive
2002/96/EC), European electrical equipment users must now return old
or end-of life equipment to the Producer for disposal at no charge to the
user.
Note: For equipment supplied or produced by "Radiometer Analytical",
please contact www.hach-lange.com and select your country for instructions on how to return your equipment for proper disposal."
This symbol, when noted on the product, identifies the location of a fuse
or current limiting device.
Warning!
The TitraLab 840 and 845 have been developed to meet the requirements of volumetric
titration applications. It is therefore aimed at experienced users who have the knowledge
required to operate the instrument and implement the security instructions enclosed.
Please remember that the Titration Manager must not, under any circumstances, be used
to perform tests on living beings.
We accept no responsibility for using theTitration Manager and its peripheral
devices under conditions that are not specified in this Reference Manual and its associated
User’s Guide (part no. D21T065).
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Starting up instructions
Set up the instrument in a properly ventilated place. The power supply connector on the rear
panel must remain accessible and close to the user (2 m maximum) so that you can quickly
disconnect the cables in case of emergency.
The room temperature must be between 5 and 40°C.
The relative humidity must be between 20 and 80°C.
To a mains supply socket
Connect the mains socket of the Titration Manager to the mains supply using the 3-lead power
cord provided. The Titration Manager must be connected to an earthed mains socket for safety
reasons. Efficient grounding is essential for reliable measurements and security.
In the USA or Canada, use a UL listed power cord only.
Switch on the Titration Manager (O/I power switch set to "I")
The Titration Manager displays during a few seconds an identification screen (name and
embedded software version) followed by the Main window, see "Main window", page 83.
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Read me!
An important feature of this Titration Manager interface is that it controls the presence of different elements necessary to run the defined application for a selected method/sequence, before
the method/sequence is run.
Working in Supervisor mode
A Supervisor has access to all the libraries for creation purposes.
When programming the Titration Manager in “SUPERVISOR” mode, it is recommended to
work in stages. These stages must be carried out in the order described below:
A.To program method
1.Define your electrode(s)
Identify electrodes (including temperature sensors) to be used for the analysis:
Electrodes can be created from the following lists:
Catalogue, see "Catalogue list", page 56.
Other, see "Others list", page 128.
Copy from, see "Copy electrode", page 63.
When creating the electrode, define if electrode calibration is required (or not), if yes specify
the "periodicity" of the calibrations and the pH standards to be used. Refer to "Calibrate elec-
trodes", page 55.
2. Define reagent
Identify reagents to be used for the analysis
Reagents can be created from the following lists:
Catalogue, see "Catalogue list", page 56.
Other, see "Others list", page 128.
Copy from, see "Copy reagent", page 64.
When creating the reagent, define if reagent calibration is required (or titre entered manually),
if yes specify the "periodicity" of the calibrations and the calibration method. Refer to "Reagent
calibration", page 145.
If a sample changer is to be used, define the sample changer in the Configuration menu before
programming a SAC sequence.
If you are to perform a calibration, make sure that the electrode(s) used for the calibration are the same as those used in the method.
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3. Create new method or Edit a pre-programmed one
Create the measurement or titration method to be used for the analyses. Enter the parameters
required to calculate the results, see "Programming methods", page 25.
When you have finished programming, select the method or pre-programmed application, see
"Select method", page 175.
If you are using a sample changer, edit the sequence and program the sample stack, see
"Sample stack", page 174.
4. Check icons
The following icons indicate the exact state of your working system:
Sunny icon:
Everything is OK. Run the method or sequence.
Cloudy icon:
Electrode/reagent calibration required within 12 or 24 hours.
Stormy icon:
Electrode/reagent calibration date elapsed or reagent(s) not installed.
Question mark:
Programming error.
Refer to "Electrode icons", page 87.
Refer to "Reagent icons", page 149.
Sunny icons are needed in order to run the selected method.
If Cloudy/Stormy/Question mark icons are displayed in the Reagent/Electrode window
press 1 to activate the “Check” command. The Titration Manager will automatically
guide you through the operations required to solve the errors encountered.
B.Running methods
To run a method or sequence, see "Working in Routine mode", page 18.
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Working in Routine mode
A.Access methods
A Routine operator has access to all screens for checking purposes
B.Running methods
When working in “ROUTINE” mode, it is necessary to install your titration system according to
the selected method or sequence, prior to running a method or sequence.
1. Select the method or sequence
Refer to "Select method", page 175.
Refer to "Select sequence", page 175.
2. Connect the electrodes
Refer to "Electrode connection", page 86.
3. Check icons
Refer to "Check icons", page 17.
Depending on the icons displayed, the Titration Manager will automatically guide you through
the steps necessary to run the analysis, see below:
a. Install reagents(s)
Check that the burette is installed, if not, see "Install burette", page 107.
Now, install the reagent, see "Install reagent", page 108.
b. Calibrate electrode(s)
Now, run the calibration, see "Calibrate electrodes", page 55.
c. Calibrate reagent(s) or Enter titre
Now, run the calibration or enter the titre.
Refer to "Reagent calibration", page 145.
Refer to "Enter titre", page 92.
d. Run the method or the sequence
Refer to "Running a method (preliminary steps)", page 162.
Refer to "Running a sequence with a sample changer", page 166.
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Practical examplesxamples
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Programming electrodes
1.
Press 4.
4.
2.
Press 1.
5.
3.
Select Function.
Select ID.
6.
Select ID from Catalogue or
Others list.
Press 1 to confirm.
Press 1 to confirm the creation
of the new electrode.
For a combined or a simple
electrode or for a reference
electrode, enter the potential (in
mV) of the reference versus the
Standard Hydrogen Electrode
(SHE).
For a combined or a simple
electrode if you have selected
the Others list, enter the internal pH of the electrode.
Enter the address of the electrode.
Select Yes if a calibration is required, go to step 7.
Select No, for no calibration,
press Esc to leave the menu.
Programming is completed.
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7.
Enter the calibration parameters.
10.
8.
Press 1.
11.
9.
Enter the electrode calibration
parameters. Press Esc then 2.
12.
Select the buffer solutions
used. Press Esc then 3.
Enter the results parameters.
Press Esc then 4.
Enter the printouts parameters.
Press Esc twice. Electrode
programming is completed.
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Programming reagents
1.
Press 5.
4.
2.
Press 1.
5.
3.
Press ✓.
6.
Select ID from Catalogue list or
Others list.
Enter the target titre and unit.
Press 1 to confirm.
Confirm the creation of the
new reagent.
Enter the burette address
(TIM845 only).
Select Titre = Calibrate if a
calibration is required, go to
step 7.
Select Titre = Enter to enter
the titre manually. Press Esc
to leave the menu.
Programming is completed.
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7.
Enter the calibration parameters.8.Press 1.
10.
11.
9.
Select the electrode used for
the calibration. This electrode
must be the one defined in
the method using this
reagent. Enter the calibration
parameters.
Press Esc then 2.
12.
Enter the parameters of the
standard used for the calibration.
Press Esc then 3.
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Enter the Results parameters. Press Esc then 4.
Enter the printouts
parameters. Press Esc twice.
Reagent programming is
completed.
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Programming methods
Creating and editing a method
1.
Press 5.
4.
2.
Press 1.
5.
3.
Enter ID.
Press 1 to confirm.
6.
Enter method parameters.
Specify the Mode, see "Mode",
page 122.
Press 1.
Press ✓ and select the
electrode(s) from the list(s).
Do not forget to select
the same electrode(s)
as the one(s) created in the
reagent calibration method.
Enter the other method
parameters. Press Esc then 2.
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TitraLab
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TitraLab 840 and 845 Reference Manual
7.
Enter the Sample parameters.
Press Esc then 3.
8.
Enter the results parameters.
Press Esc then 4.
9.
Enter the printouts parameters.
Press Esc twice. Method programming is completed.
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TitraLab
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For a Coupled method
TitraLab 840 and 845 Reference Manual
1.
Press 5.
4.
2
Press 1.
3.
Enter the Method ID and press
1 to confirm.
Select Mode = Coupled.
Enter the 2 methods to be
linked. Press Esc twice.
Method programming is
completed.
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TitraLab
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TitraLab
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TitraLab 840 and 845 Reference Manual
Programming sequences
A sequence (or SAC sequence) is a sequence of methods with automatic change of the beakers. A
sample changer (SAC80 or SAC850) is used.
1.
Press Stop for 3 seconds to
enter the SETUP menu.
4
2.
Press 1.
5.
3.
Select a Sample Changer
(SAC80 or SAC850). Enter the
parameters of the sample
changer selected (number of
rinses, rinse time, etc.).
Press Esc then 5 (Exit) to quit
the Setup menu.
Press 3.
Enter a name for the sequence.6.Press 3.
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TitraLab
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TitraLab 840 and 845 Reference Manual
7.
Press 1 to add a method.
10.
8.
Select the type of method.
11.
9.
Select a method in the list of
available methods.
12.
Press 1 to add the method to
the sequence.
If Sample has been selected in
step 8, enter the number of
samples (number of times you
wish to repeat the method in
the sequence).
If a SAC850 has been selected
in step 3, enter the sample
preparation number.
Press 1 to add a second
method to the sequence.
Repeat steps 8 to 11.
3 methods can be chained in a
sequence.
After having added the last
method, press Esc twice.
Sequence programming is
completed.
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TitraLab
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TitraLab 840 and 845 Reference Manual
Programming tips
• Do not forget to declare electrode(s) while setting up reagent parameters, if calibrated.
• Do not forget to declare electrode(s) and reagents(s) when programming your method
parameters
• If reagents are calibrated, the same electrode must be used in both sample analysis
method and reagent calibration.
• If a Sample Changer is used, do not forget to declare one in the Configuration menu.
If no sun icons appear after the method has been selected, check the following points:
1. Install reagent(s) for selected method, see "Install reagent", page 108.
2. If required, calibrate electrode, see "Calibrate electrodes", page 55.
3. Calibrate/enter reagent titre,
see "Calibrate reagents", page 55,
see "Enter titre", page 92.
If Sunny icons appear
These are required to run the selected method.
If the Cloudy icon appears:
The electrode/reagent calibration should be performed within 24 hours.
This is a simple warning, it will not stop you from running the analysis.
If the Stormy icon appears:
Titrant required in the selected method is not installed or has not been calibrated.
Electrode required in the selected method has not been calibrated.
If the Question mark icon appears:
It is a programming error, reagent and/or electrode is/are not defined in the
selected method. Revise the method programming.
When a Stormy or a Question mark icon appears, press 1 “Check” . The Titration
Manager will automatically guide you through the operations necessary to solve
the errors encountered.
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TitraLab
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Page 33
Glossary
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TitraLab
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TitraLab 840 and 845 Reference Manual
0IP (result indicator)
Acceptance criteria
Refer to "Result indicators", page 157.
Acceptance criteria = Yes
Enables the user to enter preset minimum and maximum values for
measurement results of a pH electrode calibration. If the result lies
outside these values an alarm message appears and the results are
rejected by the instrument.
Therefore, acceptance limits can be set on:
• the response slope of a pH electrode,
see "Min. sensitivity - Max. sensitivity", page 120.
• the pH0 of a pH electrode,
see "Min. pH0(25) - Max. pH0(25)", page 120.
• the pH buffer measurement temperature,
see "Min. Temp. - Max. Temp.", page 121.
Acceptance criteria = No
The measurement results of a pH electrode calibration are accepted
irrespective of the values found.
Acceptation
Enter in:
Edit electrode > Results
Result acceptance time limit.
When the time entered for the Acceptation has elapsed the
measurement will be accepted whether stable or not.
For the signal to be accepted once the Acceptation has
elapsed, the Max. Stab. time must be greater than the Accep-
tation time.
Enter in:
Edit method > Parameters menu
Edit reagent > Calibration parameters menu
Edit electrode > Calibration parameters menu
Range available:
0 to 59:59 min:s
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TitraLab
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TitraLab 840 and 845 Reference Manual
Access routine mode
Add method menu
Press Stop for 3 seconds from the Main window then press 2.
These rules can be set by the Supervisor to allow the routine user
access to certain operations.
Enter in:
Setup menu > Access routine mode
Use this menu to set the ID and type of method to be added to a
sequence.
Add. reagent = Titrant
Page 36
In the title bar, x/y (eg. 1/1) indicates the position "x" of the method in
the sequence and "y" the total number (1 to 3) of methods in the
sequence.
To access:
Press 1 in the Edit sequence menu.
The reagent used for addition is the same as the titrant used for the
titration.
Press ✓ and define an addition reagent different from the titrant in the
Parameters screen of the method.
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TitraLab
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TitraLab 840 and 845 Reference Manual
Addition
Addition volume
Option available with TitraLab 845.
Select Yes to carry out a reagent addition at the start of the titration or
a reagent calibration. This addition takes place before the titration
starts (predose included).
The reagent is added using a second burette controlled by the Titration
Manager. This second burette is installed on the Titration Manager.
Use a sample preparation when you want to add a solvent
using a pump installed on a SAC850 Sample Changer. Refer
to "Sample preparation no.", page 172.
Enter in:
Edit method > Parameters
Edit reagent > Calibration parameters
Refer to "Reagent addition volume", page 145.
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TitraLab
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Address
The position where the electrode and burette are placed during
operation:
Electrode address
The electrode address is defined using the format “TIM/y” where “TIM”
corresponds to the instrument (TIM840 or TIM845) where the
electrode is connected and “y” corresponds to the socket.
For example TIM/E1, indicates that the electrode is connected to E1
socket on the Titration Manager.
Refer to "Electrode connection", page 86.
Burette address (Option available with TitraLab 845)
The burette address is defined using the format “TIM/y” where “TIM”
corresponds to the TIM845 Titration Manager where the burette is
placed and “y” corresponds to the position.
For example TIM/1, indicates that the burette is placed on the TIM845
in position 1.
Position 2
Position 1
Address conflict (between electrode IDs)
Alarm: Locked
Figure 1: Burette positions
Two electrodes have been defined at the same address.
Enter the Edit electrode menu and modify the address of one of the
electrodes.
The user cannot bypass an electrode calibration if the last result
obtained lies outside the acceptance range.
Enter in:
Setup menu > Access routine mode
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TitraLab
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TitraLab 840 and 845 Reference Manual
Alarm: Unlocked
Alphanumeric characters
Enables the user to bypass an electrode calibration if the last result
obtained lies outside the acceptance range.
Enter in:
Setup menu > Access routine mode
The following alphanumeric characters can be obtained using the
Titration Managers Keypad:
Keys Characters
7 7, A, B, C, a, b, c, @
8 8, D, E, F, d, e, f
9 9, G, H, I, g, h, i
4 4, J, K, L, j, k, l
5 5, M, N, O, m, n, o, µ
6 6, P, Q, R, p, q, r
1 1, S, T, U, s, t, u
Amount unit
2 2, V, W, v, w
3 3, X, Y, Z, x, y, z
0 0, -, +, *, ^, =, #, <, >, .
space, /, (, ), [, ], |, ?, !, %, °
Table 1: Entering alphanumeric characters
Unit of the amount of standard used to calibrate the titrant. The
standard can be expressed as a weight (g or mg) or a volume
(ml or µl).
Enter in:
Edit reagent > Standard
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TitraLab
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TitraLab 840 and 845 Reference Manual
Applied signal (AC/DC)
Archives data lost - Cal. Data lost - Methods kept
Autochaining
Specifies the current type (alternative AC or direct DC) to be sent to
the Pt-Pt socket on the Titration Manager. The AC signal frequency is
1.67 Hz. This option is available if mV(i>0) has been selected for
Measurement in the Edit method or Edit reagent menus.
Enter in:
Method parameters menu
Reagent parameters menu
Instrument internal failure. Only the method parameters have been
kept.
This option is valid for a Coupled method which is not part of a
sequence.
Autochaining = No
At the end of each method run, you must confirm the result in order to
perform the next method. If a Notification message has been
selected, a message is displayed between each method of the Coupled method.
Autochaining = Yes
At the end of each method run, The methods are chained
automatically in the Coupled method. If a Notification message has
been selected, a message is displayed upon starting the first method
(no message is displayed after).
Refer to "Notification message", page 124.
Enter in:
Edit method menu (for a Coupled method)
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TitraLab 840 and 845 Reference Manual
Auxiliary input
The auxiliary input socket can be connected to an external device unit
used to send an analysis start command to the Titration Manager. The
analysis is a method with manual change of the titration beakers (no
sample changer used).
The external device unit is to be connected to the red and black IN
banana sockets of the Titration Manager. The red banana socket
receives the TTL 0 ± 5 V auxiliary signal and the black banana socket
is connected to the instrument electrical zero.
Proceed as follows to trigger a sequence of methods by an auxiliary
signal input:
• In the Configuration menu, select
Controlled by TTL IN = Yes.
• Connect the auxiliary control unit to red and black IN banana
sockets of the Titration Manager.
• Run the sequence. The Titration Manager displays a waiting for
auxiliary signal message. The sequence is started as soon as the
auxiliary signal is received.
Spécifications of the auxiliary input signal
Refer to "TTL IN (sockets)", page 193.
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TitraLab
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TitraLab 840 and 845 Reference Manual
Auxiliary output
The auxiliary outputs are used to control external equipment such as
valves or pumps during titrations. This signal is sent between the red
and black banana sockets 5 V OUT of the Titration Manager.
Auxiliary output (5 V, No)
Activate to 5 V or disable the auxiliary signal.
Specifications of the auxiliary ouput signal:
see "TTL 5 V OUT (sockets)", page 192.
Aux. action
Titration start
The auxiliary signal is initiated at titration start (before predose if relevant). Duration is set by Aux. on for.
Titration end
The auxiliary signal is initiated at titration end. Duration is set by
Aux. on for.
Whole titration
The auxiliary signal is initiated at titration start (before predose if relevant), and lasts the whole titration.
Aux. on for
Aux. action / Aux. on for
Time during which the auxiliary signal is set to 5 V when the
Titration start or Titration end is selected for
Aux. action.
Enter in:
Method parameters menu
Reagent parameters menu
Range available:
Aux. on for: 0 to 99:59 min:s
Measurement method:
The Aux. action parameter is not available in a
Measurement method. An auxiliary output can be activated:
•at the measurement start (duration set by Aux. on for)
•or during the whole measurement including measurement
stabilisation delay. In this case, select a 5 V auxiliary output
and set Aux. on for = 0.
Refer to "Auxiliary output", page 42.
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Back reagent = Titrant
Back reagent unknown
Back titration
Back titration ID
The reagent used for the back titration is the same as the titrant used
for the titration.
Press ✓ and define a back reagent different from the titrant in the
Parameters screen of the method.
The method uses a back reagent which has not been defined.
Press ✓ and enter a back titration ID in the Parameters screen of the
method.
An excess of reagent is added to the sample and after a short time, the
excess is then back-titrated using the titrant.
In volumetric analysis, back titrations are useful when a direct titration
runs too slowly.
Name of the excess reagent to be added during the titration. This
name is entered directly using the keypad (max. 20 alphanumeric
characters), with the unit (mM, M, mN or N).
Back titration No/Manual/ Automatic
Enter in:
Edit method > Parameters menu (back titration method)
Back titration = No
This is a direct titration.
Back titration = Manual
This is a back titration where the excess reagent is added using a
separate burette or a pipette not controlled by the Titration Manager.
This reagent is defined using its titre and volume in the Parameters
screen. This reagent is not selected in the Reagent library.
Back titration = Automatic
Option available with TitraLab 845.
This is a back titration where the excess reagent is added using a
second burette controlled by the Titration Manager. This second
burette is installed on the Titration Manager.
The excess reagent is created or selected from the User list.
Enter in:
Edit method > Parameters menu
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TitraLab
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Balance cables A95Z201,
A95Z202
TitraLab 840 and 845 Reference Manual
1 m
Titration
Manager
Balance
socket
A95Z201
BALANCE
METTLER
1
RxD
2
3
TxD
4
DTR
5
GND
6
DSR
RTS
7
8
CTS
9
DTE
Female 9-pin
Figure 2: Balance cable, A95Z201
1 m
Titration
Manager
Balance
socket
A95Z202
1
TxD
3
RxD
2
CTS
5
7
GND
4
RTS
DSR
6
20
DTR
DCE
Male 25-pin
BALANCE
SARTORIUS
1
RxD
2
3
TxD
DTR
4
5
GND
6
DSR
RTS
7
CTS
8
9
DTE
Female 9-pin
Figure 3: Balance cable, A95Z202
1
TxD
2
RxD
3
CTS
5
7
GND
Gnd
4
Return
20 DTR
25
DTE
Male 25-pin
Page 44
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TitraLab
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Balance cables A95Z204,
A95Z205
TitraLab 840 and 845 Reference Manual
2 m
Titration
Manager
Balance
socket
A95Z204
BALANCE
SARTORIUS
1
RxD
2
3
TxD
DTR
4
5
GND
6
DSR
RTS
7
CTS
8
9
DTE
Female 9-pin
Figure 4: Balance cable, A95Z204
2 m
Titration
Manager
Balance
socket
RxD
TxD
1
2
3
A95Z205
1
TxD
2
RxD
3
CTS
5
7
GND
Gnd
4
Return
20 DTR
25
DTE
Male 25-pin
BALANCE
METTLER
1
TxD
3
RxD
2
4
DTR
5
GND
6
DSR
RTS
7
8
CTS
9
DTE
Female 9-pin
Figure 5: Balance cable, A95Z205
CTS
5
7
GND
4
RTS
DSR
6
20
DTR
DCE
Male 25-pin
Page 45
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TitraLab
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Balance cables A95Z206,
A95Z207
TitraLab 840 and 845 Reference Manual
1 m
Titration
Manager
Balance
socket
A95Z206
BALANCE
METTLER
Female 9-pin
RxD
2
3
TxD
4
DTR
5
GND
6
DSR
RTS
7
CTS
8
9
DTE
Figure 6: Balance cable, A95Z206
1.20 m
Titration
Manager
Balance
socket
RxD
TxD
1
2
3
A95Z207
TxD
12
RxD
2
CTS
3
13
GND
METTLER PLUG
15-pin
BALANCE
PRECISA
1
TxD
2
RxD
3
Page 46
4
DTR
5
GND
6
DSR
RTS
7
CTS
8
9
DTE
Female 9-pin
Figure 7: Balance cable, A95Z207
CTS
5
7
GND
4
RTS
25
20
DTR
DTE
Male 25-pin
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TitraLab
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Balance cables A95Z208
TitraLab 840 and 845 Reference Manual
1 m
Titration
Manager
Balance
socket
RxD
TxD
DTR
GND
DSR
RTS
CTS
1
2
3
4
5
6
7
8
A95Z208
BALANCE
PRECISA
1
TxD
2
3
4
5
GND
6
RxD
7
8
9
DTE
Female 9-pin
Figure 8: Balance cable, A95Z208
RJ45
Male 8-pin
Page 47
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TitraLab
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TitraLab 840 and 845 Reference Manual
Balance connection
Connect the balance to the Titration Manager using the cable corresponding to the type of balance used, see table below:
Balance Type Cable Length
Mettler PE + option 016
AE + option 012 or 011
AM, PM, SM, AT, MT,
A95Z201
A95Z205
1 m
2 m
A95Z206 1 m
UMT, PJ, AJ
Sartorius MasterPro, QC, MP8-4
BP110S, CT224S,
LE244S-OCE
A95Z202 1 m
A95Z204 2 m
Precisa All models (except XB220) A95Z207 1 m
XB220 A95Z208 1 m
Table 2: Balance types
Cables can be made to your desired specifications. Please contact our
sales representative if you require information regarding the type of
cable to use with your balance.
Format of messages accepted by the Titration Manager:
•Messages end: LF or CR, LF+CR,
• Units, g, mg, kg,
• The character “g” of the unit is required to mark the end of the data
recognised by the instrument,
• Spaces are ignored,
• The number of characters situated between the first character in the message and the “g” in the unit must not be more than 30, (spaces not
included),
• The number of characters received after the “g” and before the end of the
message LF, is insignificant,
• The numeric data of the weight must be transmitted before the unit.
RS232C parameters (to set on the balance):
2400 baud, even parity, 7 data bits and 1 stop bit
Example of a message transferred from a balance, type Mettler
SI 12.3456 gCRLF
data received: 12.3456 g
Page 48
The units selected in the Titration Manager must be identical to the
units used by the balance.
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TitraLab
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TitraLab 840 and 845 Reference Manual
Balance in use
When using a balance connected to the Titration Manager, proceed
as follows:
1. Press 1 to run the method.
2. If required, enter a User ID, confirm.
3. If required, enter a Sample ID.
4. Place the sample in the sample container.
5. Place the sample container on the balance and set the balance to
zero “tare”.
6. Introduce the sample into the titration cell.
7. Weigh the “empty” sample container
8. Press ✓ in the field Test 1.
Bar code reader connection
9. Press ✓ to accept the sample amount.
10. Press 1 to continue the titration.
Make sure that the sample amount unit is expressed in g or
mg.
Connect a bar code reader to the Titration Manager via the 6-pin mini
DIN port situated on the right hand side of the instrument.
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Beaker detection
On a SAC850 sample changer, a Beaker detection module (ultrasonic
transducer) makes it possible to detect beakers containing liquid
sample with a height higher than the minimum detection limit
(10 mm), see "Beaker detection minimum height", page 51.
In all other cases, the beaker positions are not detected, that is to say:
a. empty positions (positions not occupied by beakers),
b. empty beakers or beakers considered as empty (i.e. beakers
with heights of liquid less than the minimum detection limit),
c. beakers containing solid or powder samples.
In case of a position not detected, you can ask the workstation to
jump the position (analysis not performed on that position): tick both
options Beaker detection and Skip empty posi-
tion. Refer to "Skip empty position", page 179
The option Beaker detection
If you tick the option Beaker detection, then you can ask the
workstation to jump or not the positions which will be not detected
(depending on your selection for the option Skip empty posi-
tion).
If you clear the Beaker detection option, the ultrasonic transducer is disabled. All the positions between the first and the last
beaker of the sample stack (including the static rinse and park
beakers) will be regarded as occupied by a beaker.
Thus, place beakers on all these positions. In this case, the Skip
empty position option is not available (option is greyed).
Enter in:
Setup menu > Configuration
If Sample changer = SAC850
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TitraLab 840 and 845 Reference Manual
Beaker detection minimum height
The table below reports the minimum height of liquid that must be
present in the beaker in order to detect the beaker as not empty, see
also "Beaker detection", page 50.
Beaker type
diameter x height (mm)
400 ml tall form 70 x 131 10 mm (40 ml)
250 ml low form 70 x 95 10 mm (40 ml)
250 ml tall form 60 x 120 10 mm (30 ml)
125 ml, Gosselin, PP,
54 x 73
180 ml, Gosselin, PP,
54 x 103
150 ml tall form 60 x 80 10 mm (30 ml)
150 ml low form 62 x 81 10 mm (30 ml)
40-100 ml, PP 60 x 80 10 mm (30 ml) 904-490 (pack of 50)
100 ml tall form 48 x 80 10 mm (20 ml)
Detection minimum
height
10 mm (25 ml) X31T087 (pack of 50)
10 mm (25 ml) X31V005 (pack of 50)
Part no.
50 ml low form 42 x 60 10 mm (15 ml) 904-489 (pack of 50)
22-45 ml, PP 44 x 70 10 mm (15 ml) 904-489 (pack of 50)
8-25 ml, PP 44 x 70 10 mm (15 ml) 904-488 (pack of 50)
Page 51
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TitraLab
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TitraLab 840 and 845 Reference Manual
Beaker menu
Use this menu to prepare a sample or calibration stack. This menu
defines individual data for all the samples or standards used in the
sequence.
Figure 9: Beaker menu (for a sample stack)
To access (for a sample stack):
1. Press 3 Sequence/Sample stack in the Main window.
A Sample Changer must be declared in the Configuration
menu. Refer to "Sample changer", page 169.
2. Press 1 Sample stack.
The sequence must have been edited in the Edit sequence
menu. Refer to "Edit sequence menu", page 81.
Refer to "Sample stack", page 174.
To access (for a reagent calibration stack):
1. In the Reagent window, press 1 Calibrate/Enter titre.
2. Press 3 Calibration sequence.
A Sample Changer must be declared in the Configuration
menu. Refer to "Sample changer", page 169.
The reagent calibration method must have been edited
beforehand. Refer to "Edit reagent menu", page 80.
Refer to "Reagent calibration stack", page 148.
To access (for an electrode calibration stack):
1. In the Electrode window, press 1 Calibrate electrodes.
2. Press 2 Calibration sequence.
A Sample Changer must be declared in the Configuration
menu. Refer to "Sample changer", page 169.
The electrode calibration method must have been edited
beforehand. Refer to "Edit electrode menu", page 78.
Refer to "Electrode calibration stack", page 85.
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TitraLab
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TitraLab 840 and 845 Reference Manual
Beakers: [F;L]
Beep
Blank (Yes/No)
The beakers information is displayed in the Edit sequence menu of a
sequence.
It indicates the First and Last positions occupied by the beakers in the
sequence.
If Yes has been selected, three beeps will sound when a result is
obtained.
Enter in:
Setup menu > Configuration
Select Yes to subtract the volume of reagent used to titrate the solvent
from the volume found for the dissolved or diluted sample.
When you run for the first time a method with a blank, you start with
the determination of the blank. The blank volume is saved with the
method. If you start again this method, you have the choice between
running an analysis with the blank alone or running an analysis of the
sample with subtraction of the blank volume to the result.
Blank not required
Blank on inflection no.
Blank required
Enter in:
Edit method menu
This message appears at the start of a sequence, if a method
sequence programmed with a blank titration has now been
reprogrammed without a blank.
Go to Sequence/Sample stack, Edit sequence menu and remove the
blank titration method from the sequence.
Inflection point number (1 to Number of IP) on which the blank volume
will be subtracted.
Enter in:
Edit method > Results (for Monotonic IP, Dynamic IP or Continuous IP
method).
This message appears at the start of a titration when a blank has
been programmed in the method, but a blank value is not available.
Press ✓ and run blank.
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TitraLab
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TitraLab 840 and 845 Reference Manual
Blank volume
Burette functions menu
Volume of titrant consumed by the titration on a blank sample.
If you run an End point titration with several E.P., a blank volume is
found for each E.P. If you run an Inflection point titration, one blank
volume is found irrespective of the number of Inflection points found
for the method. This blank volume is determined on a particular
inflec tion point of the titration curve, see "Min. ordinate Max. ordinate
- Blank", page 120.
When you run a method with a blank for the first time, the blank is
determined and stored along with the method. If the method is
restarted, you will be given the choice to run a sample analysis or a
blank analysis.
For a sample analysis using an End point method, a blank volume will
be automatically subtracted from each end point found.
For a sample analysis using an Inflection point method, a blank
volume will be automatically subtracted from the Inflection point
selected by the user, see "Blank on inflection no.", page 53.
These functions can be activated during the preparation of the
burette, before installing the reagent.
To access, press 3 in the Reagents window. To run a burette function,
select the burette in the Address field, then press 1 to 5
corresponding to the required procedure. The title bar shows the
volume of the burette in use. You can replace (key 4) or remove this
burette (key 5).
Burette speed
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Figure 10: Burette functions menu (burette installed/not installed).
The maximum burette speed (in ml/min) is three times the nominal
value of the burette per minute. However, for the 50 ml burette the
maximum burette speed is 1.5 times the nominal value, i.e. 75 ml/min.
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Burette volume
Calculate with EP no.
Calculate with IP no.
The burette volume is entered while installing or replacing the burette.
This volume is indicated on the burette.
Enter in:
Install burette or Replace burette menu.
Range available:
1 ml, 5 ml, 10 ml, 25 ml or 50 ml.
End point number (1 to Number of EP) for which the volume will
be used to calculate the result. Depending on the option selected for
Results by cumulate or difference, this will be the volume delivered
from the titration start to the end point no. "n" or the volume delivered
between the end points no. “n-1” and “n”.
Enter in:
Edit method > Results
Inflection point number (1 to Number of IP) for which the volume
will be used to calculate the result. Depending on the option selected
for Results by cumulate or difference, this will be the volume delivered
from the titration start to inflection point no. "n" or the volume
delivered between the inflection points no. “n-1” and “n”.
Calibrate electrodes
Calibrate reagents
Calibration delay elapsed
Enter in:
Edit method > Results
Refer to "Electrode calibration", page 82.
Refer to "Electrode calibration (SAC sequence)", page 83.
Refer to "Reagent calibration", page 145.
Refer to "Reagent calibration (SAC sequence)", page 146.
This message appears at titration start. A new electrode or reagent
calibration is required. The delay Periodicity entered in the Edit electrode or Edit reagent screen has elapsed, see "Periodicity", page
129.
Press ✓ and perform a calibration.
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Calibration parameters
Calibration request
Calibration results parameters
For an electrode calibration method, see "Electrode calibration
parameters", page 84.
For a reagent calibration method, see "Reagent calibration parame-
ters", page 147.
Available if Electrode type = pH
Select the option Calibrate request = Yes to calibrate
electrodes.
The corresponding calibration parameters and pH standards will be
displayed.
Enter in:
Edit electrode menu
Refer to "Results menu", page 160.
Calibration sequence
Calibration stack
Catalogue list
To run an electrode calibration sequence, see "Electrode calibration
(SAC sequence)", page 83.
To run a reagent calibration sequence, see "Reagent calibration (SAC
sequence)", page 146.
To prepare an electrode calibration stack, see "Electrode calibration
stack", page 85.
To prepare a reagent calibration stack, see "Reagent calibration stack",
page 148.
For an electrode calibration method, see "Electrode calibration
stack", page 85.
For a reagent calibration method, see "Reagent calibration stack",
page 148.
List of Radiometer Analytical names of electrodes and commonly
used reagents. This list cannot be modified.
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Cell grounding
Cell window
Defines the grounding of the measuring cell. Select one of the
following options:
Reference
Grounding is ensured by a reference electrode - general use.
Metal
Grounding is ensured by a metal electrode connected to the GND
socket on the Titration Manager. Use this option in case of high
resistive solutions in order to avoid measuring background noise at
the electrodes.
Others
Grounding is not ensured by the reference electrode and is defined
outside the method.
Enter in:
Edit method menu
Use LEFT/RIGHT arrow keys to access.
This window controls the stirring function of the measurement cell.
Change electrode name
Start/stop stirrer
Select stirring speed: 100 to 1100 rpm
Animated icon: indicates when stirrer
or propeller is in operation
An external stirrer (propeller) can be connected to the
Titration Manager.
Refer to "Stirring", page 185.
1. Display the Electrode window.
2. Press 4 then 2.
3. In the ID field, enter the new name for the electrode
(16 characters maximum).
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Change method name
Change reagent name
Change sequence name
1. Display the Main window.
2. Press 5 then 2.
3. In the ID field, enter the new name (16 characters maximum).
1. Display the Reagent window.
2. Press 5 then 2.
3. In the ID field, enter the new name (20 characters maximum).
1. Display the Main window.and select Sequence or SAC sequence.
If the SAC Sequence command is not available,
declare a Sample Changer (SAC80, SAC850) in the Setup >
Configuration menu (Supervisor access only).
Refer to "Sample changer", page 169.
2. Press 2 Sequence/Sample stack
3. In the Sequence/Sample stack menu, select ID.
4. Enter the new name (16 characters maximum).
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Check command
If a Stormy or a Question mark icon appears in the Reagent/Electrode
windows, press 1 to run the “Check” command. The Titration Manager
will automatically guide you through the operations required to solve
the problems encountered.
For example:
Press 1
Press ✓
Check electrodes
Check reagents
Press 2 to start the Reagent
Installation procedure.
Refer to "Select method", page 175.
Refer to "Select method", page 175.
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Communication failure (SAC error)
Concentration
Concentration unit
The data transmission between the sample changer and the workstation cannot be performed properly.
Check the cable connections and make sure that the sample changer
is switched on and connected to the workstation via the RS232 serial
cable.
Press the workstation key ✓ or Stop and restart the sequence. It is
not possible to continue the sequence from the point it stopped.
Concentration of the titrated species present in the standard.
Enter in:
Edit reagent > Standard
Range available:
0.001 to 10000 (unit = Concentration unit)
Standard concentration unit.
Enter in:
Edit reagent > Standard
Configuration menu
Range available:
If Amount unit = ml or µl: eq/l, meq/l, mol/l, mmol/l, g/l, mg/l, mg/ml
If Amount unit = g or mg: eq/kg, meq/kg, mol/kg, mmol/kg, mg/g,
mg/kg,%
Press Stop 3 seconds in the Main window then press 1.
Contains the configuration parameters for the instrument. .
Refer to "Setup menu", page 178.
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Connections
Balance: Refer to "Balance connection", page 48.
Bar code reader: Refer to "Bar code reader connection", page 49.
Electrodes: Refer to "Electrode connection", page 86.
PC keyboard: Refer to "Keyboard connection", page 112.
PC: Refer to "PC connection", page 128.
Printer: Refer to "Printer connection", page 135.
Sample changer: Refer to "Sample changer", page 169.
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Continuous IP method
For this type of method, the titration is carried out using continuous
addition of titrant.
The titrant addition speed is regulated between two user selectable
limits (Min. speed and Max. speed). The addition speed decreases
when the slope of the E or pH = f(Volume) titration curve increases
and vice versa. This prevents overshooting the equivalent point.
Speed
E or pH
V max
V min
Volume
Figure 11: Continuous IP - Titrant addition speed
Using a Continuous IP method, higher the slope of the titration curve
is, higher the number of measurements saved will be. A great majority
of points are saved close to the inflection point. This allows an accurate determination of the equivalent point.
E or pH
Figure 12: Continuous IP - Number of points saved
The Continuous IP method can be stopped after a given number
(1 to 4) of equivalent points has been detected.
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Contrast
Controlled by TTL IN
Copy electrode
The contrast of the display can be adjusted in the Main window.
• press 0 to increase the contrast
• press 7 to decrease the contrast
Refer to "Auxiliary input", page 41.
This procedure is used to create an electrode, without having to enter
data nor program the corresponding calibration method.
1. Enter the Electrodes window.
2. Press 4 then 1.
3. In the Function field, select the function according to the elec-
trode type then press ✓, see "Electrode type", page 89.
4. Select the ID field and press ✓ .
5. Select From = Catalogue.
6. In the ID field, select an electrode name from the Catalogue list.
7. In the id field, you can identify the electrode by assigning a
second id name. This electrode will be called "IDid".
8. Press 1 to confirm then 2 Copy from electrode.
9. In the Library field, select the Preprogrammed or User list.
10. In the ID field, select the electrode to be copied from the list of
available electrodes.
11. Press 1 to confirm. The electrode is created and saved in the
User list.
If you selected the option Preprogrammed, the list is limited to
electrodes of the same type as the "copied" electrode.
If you selected User, the list is limited to electrodes having the
same function (pH, mV (i=0), mV(i>0), T°C, Reference or
Ground) as the "copied" electrode.
It is not necessary to select Catalogue to create an
electrode using the copy function. An electrode ID created from
Other can also use the copy function.
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Copy method
Copy reagent
1. Switch to Main window.
2. Press 5 then 1.
3. Press ✓ in New method menu.
4. For ID, enter a method name.
5. Press 2 Copy from method.
6. In the Library field, select the Preprogrammed or User list.
7. In the ID field, select the method to be copied from the list of
available methods.
8. Press 1 to confirm. The method is created and saved in the User
list.
This procedure is used to create a reagent (new reagent ID), without
having to enter data nor program the corresponding calibration
method.
1. Enter the Reagents window.
2. Press 5 then 1.
3. Press ✓ in the New reagent menu.
4. Select From = Catalogue.
5. In the ID field, select a reagent name from the Catalogue list.
6. Enter the "approximate" titre for the reagent (between 0.001 and
99 999) in the Target titre field.
7. Enter the unit indicated on the reagent bottle (mM = mmol/l, M =
mol/l, mN = meq/l or N = eq/l).
8. Press 1 to confirm then 2 Copy from reagent.
9. In the Library field, select the Preprogrammed or User list.
10. In the ID field, select the reagent to be copied from the list of
available reagents.
11. Press 1 to confirm. The reagent is created and saved in the User
list.
It is not necessary to select Catalogue to create a
reagent using the copy function. A reagent ID created from
Other can also use the copy function.
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Coupled method
A Coupled method is a combination of 2 methods performed in the
same beaker. When using a coupled method, the instrument runs all
these methods on the same sample.
If you wish to run a series of methods in different beakers, it is
necessary to program a sequence using a Sample Changer instead
of a Coupled method.
Example: Combination of method 1 and method 2.
The number of test portions (for example 3) is entered during programming. The method is then repeated in the number of beakers
specified.
Sample 1
2
Method 2
Test portion 3
3
3
Method 2
Method 1
Test portion 1
1
1
Method 2
Method 1
= beaker number 1
1
Test portion 2
2
Method 1
Figure 13: Coupled method with three tests
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Create electrode
1. Enter the Electrode window.
2. Press 4 then 1.
3. Select the electrode function, see "Electrode type", page 89.
4. Press ✓ in the ID field.
5. Select From = Other.
The option From = Catalogue allows you to create an
electrode from a list of Radiometer Analytical electrodes.
6. Enter the electrode name (up to 16 alphanumeric characters).
7. In the Confirm creation screen:
• For pH, mV or ISE electrodes only; select the electrode type.
Refer to "Electrode type", page 89.
• For combined pH or single pH electrodes; enter the internal pH
(pH int) of the electrode.
Refer to "pH int", page 130.
• For combined pH, Metal/Redox or ISE electrodes or for a
Conductivity electrode; select if the electrode has a built-in
temperature sensor or not.
Create method
• For reference electrodes or combined pH, Metal/Redox, ISE
electrodes; enter the potential of the reference (in mV) versus the
Standard Hydrogen Electrode.
Refer to "Potential versus SHE", page 131.
8. Press 1 to create the electrode. The Edit electrode menu is
displayed. Enter the electrode definition parameters.
1. Enter the Main window.
2. Press 5 then 1.
3. Press ✓ in the New method screen.
4. Enter a method name (up to 17 alphanumerical characters).
5. Press 1 to create the method. The Edit method menu is
displayed.
6. Enter the method parameters.
Refer to "Programming method", page 138.
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Create reagent
1. Enter the Reagents window.
2. Press 5 then 1.
3. Press ✓ in the New reagent menu.
4. Select From = Other.
The option From = Catalogue allows you to create a reagent
from a list of commonly used reagents.
5. In the ID field, enter the reagent name (up to 14 alphanumeric
characters). It is advised to enter the chemical formula of the reagent (example: HCl). The concentration is entered on the next
line.
6. Enter the "approximate" titre of the reagent (5 characters) in the
Target titre field.
7. Enter the unit indicated on the reagent bottle (mM = mmol/l, M =
mol/l, mN = meq/l or N = eq/l).
8. Press 1 twice to create the reagent.
9. Enter the reagent parameters.
Current value
Curve
Curves data lost
- Cal. Data kept Methods kept
This is the current sent to the Pt-Pt socket on the Titration Manager.
This parameter is available if mV(i>0) has been selected for
Measurement in the Edit method or Edit reagent menus.
Enter in:
Method parameters menu
Reagent parameters menu
Range available:
-1000 to +1000 µA in steps of 1 µA
Select if you want to print the pH/mV = f(volume) titration curve at the
end of each test.
Enter in:
Edit method > Printouts
Edit reagent > Printouts
The last curve data acquisition is lost. Generally, this error occurs
when the instrument is switched off while an analysis is in progress.
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Customise
A name (max. 16 alphanumeric characters) can be assigned to the
Titration Manager. This name will be displayed in the title bar of the
Main window.
If required, a maximum of 4 lines (32 characters) is available to enter
personal information, or your company’s address. This information will
appear as a header at the start of the report printout.
Enter in:
Setup window > Customise
Date entry
Default parameters
Enter current date in following format: dd:mm:yyyy.
Use the Up/Down arrow keys to jump to the month.
Enter in:
Setup menu > Configuration
Reset the parameters programmed in the method, reagent, or electrode. Use this command to reset the preprogrammed methods, reagents or electrodes to the Titration Manager’s default values.
Proceed as follows:
1. For a method: display the Main window and press 5.
For a reagent: display the Reagent window and press 5.
For an electrode: display the Electrode window and press 4.
2. Select the method, reagent or electrode ID.
3. Press 3 Default parameters.
4. Press ✓ to confirm the reset.
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Delay after addition
Delete electrode
Option available with TitraLab 845.
This delay is counted down after a reagent addition. This time allows
the solution to stabilise after a reagent addition and before the next
titration starts.
While an addition method is running, you can carry on
regardless this delay by pressing key Del.
Enter in:
Edit method > Parameters (titration method if Addition = Yes)
Edit reagent > Calibration parameters (if Addition = Yes)
Range available:
00:00 to 99:59 min:s
1. Select the electrode to be deleted.
2. Press 4.
3. Press ✓ to confirm or ESC to leave the menu without deleting.
Delete method
Delete reagent
It is not possible to delete an electrode which is used in another method or sequence. Modify the method or sequence,
e.g. change electrode ID or remove the electrode, before
deleting.
1. Select the method to be deleted.
2. Press 4.
3. Press ✓ to confirm or ESC to leave the menu without deleting.
It is not possible to delete a method which is part of a
sequence or coupled method. Remove the method from the
sequence or from the coupled method before deleting.
1. Select the reagent to be deleted.
2. Press 4.
3. Press ✓ to confirm or ESC to leave the menu without deleting.
It is not possible to delete a reagent which is used in another
method or sequence. Modify the method or sequence, e.g.
change reagent ID or remove the reagent, before deleting.
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Delete sequence
Demand: Locked
Demand: Unlocked
Deleting a sequence consists of removing all the methods present in
the sequence.
Refer to "Empty sequence", page 90.
Electrode or Reagent calibration
The routine user is not allowed to bypass an electrode and/or reagent
calibration demand before continuing measurements. It means that
the electrode and/or reagent calibration periodicity has(have) been
elapsed.
Sequence edition
The routine user is not allowed to create, edit or delete sequence of
methods.
Enter in:
Setup menu > Access routine mode
Electrode or Reagent calibration
The routine user is allowed to bypass an electrode and/or reagent
calibration demand and continue measurements. This happens when
the electrode or the reagent calibration periodicity has elapsed.
Derivative
Sequence edition
The routine user is allowed to create, edit or delete sequence of
methods.
Enter in:
Setup menu > Access routine mode
Specify if you want to print the derivative curve at the end of each test.
Enter in:
Printouts menu of Monotonic IP, Dynamic IP or Continuous IP method.
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Detailed
This parameter sets level of details of report printouts.
Detailed = Low
• The header only comprises the analysis name, time and date and
the instrument serial number. These data are printed on the same
line.
• Reagent or electrode calibration method: results are printed.
Detailed = Medium
This is the printout level selected by default.
• The header comprises the analysis name, time and date, the
instrument serial number and the laboratory coordinates.
• Reagent or electrode calibration method: results are printed.
Detailed = High
• The header comprises the analysis name, time and date, the
instrument serial number and the laboratory coordinates.
• Electrode data, electrode calibration data and results, burette serial
number, reagent data and reagent calibration data and results are
printed.
• The buffer data (name, potential value) are printed.
• End point/Inflection point coordinates (potential, volume) are
printed (except for a reagent calibration).
Enter in:
Edit method > Printouts
Edit reagent > Printouts
Edit electrode > Printouts
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Direction
Direct measurements
Display contrast
Determines whether the addition of titrant increases or decreases the
pH or mV value.
This parameter informs the Titration Manager if the end point or the
Stop point is already passed before the start of the titration.
Example:
If the titration is performed with an acidic titrant on an alkaline sample,
the addition of titrant will decrease the pH value. In this case, select
Direction = Decreasing pH.
Enter in:
Edit method > Parameters menu
Edit reagent > Calibration parameters menu
Refer to "Display measurement", page 73.
Refer to "Contrast", page 63.
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Display measurement
Press 2 in the Electrode window.
The signal measured of a connected electrode in the current system
is displayed. If several electrodes are connected, select the electrode
at the ID line.
Depending on the type of electrode connected, the display shows:
• pH and corresponding potential difference in mV (pH electrodes)
• potential difference in mV (metal/redox or ISE electrodes)
• temperature in °C (temperature sensors)
• potential difference in mV and polarisation current in µA (mV(i>0)
measurement mode for a double metal electrode). The polarisation
signal parameters are entered in the Method parameters or
Reagent parameters menus.
Refer to "Applied signal (AC/DC)", page 40.
Refer to "Current value", page 67.
Press Esc to stop measurements.
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Dyn. rinse
You have the choice between rinsing dynamically the electrodes :
• N-1/st in Park: in previous (just analysed) beaker except
1st and calibration beakers
• N-1/st in Rinse 2: in previous (just analysed) beaker
except 1st and calibration beakers
• In Park: in park (all dynamic rinses performed in the park
beaker).
For the first dynamic rinse of sample changer cycle run, we have the
choice between rinsing dynamically the electrodes in the Park beaker
or in the R2 beaker (static rinse beaker no.2). If R2 is selected, it
means that only 1 beaker remains available for static rinses (static
rinse beaker no.1 (R1)).
Refer to "Number of static rinses", page 127.
At the end of a dynamic rinse, the electrodes are left above a
nearly emptied rinse beaker. The beaker contains a little
solvent which has been used to rinse the end of the electrodes and the addition tips.
Refer to "Dynamic rinses", page 77.
Dynamic rinses can not occur in calibration beakers. When
an electrode or a reagent calibration beaker is found in the
sequence, the dynamic rinse which follows the measurement
will occur in the Park or Rinse 2 beaker depending on the
option selected for
in park,
in R2 (static rinse beaker no.2),
Dyn. rinse
.
Static rinse beakers and Park beakers: Refer to User’s
Guide of the SAC850 sample changer (part no. D21T085).
Enter in:
Setup menu > Configuration
Range available:
N-1/1st in Park, N-1/1st in Rinse 2 or In Park.
If Sample changer = SAC850
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Dynamic dose
During Incremental IP titration the size of the increments is controlled
by the Dynamic dose. Small increments will be added in the vicinity of
the curve inflections, and larger increments will be added at the flat
part of the curve. The size of the increments cannot be greater than
the Maximum dose.
The higher the value is, the larger the increments will be. Decreasing
the Dynamic dose value slows down the titration, but leads to more
accurate titration. However, too small a value can lead to the detection
of false inflection points.
The standard value, 10, will be appropriate for standard applications. If you want to use increments of the same size, select
an IP Monotonic method.
Enter in:
Method parameters menu of a Dynamic IP method.
Range available:
1 to 999
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Dynamic IP method
A volume of titrant (increment) of varying size is added to the solution
as soon as the electrode response satisfies the measurement variations satisfy the stability criterion or once the preset Acceptation time
has elapsed. The increment size is inversely proportional to the slope
of the titration curve.
In Dynamic IP, one measurement is saved per increment added.
E or pH
Figure 14: Dynamic IP method - size of the increments
Select a Dynamic IP method when you want to optimise the ratio titration duration/accuracy of the EP/IP points detected. Dynamic IP is well
adapted to single EP/IP titrations or to titrations with well-defined EP/
IP points.
The Dynamic IP method is stopped after a given number of equivalent
points (1 to 4) has been detected.
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Dynamic rinses
Dynamic rinses are performed by a SAC850 Sample Changers if the
Dynamic rinsing module is installed on the sample changer.
A Dynamic rinse performed in a Park or Rinse beaker consists of the
following operations:
1. The electrode are positioned above the Park or Rinse beaker.
2. The electrodes are dipped into the beaker. The beaker is emptied
to a waste in the same time. At the end, the electrodes are
located in the emptied beaker at their downmost position.
3. The electrodes are washed with rinse solution (usually demineral-
ised water) then start to move up under rinsing. At the end, the
electrodes are located above a beaker filled with rinse solution
and some remaining impurities.
4. Steps 2 and 3 can be repeated up to 8 times as up to 9 dynamic
rinses can be programmed. Steps 2 and 3 are performed under
stirring.
A Dynamic rinse performed in a Sample beaker consists of the following operations:
1. The electrodes are dipped into the Sample beaker. The beaker is
emptied to a waste in the same time. At the end, the electrodes
are located in the emptied beaker at their downmost position.
2. The electrodes move up and are washed in the same time with
rinse solution (usually demineralised water). At the end, the electrodes are located above a beaker filled with rinse solution and
some remaining impurities.
3. The sample beaker is emptied to a waste.
4. A last rinsing of the electrodes and delivery tips is carried out. At
the end, the electrodes are located above a nearly emptied
beaker containing a little solvent that was used to flush the electrodes and delivery tips.
5. Steps 1 to 3 can be repeated up to 8 times as up to 9 dynamic
rinses can be programmed. Steps 1 to 3 are performed under
stirring.
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Edit electrode menu
In this menu, you can rename the electrode (line ID), revise electrode
data, decide if you want to calibrate the electrode
(line Calibration request) and enter the electrode
calibration data if relevant.
To access:
1. Press 4 in the Electrode window.
2. Press 2 Edit electrode.
The following menus are accessible using the arrow keys:
Calibration parameters.
Refer to "Electrode calibration parameters", page 84.
Calibration solutions.
Refer to "Solution menu", page 181.
Results.
Refer to "Results menu", page 160.
Printouts.
Refer to "Printouts menu", page 137.
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Edit method menu
In this menu, you can rename the method (line ID), revise and enter
method data.
To access:
1. Press 5 in the Main window.
2. Press 2 Edit method.
The following menus are accessible using the arrow keys:
Method parameters.
Refer to "Method parameters menu", page 117.
Sample.
Refer to "Sample menu", page 171.
Results.
Refer to "Results menu", page 160.
Printouts.
Refer to "Printouts menu", page 137.
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Edit reagent menu
In this menu, you can rename the reagent (line ID), revise reagent
data, decide if you want to calibrate the reagent
(line Titre) and enter the reagent calibration data if relevant.
To access:
1. Press 5 in the Reagents window.
2. Press 2 Edit reagent.
The following menus are accessible using the arrow keys:
Calibration parameters.
Refer to "Reagent calibration parameters", page 147.
Standard.
Refer to "Standard menu", page 183.
Results.
Refer to "Results menu", page 160.
Printouts.
Refer to "Printouts menu", page 137.
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Edit sequence menu
1. Perform steps 1 to 6 of the "Programming sequence" procedure.
Refer to "Programming sequence", page 139.
2. In the Sequence/Sample stack window (access: press 2
Sequence/Sample stack from the main window),
press 3 Edit sequence.
Select the methods to be included in
the sequence. Use the Add method
(key 1)/ Insert method (key 2)
procedures.
In the title bar, “x/y” (1/1) indicates the
position "x" occupied by the method in
the sequence and "y" the total number
of methods listed in the sequence.
The ID and type of the selected
method cannot be modified at this
level. They are defined in the Add
method or Insert method
menu.
Refer to "Add method menu", page 36.
Refer to "Insert method menu", page 106.
3. At the line Number of samples, enter the number of times a
method must be repeated within the sequence.
At the line Beakers: [F;L], the instrument displays the positions F
and L occupied by the first and last beakers In the sequence.
4. If a SAC850 is used and declared in the Configuation menu, you
can also choose a sample preparation number used for the
selected method, see "Sample preparation no.", page 172.
The last step of the sequence programmation consists of editing the
sample stack, see "Sample stack", page 174.
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Electrode calibration
1. Select the method which uses the electrode to be calibrated.
2. Connect the electrode system, see "Electrode connection", page
86.
3. Press 1 Calibrate electrodes in the Electrode window.
4. Press 1 to Run, and follow the messages on the display:
- entry of the User ID and standard temperature, if relevant,
- Rinse and dip the electrode in beaker 1 containing buffer no. 1.
5. Measurements start in buffer no.1.
The instrument displays the potential
measured. The displayed temperature is
the temperature measured, entered or is
equal to 25°C according to the
calibration method programmed.
The electrode zero pH and sensitivity are calculated at the end of
a multi-point calibration. For a 1-point calibration, only the zero pH
is calculated, the slope comes from the last calibration performed
or is equal to the default value (59.16 mV/pH unit). The calibration
results are saved with the electrode.
To consult the calibration results, see "GLP-Archives menu",
page 104.
It is recommended to maintain all your standards at the same
temperature. Then the temperature entered at the start of a
calibration cycle is valid for all your standards.
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Electrode calibration (SAC sequence)
In a calibration sequence, the standard solution beakers are handled
automatically using a sample changer. A SAC80 or SAC850 Sample
Changer must be connected and declared in the Configuration menu.
1. Install the sample changer and connect it to the SAC socket of the
Titration Manager using the cable, part no. A95A202 or A95X501.
Refer to the User’s Guide of the sample changer
(part no.: D21T013 for a SAC80, D21T085 for a SAC850).
2. If a Question mark "?" is present in the Reagent and/or Electrode
tabs, it means that the sequence needs to be programmed - a
reagent or an electrode is missing. Review programming in
Supervisor mode. Refer to "Programming sequence", page 139.
3. Connect the electrode system, see "Electrode connection", page
86.
4. Press 1 Calibrate electrodes in the Electrode window.
5. Select the electrode from the list of the electrode system.
6. Press 2 Calibration sequence.
7. Prepare the electrode calibration stack, see "Electrode calibration
stack", page 85.
8. Press Esc then 1 to run the calibration sequence. Follow the
messages on the display.
9. The sample changer cycle is initiated.
- 1 to 9 dynamic rinses (if programmed with a SAC850
- 1 to 3 static rinses (if programmed).
- Electrodes are dipped into the first standard solution.
Measurement starts.
- Between each standards (beakers), 1 to 9 dynamic rinses (if
programmed with a SAC850) then 1 to 3 static rinses are performed (if programmed to do so).
10. At the end, the Titration Manager displays the calibration results.
The calibration results are saved with the electrode.
To consult the calibration results, see "GLP-Archives menu",
page 104.
When running a calibration sequence with a SAC80 Sample
Changer, do not use the STOP key of the SAC80.
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Electrode calibration not required
Electrode calibration parameters
Message appears at the start of a sequence, if a method sequence
has been programmed with an electrode calibration. The electrode
used has been programmed without calibration Calibration
request = No.
Go to Sequence/Sample stack, Edit sequence menu and
remove the electrode/reagent calibration method.
This menu contains the general parameters concerning the pH electrode calibration method (measurement stabilisation criteria in
particular).
To access:
1. From the Electrode window, press 4.
2. Select the pH electrode to be edited.
3. Press 2 Edit electrode and check that the Calibration
request = Yes option has been selected.
4. Edit the electrode calibration general parameters.
5. Use the LEFT/RIGHT arrow keys to move to the last Edit
electrode display.
6. Press 1 Calibration parameters.
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Electrode calibration stack
The electrode calibration stack defines individual data for each buffer
solution beakers present in an electrode calibration sequence.
1. In the Configuration menu, declare the model of sample changer
used (SAC80 or SAC850).
Refer to "Configuration menu", page 60.
Depending on the model of sample changer used, enter the
sample changer configuration parameters.
Refer to "Sample changer", page 169.
2. Enter the Electrode window and press 1 Calibrate electrodes.
3. Select the electrode to calibrate.
4. Press 2 Calibration sequence.
<1/5> means the first beaker over 5
programmed in the sequence. Use the LEFT/
RIGHT arrows to review the other beakers in
the sequence.
The number of beakers is entered in the Edit
electrode menu. The buffer solutions are
selected in the Solutions menu.
Label the beakers indicating the running number in the
sequence, for example: 1/5, 2/5 etc.... and the name of the
buffer solution.
Place the beakers in the numbered position on the sample
changer.
If rinses are programmed, position the corresponding rinse
beakers at the right places.
Refer to "Number of static rinses", page 127.
Refer to "Dynamic rinses", page 77.
You can print the calibration stack by pressing Print from the
calibration menu.
Press Esc then run the sequence by pressing 1 Run calibration.
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Electrode connection
1. In the Main window, press 2 Select method and select the method
to be run. The electrodes to be connected are listed with their
addresses.
2. Install electrodes on the Titration Manager (TIM), or sample
changer (SAC80 or SAC850).
3. Connect electrodes to the rear panel socket of the Titration
Manager (TIM). See figure and table below. Example: pHC2401-8
to E1 socket (address TIM/E1). Refer to "Address", page 38..
T
empGND
Pt-Pt Ref E1E2
Figure 15: Electrode sockets
Socket Electrode
REF Single reference
TEMP Temperature
GND Single metal for cell grounding only
Pt-Pt Double metal
E1 Others
Table 3: Connecting electrodes
When installing/checking an electrode system, do not forget to
connect all the electrodes to the Titration Manager and disconnect all
the electrodes that are not used by the method or sequence.
In particular, if you are about to run a pH (or potential at zero current)
measurement, check that there is no double metal electrode connected to the Pt-Pt instrument socket before running the method (disconnect this electrode, if any).
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Electrode function
Electrode icons
Refer to "Function", page 102.
Select to access Electrode window.
Indicates the state of the electrode system.
Sunny icon:
The calibration has been performed on all the electrodes
present in the system.
Cloudy icon:
The electrode calibration of one of the electrodes present
in the system should be performed within 24 hours.
Note: when the Periodicity is set to 1 day, this icon will
appear to indicate that a calibration must be performed
within 12 hours.
Stormy icon:
The calibration date has elapsed for one of the electrodes
present in the system.
If acceptance limits have been set for the calibration: at
least one calibration result lies outside the programmed
acceptance limits.
Electrode ID
Question mark:
The electrode system has not been programmed
correctly. Enter Supervisor mode and Check the
electrode parameters in the Method parameters menu. If
a temperature sensor has been defined in the Electrode
menu, use the same sensor in method.
For a reagent calibration, make sure that the electrode(s)
used for the calibration are the same as those used in the
method.
Press 1 in the Main window, the instrument will indicate the
possible errors and prompt you to correct them.
Name assigned to the electrode (max. 16 alphanumeric characters).
Enter in:
Electrode window > Edit electrode
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Electrode identification
Electrode library
An electrode is identified by its name (ID). The ID and other electrode
specifications are entered in the Edit Electrode menu. These other
parameters are :
•Type
• Address
To access, press 4 in Electrode window.
The electrode library comprises the following menus and commands:
Electrode
library
Commands/
actions
New
electrode
Default
parameters
Delete
electrode
Programming
data
Edit electrode
Calibration parameters
Calibration solutions
Results
Electrode not calibrated
Electrode system
Printouts
Figure 16: Electrode library overview
The electrode has not been calibrated and there is no electrode data
stored in the archives. Press ✓ and calibrate the electrode.
An electrode system comprises all the electrodes necessary to run a
method or a sequence of methods.
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Electrode type
The electrode type is displayed with respect to the function selected
( see "Function", page 102). The electrode type is defined when a new
electrode is created.
Refer to "Create electrode", page 66.
The different electrode types are listed below:
Type Function
Single pH pH
Combined pH (without temp. sensor) pH
Single metal/redox mV (i=0)
Combined metal/redox (without temp.
sensor)
ISE single mV (i=0)
ISE combined (without temp. sensor) mV (i=0)
Reference Reference
Temperature sensor T°C
Metal Ground
mV (i=0)
Double metal mV (i >0)
Table 4: Electrode functions and types
If Combined pH is defined, the Titration Manager prompts
you to specify if it has a built-in temperature sensor.
If a Single electrode is defined, the Titration Manager
prompts you to define a reference electrode.
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Electrode window
Electrodes are different
This window contains all the information and operations concerning
the electrodes.
To access:
Use LEFT/RIGHT arrow keys from the Main window.
This message appears if the active electrode used for the reagent
calibration is different from the electrode used in the method.
Check the method and reagent calibration parameters menus.
Empty burette
Empty sequence
1. Enter the Burette functions menu.
2. Select the burette in the Address field,
see "Address", page 38.
3. Press 2 Empty. The burette is emptied at maximum speed
(approximate emptying time: 25 s).
Involves removing all the methods present in the sequence.
Proceed as follows:
1. Select the sequence to be emptied, see "Select sequence", page
175.
2. Press 3 Sequence/Sample stack then 3 Edit sequence.
3. Press 3 Delete.
4. Press 2 Delete sequence then ✓ to confirm or press Esc to leave
the screen without emptying the sequence.
To remove a particular method from a sequence, see "Remove
method from a sequence", page 153.
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End point
End point delay
Adjustable pH/mV value to which titrant is to be dispensed.
Enter in:
Edit method > Parameters menu (end point method)
Edit reagent > Calibration parameters menu (end point method)
Range available:
-9.000 pH to +23.000 pH or -2000.0 mV to +2000.0 mV
Time during which the electrode signal is monitored after an end point
has been reached. If the electrode signal swings back, the burette
adds extra titrant to reach the end point and the count down of the
End point delay is repeated.
Enter in:
Edit method > Parameters menu (end point method)
Edit reagent > Calibration parameters menu (end point method)
Range available:
00:00 to 99:59 min:s
End point method
For this method, the user enters one or several pH/mV values, corresponding to the end points to be found during the titration.
Up to 2 end points can be determined per method.
The titration is carried out using the continuous addition technique.
The speed of addition is adjusted with respect to the distance which
separates the end point from the slope of the titration curve and the
method parameters entered by the user.
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Enter titre
Available if Titre = enter, see "Titre Enter/Calibrate", page 192.
1. Select the method or sequence which uses the current titrant.
2. If necessary, install the reagent, see "Install reagent", page 108.
3. Press 1 in the Reagent window.
4. If the method/sequence contains several reagents, press ✓ and
select the reagent from the list.
5. Press 1.
6. Enter user ID.
7. Enter the titre value in the Titre line.
8. Press 1 to confirm.
Range available:
0 to 1 x 10
10
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Equation formula
One or two user defined equations can be entered to calculate results
using user required units.
The formula specifies how the calculations should be performed. A
formula can use up to 64 characters and can consist of operators and
operands, that are derived from the completed titration data.
Enter in:
Edit method > Result
Operands
1.23, -24, -2.34E-5 Constants
pi 3,141592654
e 2,718281828 (base of the Natural loga-
rithm)
Ri where i = 1 to 4 Result no. i calculated for the method
Ei where i = 1 or 2
(for EP) and 1 to 4
(for IP)
Vi where i = 1 or 2
(for EP) and 1 to 4
(for IP)
Potential difference or pH measured at
EP/IP no. i
Cumulate volume delivered at EP/IP no. i
V Total volume delivered
SA Sample amount
T Last temperature measured (in °C)
CT Titrant concentration
CE Excess reagent concentration
VE Excess reagent volume
Bi with i = 1 or 2 (for
EP) i = 1 (for IP)
F Results factor
Table 5: Equation formula: operands
Blank volume for EP/IP no. i
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Equation formula
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Operators
+ Addition
- Subtraction or negation
* Multiplication
/ Division
( ) Operation defined in brackets. Each
abs Absolute value of variable following
TitraLab 840 and 845 Reference Manual
"(" bracket must be associated to one
")" bracket. Up to 10 sets of "( )" are
accepted per formula.
the symbol after the space
Equation - ID
abs ( ) Absolute value of variable defined in
brackets
x^y x power y
ln Natural logarithm: ln 2 or ln(2)
log logarithm 2 or log(2)
Table 6: Equation formula: operators
The name assigned by default to a result issued from an equation is
E1. You can change the E1 name (16 alphanumerical characters
maximum).
Enter in:
Edit method > Results
Refer to "Results menu", page 160.
If you change an equation result name (for example, from E1
to «My result»), the equations taking this result into account
continue to use the original operand name (E1 in our
example).
Refer to "Equation formula", page 93.
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Equation - unit
Use the numeric keypad to enter the units of the result calculated
using the equation.
Enter in:
Edit method > Results
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Equivalent point determination (IP methods)
An equivalent point of a titrated species/titrant reaction is determined
in two ways depending on the titrant addition mode (continuous or
incremental) selected:
Continuous addition of the titrant (Continuous IP method):
• acquisition of the titration curve E (electrode) = f (volume of titrant
dispensed),
• calculation of the first derivative curve with smoothing process
(method parameter: smoothing criterion),
• determination of the second derivative curve,
• determination of the inflection points on the first derivative curve
from the minimum and maximum of the second derivative curve,
• determination of the tangents to the first derivative curve for these
inflection points,
• determination of the equivalent point as the intersection of the two
tangents.
E or pH
Page 96
Figure 17: Determination of an equivalent point - Continuous IP method
An equivalent point is determined and plotted live on the titration
curve. The method can be stopped after a given number (1 to 4) of
equivalent points has been detected.
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Equivalent point determination (IP methods)
Incremental addition of the titrant (Monotonic/Dynamic IP
methods):
• acquisition of the titration curve E (electrode) = f (volume of titrant
dispensed),
• determination of the first derivative curve using a smoothing process (depending on the value set for IP filter),
• determination of the second derivative curve,
• determination of the maxima of the first derivative curve using the
IP filter parameter. These maxima correspond to the zeros of the
second derivative curve.
• determination of the equivalent point: for this point the maximum of
the first derivative curve must be equal to or greater than the preset
IP reject method parameter.
E or pH
Figure 18: Determination of an equivalent point - Monotonic or Dynamic IP
method
An equivalent point is determined and plotted live on the titration
curve. The method is stopped after a given number of equivalent
points (1 to 4) has been detected.
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ERR#32 (SAC error)
Refer to "SAC switch Off/On (SAC error)", page 167.
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Error messages
If you have forgotten an operation while editing the method, icons
visible in the Electrode and Reagent windows indicate that an error(s)
has occured. To find out where the error has occured and to help you
solve them, run the “Check” command in the Main window. The
Titration Manager will automatically guide you through the operations
required to solve the errors encountered.
Refer to "Check command", page 59.
Refer to "Electrode icons", page 87.
Refer to "Reagent icons", page 149.
List of Titration Manager error messages:
"No active electrode defined in "method ID"": see page 124.
"Add. reagent = Titrant": see page 36.
"Address conflict (between electrode IDs)": see page 38.
"Archives data lost - Cal. Data lost - Methods kept": see page 40.
"Back reagent = Titrant": see page 43.
"Back reagent unknown": see page 43.
"Blank not required": see page 53.
"Blank required": see page 53.
"Calibration delay elapsed": see page 55.
"Curves data lost - Cal. Data kept - Methods kept": see page 67.
"Electrode calibration not required": see page 84.
"Electrode not calibrated": see page 88.
"Electrodes are different": see page 90.
"Ground conflict": see page 104.
"Insufficient number of beakers": see page 109.
"Max. stab reached": see page 114.
"Max. vol - Predose > Bur. vol": see page 114.
"Max. volume reached": see page 115.
"Method wrong type": see page 118.
"Missing EP": see page 122.
"Missing IP": see page 122.
"Reagent calibration not required": see page 146.
"Reagent not calibrated": see page 150.
"Reagent titre not entered": see page 150.
"Reset memory": see page 156.
"Same buffer change buffer": see page 168.
"Sample unit conflict": see page 174.
"The sequence is empty": see page 190.
"Wrong buffer": see page 195.
List of SAC error messages:
"Communication failure (SAC error)": see page 60.
"ERR#32 (SAC error)": see page 98.
"Missing beaker (SAC error)": see page 122.
"SAC arm obstructed (SAC error)": see page 166.
"SAC option missing (SAC error)": see page 167.
"SAC switch Off/On (SAC error)": see page 167.
"Tray missing (SAC error)": see page 192.
"Turntable blocked (SAC error)": see page 193.
"Wrong type (SAC error)": see page 195.
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Error in equation formula
Excess reagent ID
The possible errors you may encounter when entering a formula:
• Operand unknown: term used does not exist, e.g. R2 if only one
result defined in the method.
• Syntax error: typing error in the formula, e.g. a missing bracket.
Refer to "Equation formula", page 93.
Identification of the excess reagent added during a back titrations.
For a manual back titration, the ID is entered manually.
During an automatic back titration, a name can be selected from a
Users or Preprogrammed list.
Refer to "Back titration No/Manual/Automatic", page 43.
Range available:
20 alphanumeric characters with units (mM, M, mN or N).
Enter in:
Edit method menu > Method parameters (for a back titration)
Excess titre
Excess volume
Titre of the excess reagent. Parameter only available for manual back
titrations. In the case of an automatic back titration, the titre is known
in advance by the Titration Manager.
Enter in:
Edit method > Parameters menu (Manual back titration method)
Range available:
0 to 1.000 10
Units (mM, M, mN or N), entered with the excess reagent ID.
Volume of excess reagent to be added during the titration.
Enter in:
Edit method > Parameters menu (back titration method)
Range available:
0.0 to 999.9 ml.
+8
.
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