899 Coulometer: Manual
899 Coulometer: Manual
Manual
8.899.8001EN
Metrohm AG
CH-9100 Herisau
Switzerland
Phone +41 71 353 85 85
Fax +41 71 353 89 01
[email protected]
www.metrohm.com
899 Coulometer
Manual
Table of contents
1 Introduction 1
1.1 Instrument description ......................................................... 1
1.1.1 Connectors .............................................................................. 1
1.1.2 Intended use ........................................................................... 2
1.2 About the documentation ................................................... 2
1.2.1 Symbols and conventions ........................................................ 2
1.3 Safety instructions ................................................................ 3
1.3.1 General notes on safety ........................................................... 3
1.3.2 Electrical safety ........................................................................ 3
1.3.3 Tubing and capillary connections ............................................. 4
1.3.4 Flammable solvents and chemicals ........................................... 5
1.3.5 Recycling and disposal ............................................................. 5
3 Installation 8
3.1 Setting up the instrument .................................................... 8
3.1.1 Packaging ................................................................................ 8
3.1.2 Checks .................................................................................... 8
3.1.3 Location .................................................................................. 8
3.2 Setting up the coulometer cell ............................................ 9
3.2.1 Inserting the coulometer cell .................................................... 9
3.2.2 Preparing the coulometer cell .................................................. 9
3.2.3 Mounting the addition and aspiration tube (utilization with Ti
Stand) ................................................................................... 13
3.2.4 Using the coulometer cell with a Karl Fischer oven ................. 14
3.2.5 Using the coulometer cell with a sample changer .................. 14
3.3 Connecting the coulometer to the power supply ............ 14
3.3.1 Connecting the power supply unit ......................................... 14
3.3.2 Connecting the Power Box .................................................... 15
3.4 Connecting sensors ............................................................ 17
3.4.1 Connecting a generator electrode .......................................... 17
3.4.2 Connecting an indicator electrode ......................................... 18
3.4.3 Connecting a temperature sensor .......................................... 20
3.5 Connecting an additional stirrer ....................................... 21
3.6 Connecting a balance ......................................................... 22
3.7 Connecting a keyboard, printer and other USB devi-
ces ........................................................................................ 24
4 Coulometric titration 28
4.1 Principle of coulometry according to Karl Fischer .......... 28
4.2 Working with water standards ......................................... 29
4.2.1 Certified water standards ....................................................... 29
4.2.2 Practical recommendations .................................................... 29
4.3 Sample addition .................................................................. 31
4.3.1 Size of the sample size ........................................................... 31
4.3.2 Working with liquid samples .................................................. 32
4.3.3 Working with solid samples ................................................... 32
4.4 Optimum working conditions ........................................... 33
4.4.1 General ................................................................................. 33
4.4.2 Drift ...................................................................................... 33
4.4.3 Reagent replacement ............................................................. 34
4.4.4 Indicator electrode ................................................................ 34
5 Operation 35
5.1 Switching the instrument on and off ............................... 35
5.2 Fundamentals of operation ............................................... 36
5.2.1 The keypad ............................................................................ 36
5.2.2 Structure of the dialog windows ............................................ 36
5.2.3 Navigating in the dialog ......................................................... 37
5.2.4 Entering text and numbers ..................................................... 37
5.2.5 Selecting from a selection list ................................................. 38
5.3 Formula editor .................................................................... 39
5.4 Methods .............................................................................. 40
5.4.1 Method templates ................................................................. 40
5.4.2 Loading a method template ................................................... 40
5.4.3 Saving a method ................................................................... 41
5.4.4 Exporting a method ............................................................... 42
5.5 Control ................................................................................. 43
5.6 Sample data ........................................................................ 44
5.6.1 Entering sample data in the main dialog ................................ 44
5.6.2 Requesting sample data at the start of the determination ...... 45
5.7 Sample table ....................................................................... 45
5.7.1 General ................................................................................. 45
5.7.2 Editing the sample data ......................................................... 47
5.7.3 Sending the sample size from a balance ................................. 49
5.8 Carrying out a determination ............................................ 49
5.9 Live modifications .............................................................. 52
5.9.1 Editing the sample data of the running determination ............ 52
5.9.2 Editing the sample table while a determination is running ...... 53
6 System settings 62
6.1 Basic settings ...................................................................... 62
6.2 Managing common variables ............................................ 65
6.2.1 General ................................................................................. 65
6.2.2 Editing common variables ...................................................... 65
6.3 File management ................................................................ 66
6.4 Configuring external devices ............................................. 68
6.5 Instrument diagnosis .......................................................... 71
6.5.1 Loading program versions and language files ......................... 71
6.5.2 Diagnosis functions ............................................................... 72
7 Parameters 73
7.1 Coulometric Karl Fischer titrations (KFC) ......................... 73
7.1.1 Conditioning ......................................................................... 73
7.1.2 Start conditions ..................................................................... 75
7.1.3 Control parameters ................................................................ 76
7.1.4 Titration parameters .............................................................. 79
7.1.5 Stop conditions ..................................................................... 81
7.1.6 Calculation ............................................................................ 81
7.1.7 Statistics ................................................................................ 85
7.1.8 Reports .................................................................................. 86
9 Troubleshooting 89
9.1 Karl Fischer titration .......................................................... 89
9.2 Miscellaneous ..................................................................... 91
10 Appendix 92
10.1 Stirring rate ......................................................................... 92
10.2 Balance ................................................................................ 92
10.3 USB devices ......................................................................... 93
10.3.1 6.2147.000 numerical USB keypad ........................................ 93
10.3.2 Key assignment of a USB keyboard ........................................ 94
10.3.3 PC mouse .............................................................................. 95
Index 167
Table of figures
Figure 1 Front 899 Coulometer ....................................................................... 6
Figure 2 Rear 899 Coulometer ........................................................................ 7
Figure 3 Inserting the coulometer cell ............................................................. 9
Figure 4 Filling the adsorber tube .................................................................. 10
Figure 5 Equipping the coulometer cell ......................................................... 11
Figure 6 Mounting the addition and aspiration tube ...................................... 13
Figure 7 Connecting the power supply unit ................................................... 15
Figure 8 Connecting the Power Box .............................................................. 16
Figure 9 Unscrewing the cover from the generator electrode ........................ 17
Figure 10 Screwing the electrode cable to the general electrode ..................... 18
Figure 11 Connecting a generator electrode ................................................... 18
Figure 12 Unscrew the cover from the indicator electrode .............................. 19
Figure 13 Screwing on the electrode cable to the indicator electrode .............. 19
Figure 14 Connecting an indicator electrode ................................................... 19
Figure 15 Connecting a temperature sensor .................................................... 20
Figure 16 Connecting a stirrer ......................................................................... 21
Figure 17 Connecting the balance via RS-232/USB Box .................................... 22
Figure 18 Connecting USB devices .................................................................. 24
Figure 19 Connecting the USB flash drive ........................................................ 26
Figure 20 Connecting the 6.2147.000 USB keyboard with USB flash drive and
printer ............................................................................................. 26
Figure 21 Connecting the USB hub with USB flash drive, printer and 6.2148.030
RS-232/USB Box .............................................................................. 27
Figure 22 Connecting a remote cable ............................................................. 27
Figure 23 Keypad 899 Coulometer .................................................................. 36
Figure 24 Directory structure on the USB flash drive ........................................ 67
Figure 25 Rotational speed depending on stirring rate .................................... 92
Figure 26 Control parameters and polarization current .................................... 96
Figure 27 Pin assignment of remote socket and remote plug .......................... 99
Figure 28 Remote status diagram .................................................................. 100
Figure 29 Connecting the RS-232/USB Box to the PC .................................... 101
1 Introduction
1.1.1 Connectors
The instrument is equipped with the following connectors:
■ Electrical connection
For connecting to the mains supply with the aid of the power supply
unit provided or for connection to the 6.2164.500 Power Box.
■ MSB connector (Metrohm Serial Bus)
For connecting an additional stirrer.
■ USB (OTG) connector
The 6.2151.100 adapter can be used to connect, for example, a
printer, a USB flash drive or a USB keyboard.
■ Sensor connectors
Three connectors for the following sensor types:
– Double Pt electrode
– Generator electrode
– Temperature sensor (Pt1000)
■ Grounding socket
For grounding the Coulometer.
■ Remote connector
For connecting instruments with a remote interface (e.g. 885 Compact
Oven SC).
Caution
Warning
This symbol draws attention to a possible hazard due
to electrical current.
Warning
This symbol draws attention to a possible hazard due
to heat or hot instrument parts.
Warning
This symbol draws attention to a possible biological
hazard.
Caution
This symbol draws attention to a possible damage of
instruments or instrument parts.
Note
This symbol marks additional information and tips.
Warning
This instrument has left the factory in a flawless state in terms of technical
safety. To maintain this state and ensure non-hazardous operation of the
instrument, the following instructions must be observed carefully.
Warning
Warning
Mains voltage
Warning
Warning
Caution
Leaks in tubing and capillary connections are a safety risk. Tighten all
connections well by hand. Avoid applying excessive force to tubing
connections. Damaged tubing ends lead to leakage. Appropriate tools
can be used to loosen connections.
Check the connections regularly for leakage. If the instrument is used
mainly in unattended operation, then weekly inspections are manda-
tory.
Warning
2.1 Front
3 Keypad
2.2 Rear
1 2 3 4 5 6 7 89
Figure 2 Rear 899 Coulometer
9 Grounding socket
For grounding the Coulometer. Socket B,
4 mm.
3 Installation
3.1.2 Checks
Immediately after receipt, check whether the shipment has arrived com-
plete and without damage by comparing it with the delivery note.
3.1.3 Location
The instrument has been developed for operation indoors and may not be
used in explosive environments.
Place the instrument in a location of the laboratory which is suitable for
operation, free of vibrations, protected from corrosive atmosphere, and
contamination by chemicals.
The instrument should be protected against excessive temperature fluctu-
ations and direct sunlight.
6.1464.320
6.2047.030
2 Insert the 6.1464.320 coulometer cell into the titration vessel holder.
Before setting up the coulometer cell the 6.1403.030 adsorber tube has
to be filled with 6.2811.000 molecular sieve. Proceed as follows:
6.1403.030
6.2811.000 2
1 Insert a small cotton plug into the bottom of the adsorber tube. Do
not pack the cotton too tightly.
3 Place a small cotton plug on the molecular sieve. Do not pack the
cotton too tightly.
Note
3
6.1403.030
2
6.2713.020
5
6.0341.100 4 6.0345.100
6.0344.100
6.2713.000
6.1437.000
6.2701.040 2 2
6.2713.010
6
6.1448.020
6.1464.320
1
6.1903.030
6.1437.000
2
6.2713.000
1
5
6
6.1439.010
6.2713.000
3
1 Attach the 6.2713.000 ground-joint sleeve that has been cut to size
to the ground joint of the 6.1437.000 stopper.
2 Insert the stopper into the 6.1439.010 addition and aspiration tube.
3 Attach the 6.2713.000 ground-joint sleeve that has been cut to size
to the ground joint of the addition and aspiration tube.
5 Connect the tubing for the reagent addition at the upper connector
of the addition and aspiration tube (5).
6 Connect the tubing for the aspiration of the coulometer cell at the
lower connector of the addition and aspiration tube (6).
Details regarding how to connect the addition tubing and the aspiration
tubing can be found in the manual for the 803 Ti Stand.
Warning
1 Connect the plug of the external power supply unit with the mains
connection (2-7) of the Coulometer.
Note
2 Connect the mains cable with the external power supply unit of the
Coulometer and with the mains supply.
Caution
Switch off the Coulometer correctly by pressing the red [STOP] key
before you interrupt the electricity supply. If this is not done, then there
is a danger of data loss.
1 Connect the plug of the Power Box with the mains connection (2-7)
of the Coulometer.
Note
Caution
Switch off the Coulometer correctly by pressing the red [STOP] key
before you interrupt the connection with the Power Box. If this is not
done, then there is a danger of data loss.
Caution
Under all circumstances, avoid mixing up the electrode cable from the
indicator electrode with the one from the generator electrode. Attach
corresponding markings on the screw heads of the cables.
6.2104.120
2
1 Plug the electrode plug into the Gen. socket of the Coulometer.
Note
2 Screw the 6.2104.020 electrode cable tightly onto the indicator elec-
trode.
6.2104.020
1 Plug the electrode plug into the Ind. socket of the Coulometer.
Note
1 Insert the plugs of the temperature sensor into the Temp. sockets of
the Coulometer.
Note
Always insert the red plug into the red socket. It is only this way that
the shielding against electrical interferences is ensured.
Note
Make sure that the flat side of the plug matches the marking on
the socket.
Note
The parameters for the RS-232 interfaces on the 899 Coulometer must
match those on the balance (see "Editing the COM1 settings", page
69). Also check the manual for the balance.
The following table offers an overview of the balances that you can use
together with the 899 Coulometer and of which cable you will need for
connection to the RS-232 interface:
Balance Cable
AND ER, FR, FX with RS-232 inter- 6.2125.020 + 6.2125.010
face (OP-03)
Mettler AB, AG, PR (LC-RS9) In the scope of delivery for the
balance
Mettler AM, PM, PE with interface 6.2146.020 + 6.2125.010
option 016
also from Mettler: ME 47473
or adapter and either ME 42500
hand switch or ME 46278 foot
Mettler AJ, PJ with interface
switch
option 018
Mettler AT 6.2146.020 + 6.2125.010
also from Mettler: ME 42500
hand switch or ME 46278 foot
switch
Mettler AX, MX, UMX, PG, AB-S, 6.2134.120
PB-S, XP, XS
Mettler AE with interface option 6.2125.020 + 6.2125.010
011 or 012
also from Mettler: ME 42500
hand switch or ME 46278 foot
switch
Ohaus Voyager, Explorer, Analyti- Cable AS017-09 from Ohaus
cal Plus
Precisa balances with RS-232-C 6.2125.080 + 6.2125.010
interface
Sartorius MP8, MC, LA, Genius, 6.2134.060
Cubis
Shimadzu BX, BW 6.2125.080 + 6.2125.010
6.2151.100
Caution
Note
Many USB devices need a so-called USB hub in order to work correctly.
A USB hub is a distributor to which several USB devices can be connec-
ted. USB hubs are available in specialty stores in a number of different
models.
The 6.2147.000 numerical USB keypad can, in addition to its function
as keyboard, also be used as a USB hub. It has two USB connectors.
You cannot however use these two USB connectors to connect any PC
keyboards, barcode readers or additional keypads with numerical key-
pads. These devices are recognized as input devices (like the numerical
USB keypad) and they cannot be switched in series.
The following list provides you with an overview of the various USB devi-
ces and how you can connect them to the Coulometer.
Examples:
USB stick
Printer
Figure 21 Connecting the USB hub with USB flash drive, printer and
6.2148.030 RS-232/USB Box
4 Coulometric titration
Note
Note
If you are working with the 0.1 mg/g water standard, then you
must use a glass syringe. If you are working with the 1.0 mg/g
water standard, then you may use either a plastic syringe or a
glass syringe.
4 With a folded paper towel held between thumb and index finger,
break open the ampoule at the marking.
6 Pull the piston of the syringe up to the end and swing the syringe
back and forth somewhat.
The inside of the syringe is being rinsed by water standard and freed
from water contamination.
8 Draw the rest of the water standard into the syringe, aspirating as lit-
tle air as possible.
9 Push out any air bubbles that may be present in the syringe.
10 Wipe off the needle with a lint-free paper towel and cover it with the
appropriate cap.
12 As soon as the drift on the 899 Coulometer is stable, take the syringe
by hand, press [START] and inject approx. 1 mL of the water stand-
ard through the septum.
There are two possibilities:
14 Close the syringe with the same cap and place it back on the bal-
ance.
15 Read off the value displayed by the balance and enter it on the Coul-
ometer as the sample size.
No. 209 Water content determinations in insulating oils, hydrocarbons and their
products
4.4.2 Drift
A constant drift in the range of ≤ 4 µg/min is all right. Lower values, how-
ever, are quite possible. Higher but stable values will still produce good
results, because the drift can be compensated.
A constantly high drift can be caused by water-containing deposits in
inaccessible parts of the coulometer cell. In these cases, shaking the cell
can reduce the value. Ensure that there are no drops above the liquid level
in the coulometer cell.
If you are working with a generator electrode with diaphragm, shake the
cell only hard enough that the catholyte and anolyte do not mix with one
another. If the drift remains too high for a prolonged time, even after
shaking the cell, then the electrolyte solutions should be replaced. The
catholyte should be replaced once per week.
A wet catholyte can be another reason for the excessively high drift. The
wet catholyte can be dried with a KF single-component reagent.
When you work with a Karl Fischer oven, a drift ≤ of 10 µg/min is all right.
The drift depends on the gas flow (the smaller the gas flow, the lower the
drift) and on the humidity of the surroundings.
5 Operation
Proceed as follows:
The instrument is switched off with the [STOP] key. The fact that the key
needs to be pressed down for an extended time prevents accidental
switch off.
Proceed as follows:
The current dialog title is displayed on the left-hand side of the title bar.
The current status of the system is displayed in the upper right-hand cor-
ner:
ready The instrument is in normal status.
cond.busy The working medium is being conditioned.
cond.ok The working medium is conditioned.
busy A method has been started.
hold A method has been paused.
Some dialogs have a so-called function bar on the bottom line. The func-
tions contained therein can be selected with the arrow keys [⇦] or [⇨]
and executed with [OK].
In the editing dialog for text input or numerical input, select the individual
characters with the arrow keys. Use [OK] to apply the character in the
input field. The following functions are available:
In a selection list, select the individual entries with the arrow keys [⇧] and
[⇩]. Accept the selection with [OK] or [BACK].
Variable Description
C00 Sample size
EP# Water quantity at the endpoint EP# (# = 1…9)
CI# Sample identification (# = 1…2)
R# Result (# = 1…5)
CV0# Common variable (# = 1…5)
SMN# Mean value of result R# (# = 1…5)
Var List of additional variables (see "Variables", page 39)
"#" stands for a sequential number that you must enter manually. Exam-
ple: if you apply the variable EP# in the formula, only EP is entered. You
will still need to enter the number yourself.
The meanings of the editing functions are explained in chapter 5.2.4,
page 37.
Variables
Pressing Var displays a list with additional variables. You can enter these
variables either directly into the formula or also by selecting them from the
list and applying them with [OK].
Variable Description
MCQ End quantity, i.e. total amount of removed water at the
end of the titration (in µg)
MCD Duration of the entire titration
MDC Drift for drift correction
Variable Description
DDC Time for drift correction
MIM Initial measured value, i.e. measured value prior to the
processing of the start conditions
MIT Initial temperature, i.e. temperature prior to the process-
ing of the start conditions
MCM End measured value
MCT End temperature
DD Duration of the entire determination
5.4 Methods
5.4.1 Method templates
The 899 Coulometer contains method templates which are already config-
ured except for a few parameters.
The following method templates can be selected:
KFC Coulometric Karl Fischer titration.
The blank value is not taken into account for the
calculation.
KFC-Blank Coulometric Karl Fischer titration minus the
blank value.
Blank Coulometric blank value determination.
The method templates differ only in their calculation formulas.
■ Press [BACK].
The method will be saved and the method table is displayed.
Entering a new name:
■ Press [OK].
The text editor opens.
■ Enter a method name (max. 12 characters) and apply with
Accept or [BACK].
■ Press [BACK].
The method will be saved and the method table is displayed.
Note
5.5 Control
Menu ▶ Control
In the dialog Control, the settings for the execution of a single determi-
nation or of one sample series are defined.
Sample table
If this parameter is activated, the sample data for a sample series can be
entered in a table (see Chapter 5.7, page 45).
Selection on | off
Default value off
Autostart
If this parameter is activated, a new determination is started automatically
at the end of a determination. This continues until the number specified
has been reached (see Number of autostarts).
Selection on | off
Default value off
Note
If you are working with a sample changer with oven module (e.g. 885
Compact Oven SC), then the Autostart parameter must be set to off,
because the sample changer starts the titration.
Number of autostarts
This parameter is visible only when Autostart = on.
Number of automatic starts.
Input range 1 ... 50
Selection table
Default value table
table
The number of automatic starts corresponds to the number of samples
in the sample table.
ID1
Sample identification. The sample identification can be used in calculations
as the variable CI1.
Entry max. 10 characters
Default value empty
ID2
Sample identification. The sample identification can be used in calculations
as the variable CI2.
Entry max. 10 characters
Default value empty
Sample size
Sample size. The value of the sample size can be used in calculations as
the variable C00.
Input range –999999999 ... 9999999999
Default value 1.0
Unit
Unit of the sample size.
Selection g | mg | µg | mL | µL | pieces | User-defined
Default value g
User-defined
A user-defined unit can be created. This will be added to the selection
list. The previous entry will be overwritten as soon as the new unit has
been defined.
The sample table contains numbered lines. The identification (ID1) and
the sample size of each sample are displayed.
Edit
Edit the data of the selected line, see following chapter.
Delete
Delete the selected line from the sample table.
Insert
Insert a new line above the line selected.
New
Delete the sample table completely. This function is visible only if the
instrument is in ready status.
Store
Save the sample table. The sample table is saved in the internal device
memory.
Note
You can save only one sample table. When you save a sample table,
any previously saved sample table will be overwritten automatically.
Load
Load the sample table from the internal device memory.
You will see at the very bottom the line number of the selected line and
the line number of the last line containing data. In this example, the first
line is opened and the sample table contains four lines.
One can scroll between the individual data sets with the keys [⇦] and [⇨].
Method
Method used for processing the sample.
Selection Selection of stored methods | empty
Default value empty
empty
The currently loaded method is used.
ID1
Sample identification. The sample identification can be used in calculations
as the variable CI1.
Entry max. 10 characters
Default value empty
ID2
Sample identification. The sample identification can be used in calculations
as the variable CI2.
Entry max. 10 characters
Default value empty
Sample size
Sample size. The value of the sample size can be used in calculations as
the variable C00.
Input range –999999999 ... 9999999999
Default value 1.0
Unit
Unit of the sample size.
Selection g | mg | µg | mL | µL | pieces | User-defined
Default value g
User-defined
A user-defined unit can be created. This will be added to the selection
list. The previous entry will be overwritten as soon as the new unit has
been defined.
If the sample size is sent directly from the balance, then it will always be
entered in a new line at the end of the sample table. It does not matter
which line is selected or whether the sample table is even opened. In the
above example, the sample size is entered in line 5.
Note
If you would like to enter the sample size in a particular line, then you
must open the corresponding editing dialog (i.e. the Sample data dia-
log is displayed).
If the editing dialog for the sample size is opened, then the sent value
will be ignored.
2 Starting conditioning
■ Press [START].
Conditioning starts. Conditioning not OK is displayed until the
endpoint is reached. The working medium is titrated to the endpoint.
This is indicated by Conditioning OK. The status is kept stable.
The stirring rate can be modified with the Stirrer function. The fol-
lowing dialog is opened by pressing [OK]:
The stirring rate can be reduced with Stir- and increased with Stir+.
Off switches the stirrer off. On is now displayed instead. This can be
used to switch the stirrer back on. This dialog is exited with [BACK].
3 Adding sample
■ If Conditioning OK is displayed, press [START].
Conditioning is stopped. The request for adding the sample will
be displayed for 8 s.
The sample must be added during this time.
The stirring rate can be reduced with Stir- and increased with Stir+.
Off switches the stirrer off. On is now displayed instead. This can be
used to switch the stirrer back on. This dialog is exited with [BACK].
After the completion of the titration, the results dialog is displayed:
Note
Note
Note
5.10 Results
Menu ▶ Results
After the completion of the titration, the results dialog is displayed:
The calculated result and details concerning the drift and the endpoint are
shown in the overview.
Curve
Display the curve of the current determination.
Recalculate
Recalculate the current determination. The procedure will be executed
immediately.
Statistics
Display the statistical overview of a determination series (see Chapter
5.11, page 57).
The arrow keys [⇦] and [⇨] can be used to move to the individual measur-
ing points. A cross hair is used to show the current position on the curve.
The data (water quantity, measured value, time, etc.) for the respective
measuring point is indicated on the right-hand side.
Recalculating
Note
All of the results are recalculated with the Recalculate function. This is
necessary if, for example, the calculation or the sample size has been
modified.
5.11 Statistics
Menu ▶ Results ▶ Statistics
The statistical overview of a determination series can be displayed in the
Results dialog with the Statistics function.
Note
The mean value (Mean), the absolute and the relative standard deviation
(s abs and s rel) are displayed in the overview. For the mean value, the
number of individual results from which it has been calculated is displayed
in parentheses. In this example, it is 3. The Statistics line shows how
many determinations have already been carried out and how many deter-
minations are to be carried out in total. All three determinations were car-
ried out in this example.
Details
Display additional data.
Reset
Delete all statistics data.
Increase
Add a further determination to the determination series.
The result and the sample size of each determination are shown.
On/Off
Remove the selected determination from the statistics. The line will then
be marked with an asterisk (*), the statistics will be recalculated automati-
cally. If several calculations are defined in the method, then all the results
will be removed from the statistics.
5.13.1 Stirring
Stirrers that are connected or installed in the Coulometer can be control-
led manually.
Proceed as follows:
■
■ In the function bar, select Stir- or Stir+.
The stirring rate will be increased or decreased by one step each
time the [OK] key is pressed.
The algebraic sign changes the direction in which the stirring is
done. When viewing the stirrer from above, this means:
– "+": counterclockwise rotation
– "–": clockwise rotation
6 System settings
User name
A user name can be entered here for the report. This parameter will only
be printed if a user has been defined.
Entry max. 12 characters
Default value empty
Instrument name
A instrument name can be entered here for the report. This parameter will
only be printed if a designation has been defined.
Entry max. 10 characters
Default value empty
Serial number
Serial number of the instrument. This is printed as a part of the instrument
identification in the report header.
Program version
Version number of the instrument software. This is printed as a part of the
instrument identification in the report header.
Time
Current time. Only valid numbers can be entered.
Format: hh:mm:ss
Date
Current date. Only valid numbers can be entered.
Format: YYYY:MM:DD
Language
Setting the dialog language. An additional language can be selected
besides English.
Note
Dialog type
The user dialog can be limited for routine operations. One can operate
normally with methods in the limited dialog. However, no settings can be
made or methods deleted.
The resetting of the dialog will take effect as soon as you exit the main
menu.
The limitation of the dialog results in the following:
■ The menu items System, Parameters and Control are not shown in
the main menu.
■ Methods can only be loaded, but not deleted, exported or created.
Note
If the limited dialog for routine operation is activated, then the expert
dialog cannot be activated during ongoing operation. To change the
dialog type, the 899 Coulometer must be switched off and then back
on again. The expert dialog can be forced as soon as the instrument is
started up again. Then it is possible to enter whatever settings one
wishes, e.g. the changing of the dialog type. If the instrument is
switched off again without changing the dialog type, then the routine
dialog will remain activated.
Routine
Limited dialog for routine operations.
Contrast
The contrast of the display can be adjusted with the arrow keys [⇦] and
[⇨].
■ [⇦]: the contrast will be decreased by one step each time the key is
pressed.
■ [⇨]: the contrast will be increased by one step each time the key is
pressed.
Input range 150 ... 240
Default value 212
Note
Beep
If this parameter is activated, then a short beep will sound in the following
cases:
■ When a key is pressed.
■ At the end of the determination.
■ When the system remains conditioned without interruption for 10 sec-
onds.
Selection on | off
Default value on
Proceed as follows:
Note
If you have set the parameter Statistics to on, then the mean value of
the results will be assigned to the respective common variable.
Note
This menu item is visible only if a USB flash drive has been connected as
an external storage medium.
Methods can be imported and deleted from a USB flash drive in this dia-
log. Only methods located in the Files directory are displayed in the list
(see "Directory structure on the USB flash drive", page 67).
A backup of the system can be created (all data and settings). Similarly, an
existing backup can be reloaded.
Import
Import the selected method.
Delete
Delete the selected method.
Backup
Create a backup of all data and settings on the USB flash drive.
Note
Only one backup can be created on the same USB flash drive.
If a backup is already stored on the flash drive, then this will be over-
written as soon as the function is performed once again.
Restore
Load the backup from a connected USB flash drive.
PC/LIMS report
Specification of the storage location for the PC/LIMS report. The PC/LIMS
report is a machine-readable report with all of the important data for a
determination. It can be saved as follows:
■ as a TXT file on a USB flash drive.
■ to a LIMS via an RS-232 interface. The 6.2148.030 RS-232/USB Box is
required for this purpose.
Selection COM2 | USB Stick
Default value USB Stick
COM2
The report is sent via the serial COM2 interface. The interface parame-
ters set in the dialog COM2 settings are used (see "Editing the COM2
settings", page 70).
USB Stick
The report will be saved as a TXT file on the USB flash drive in the
folder pc_lims_report.
Printer
If a printer is connected, then the printer type needs to be defined here in
order for the reports to be printed out correctly.
The printers that have the designation ESC-POS are so-called POS printers
(point-of-sale printers), i.e. they print on continuous paper.
Selection Citizen (ESC-POS) | Custom (ESC-POS) | Epson |
Epson (ESC-POS) | HP DeskJet | HP LaserJet |
Seiko (ESC-POS)
Default value Custom (ESC-POS)
Graphics width
Adjust the width of the curve to be printed out to the paper width of the
printer to be used. The default value depends on the selected printer. The
height of the curve is 2/3 of the width.
Input range 100 ... 3000 Pixels
Keyboard layout
A commercially available USB keyboard can be connected to make it eas-
ier to enter text and numbers. Specify the country-specific keyboard lay-
out.
Balance
If you have connected a balance, then you must define the balance type
here.
Selection AND | Mettler | Mettler AT | Mettler AX |
Ohaus | Precisa | Sartorius | Shimadzu
Default value Sartorius
The following table indicates the balance type that needs to be selected
for the balance model:
Baud rate
Transfer rate in characters per second.
Selection 1200 | 2400 | 4800 | 9600 | 19200 | 38400 |
57600 | 115200
Default value 9600
Data bits
Number of data bits.
Selection 7|8
Default value 8
Stop bits
Number of stop bits.
Selection 1|2
Default value 1
Parity
Type of parity testing.
Selection even | none | odd
Default value none
Handshake
Type of the data transfer protocol.
Selection hardware | software | none
Default value hardware
Note
Program files
They are instrument-specific. The file name has the following structure:
5XXXyyyy.bin where
Language files
They can be recognized by means of the two-digit language code in the
file name. A language file contains the dialog texts for various instrument
types. It is not instrument-specific. The file name has the following struc-
ture:
5848xxxxYY.bin where
Loading a file
Proceed as follows:
7 Parameters
Conditioning
If this parameter is activated, then the first time the titration is started the
working medium will be titrated to the endpoint with the specified control
parameters. The status is kept stable. The actual method run does not
begin until [START] has been pressed once more. Conditioning will be
carried out again automatically after the titration.
Selection on | off
Default value on
Start drift
If the measured drift is smaller than this value for a certain time (so-called
stabilizing time), then Conditioning OK will be displayed and the titra-
tion can be started. The stabilizing time is defined under Condition-
ing ▶ Stabilizing time.
Input range 1 ... 999 µg/min
Default value 20 µg/min
Drift correction
The end point amount can be drift-corrected. To accomplish this, the drift
is multiplied by the drift correction time and this value is subsequently sub-
tracted from the amount of the end point. The drift correction time is the
time interval between the end of conditioning and the end of the determi-
nation.
Selection auto | manual | off
Default value auto
auto
The value of the current drift is automatically applied at the start of the
titration.
manual
If the drift is known throughout a longer period of time, this can be
entered manually.
off
No drift correction takes place.
Drift value
This parameter can only be edited with Drift correction = manual.
Drift for manual drift correction.
Input range 0.0 ... 99.9 µg/min
Default value 0.0 µg/min
Automatic start
If this parameter is activated, then the determination is automatically star-
ted when the measured voltage suddenly changes. This setting will be
ignored as long as the working medium has not been conditioned.
Selection on | off
Default value off
Note
If you use the automatic start function, then we recommend that the
start drift be reduced and that a stabilizing time be defined.
Recommendation: Start drift ≤ 10 µg/min / Stabilizing time ≥ 30 s
Threshold value
This parameter can only be edited with Automatic start = on.
If the change in voltage is higher than this value, then the determination
will automatically be started.
Input range 0 ... 999 mV
Default value 50 mV
Stabilizing time
Waiting time, during which the measured drift has to be smaller than the
start drift defined until Conditioning OK is displayed. The start drift is
defined under Conditioning ▶ Start drift.
Input range 0 ... 999999 s
Default value 0s
Selection off
Default value off
Pause
Waiting time, for example for dissolving the sample. During this time no
iodine is generated.
Input range 0 ... 999999 s
Default value 0s
Request sample ID
Selection of the sample identification that is queried in the method run.
Selection ID1 | ID2 | ID1&ID2 | off
Default value off
Hold at request
If this parameter is activated, then the run will be paused during the
request. If the parameter is deactivated, then the titration will be started in
the background.
Selection on | off
Default value on
Endpoint at
Measured value for the endpoint.
Input range –1250.0 ... 1250.0 mV
Default value 50.0 mV
Selection off
Note
Titration rate
Three predefined sets of parameters can be selected for the titration rate.
Selection slow | optimal | fast | user
Default value optimal
slow
For samples with a low water content or samples which release their
moisture only slowly.
optimal
For all standard titrations. The parameters have been optimized for the
most frequent applications.
fast
For uncritical samples with high water content.
user
The individual titration parameters can be modified.
The settings of the individual titration rates are listed in table 3, page
77.
Dynamics
This parameter can only be edited with Titration rate = user.
This parameter defines the control range before the specified endpoint.
Within the control range, the iodine is generated step by step, the genera-
tion is finely controlled. The closer the endpoint, the slower the iodine is
generated until the rate defined under Min. rate is reached. The larger
the control range, the slower the titration. Outside the control range,
iodine is being continuously generated, the rate is defined under Max.
rate.
Note
Note that the parameter Dynamics is linked with the parameters End-
point at and I(pol). Explanations in this connection can be found in
chapter 10.4 Control parameters and polarization current, page 95.
Max. rate
This parameter can only be edited with Titration rate = user.
Rate at which iodine is generated outside the control range.
Input range 1.5 ... 2241.0 µg/min
Selection max.
Default value max.
Min. rate
This parameter can only be edited with Titration rate = user.
Rate at which iodine is generated at the very beginning of the titration
and in the control range at the end of the titration. This parameter has a
decisive influence on the titration rate and thus also on the accuracy. The
smaller the selected minimum rate, the slower the titration.
Input range 0.3 ... 999.9 µg/min
Default value 15.0 µg/min
Titration rate
slow optimal fast
Max. rate 1000.0 µg/min maximum maximum
Min. rate 0.3 µg/min 15.0 µg/min 30.0 µg/min
Stop criterion
The titration is canceled when the endpoint has been reached and this
stop criterion has been fulfilled. If no stop criterion has been selected then
the titration will not be canceled. The stop conditions (see Chapter 7.1.5,
page 81) always lead to a stop, even if the stop criterion has not been
reached.
Selection drift | time | rel. drift | off
Default value rel. drift
drift
The titration is canceled when the stop drift has been reached.
time
The titration is canceled if the endpoint has been exceeded during a
certain time period (Delay time).
rel. drift
The titration is canceled when the sum of the drift at the start of the
titration and the relative stop drift has been reached.
off
The titration will not be canceled until the stop conditions have been
fulfilled.
Stop drift
This parameter can only be edited with Stop criterion = drift.
The titration is canceled when the endpoint and the stop drift have been
reached.
Input range 1 ... 999 µg/min
Default value 5 µg/min
Delay time
This parameter can only be edited with Stop criterion = time.
The titration will be canceled if the following criteria are both met simulta-
neously.
■ The voltage at the indicator electrode lies in the range "endpoint +5
mV and endpoint –2 mV".
■ The time defined here has expired.
If, for example, the parameter Endpoint at is set to 50 mV and the para-
meter Delay time defined here is 10 s, then the voltage at the indicator
electrode must be between 55 mV and 48 mV for 10 seconds so that the
titration would be canceled.
Input range 0 ... 999 s
Default value 10 s
Extraction time
Minimum duration of the titration. The titration will not be canceled dur-
ing the extraction time, even if the endpoint has already been reached.
The titration is however canceled if a stop condition is fulfilled during this
time (see Chapter 7.1.5, page 81). The entering of an extraction time is
e.g. recommended with samples that release water slowly or if a Karl
Fischer oven is used.
Input range 0 ... 999999 s
Default value 0s
Generator electr.
Type of generator electrode.
Selection with diaphr. | w/o diaphr.
Default value w/o diaphr.
with diaphr.
Generator electrode with diaphragm.
w/o diaphr.
Generator electrode without diaphragm.
Generator current
Polarization current at the generator electrode.
Stirrer
The stirrer is switched on at the start of the determination when this para-
meter is activated.
Selection on | off
Default value on
Stirring rate
Setting the stirring rate. It can be set in steps of –15 to +15. The default
setting 8 corresponds to 1000 rpm. The formula for calculating the rota-
tional speed is specified in chapter 10.1, page 92. The optimum stirring
rate can be tested in the manual control.
The algebraic sign changes the direction in which the stirring is done.
When viewing the stirrer from above, this means:
■ "+": counterclockwise rotation
■ "–": clockwise rotation
Input range –15 ... 15
Default value 8
I(pol)
The polarization current is the current that is applied to a polarizable elec-
trode during the voltametric measurement.
Selection 5 µA | 10 µA | 20 µA | 30 µA
Default value 10 µA
Note
Note that the parameter I(pol) is linked with the parameters Dynamics
and Endpoint at. Explanations in this connection can be found in
chapter 10.4 Control parameters and polarization current, page 95.
Electrode test
In the case of polarizable electrodes, an electrode test can be carried out.
A check is made that the electrode is properly connected and that no
short-circuit is present. The electrode test is carried out as soon as the
determination is started.
Selection on | off
Default value off
Time interval MP
Time interval for entering a measuring point in the measuring point list.
The measuring point list is limited to 1000 measuring points.
Input range 0.1 ... 999999.0 s
Default value 2.0 s
Temperature
Temperature entered manually.
Input range –20.0 ... 150.0 °C
Default value 25.0 °C
Stop time
The titration is canceled when the specified time has elapsed since the
start of the titration.
Input range 1 ... 999999 s
Selection off
Default value off
7.1.6 Calculation
7.1.6.1 General
Menu ▶ Parameters ▶ Calculation
A maximum of five calculations can be defined in one method. A series of
variables (raw data from the determination, previously calculated results) is
available for the calculations. Definition can be made for each calculation
as to whether the result is to be saved as a common variable.
Edit
See the following chapter for editing the data of the selected calculation.
Delete
Delete the selected calculation.
Method "KFC"
Result name
The result name is the text which will be shown in the results display and
in the report.
Entry 12 characters
Default value R1: Water / R2-R5: empty
R2…R5
Display of the calculation formula. A special editor is opened for the defi-
nition (see Chapter 5.3, page 39).
Entry 30 characters
Default value empty
Decimal places
Number of decimal places used to display the result.
Input range 0 ... 5
Default value R1: 1 / R2-R5: 2
Result unit
The result unit is displayed and saved together with the result.
R1
Selection % | mg | mg/piece | mg/g | mg/mL | ppm | µg |
User-defined
Default value ppm
R2-R5
Selection % | mg | mg/piece | mg/g | mg/mL | ppm | µg |
User-defined
Default value %
User-defined
A user-defined unit can be created. This will be added to the selection
list. The previous entry will be overwritten as soon as the new unit has
been defined. A blank entry can be generated this way as well.
Save as CV
The calculated result can be saved as a method-independent variable, a
so-called common variable. The result is then also available in other meth-
ods for calculations. If Statistics has been activated, then the current mean
value of the determination series will be saved.
Selection on | off
Default value off
Method "KFC-Blank"
Result name
The result name is the text which will be shown in the results display and
in the report.
Entry 12 characters
Default value R1: Water / R2-R5: empty
CV01 is the Common Variable 01 and corresponds to the result from the
calculation of the Method "Blank", page 84.
R2…R5
Display of the calculation formula. A special editor is opened for the defi-
nition (see Chapter 5.3, page 39).
Entry 30 characters
Default value empty
Decimal places
Number of decimal places used to display the result.
Input range 0 ... 5
Default value R1: 1 / R2-R5: 2
Result unit
The result unit is displayed and saved together with the result.
R1
Selection % | mg | mg/piece | mg/g | mg/mL | ppm | µg |
User-defined
Default value ppm
R2-R5
Selection % | mg | mg/piece | mg/g | mg/mL | ppm | µg |
User-defined
Default value %
User-defined
A user-defined unit can be created. This will be added to the selection
list. The previous entry will be overwritten as soon as the new unit has
been defined. A blank entry can be generated this way as well.
Save as CV
The calculated result can be saved as a method-independent variable, a
so-called common variable. The result is then also available in other meth-
ods for calculations. If Statistics has been activated, then the current mean
value of the determination series will be saved.
Selection on | off
Default value off
Method "Blank"
Result name
The result name is the text which will be shown in the results display and
in the report.
Entry 12 characters
Default value R1: Blank / R2-R5: empty
R2…R5
Display of the calculation formula. A special editor is opened for the defi-
nition (see Chapter 5.3, page 39).
Entry 30 characters
Default value empty
Decimal places
Number of decimal places used to display the result.
Input range 0 ... 5
Default value 2
Result unit
The result unit is displayed and saved together with the result.
R1
Selection % | mg | mg/piece | mg/g | mg/mL | ppm | µg |
User-defined
Default value µg
R2-R5
Selection % | mg | mg/piece | mg/g | mg/mL | ppm | µg |
User-defined
Default value %
User-defined
A user-defined unit can be created. This will be added to the selection
list. The previous entry will be overwritten as soon as the new unit has
been defined. A blank entry can be generated this way as well.
Save as CV
The calculated result can be saved as a method-independent variable, a
so-called common variable. The result is then also available in other meth-
ods for calculations. If Statistics has been activated, then the current mean
value of the determination series will be saved.
R1
Selection on | off
Default value on
R2-R5
Selection on | off
Default value off
7.1.7 Statistics
Menu ▶ Parameters ▶ Statistics
The statistics calculation of a multiple determination is activated under
Statistics and definition is made as to how many determinations the ser-
ies contains.
Statistics
If this function is activated, then statistics calculations will be carried out
for all of the defined results.
Selection on | off
Default value off
Number of determinations
The number of determinations that are carried out for the statistics calcu-
lations.
If an additional determination has to be added to the determination ser-
ies, because one determination has been incorrect, for example, then this
can be accomplished in the statistical overview (see Chapter 5.11, page
57).
Input range 2 ... 20
Default value 3
7.1.8 Reports
Menu ▶ Parameters ▶ Reports
The reports that will be printed out automatically in connection with a
determination are defined under Reports.
Results
The result report contains the calculated results, endpoints, sample data,
etc.
Selection on | off
Default value off
Curve
Curve report. The width of the curve is defined in the system settings (see
"Graphics width", page 68).
Selection on | off
Default value off
Calculations/Statistics
Output of the calculation formulas for the individual results. Results are
specified with full accuracy. This makes recalculation with an external pro-
gram possible (see Chapter 10.9, page 103). If Statistics has been activa-
ted, then the following data will be printed out as well:
■ Result and sample size of the individual determinations
■ Mean value as well as absolute and relative standard deviation
Selection on | off
Default value off
Parameters
All of the parameters of the current method are printed out in the para-
meter report.
Selection on | off
Default value off
PC/LIMS
The PC/LIMS report is a machine-readable report with all of the data
important for a determination. The PC/LIMS report can be saved as a TXT
file on a USB storage medium or sent via an RS-232 interface to a LIMS.
The output location is defined in the system settings (see "PC/LIMS
report", page 68).
The file name of the TXT file is constructed as follows: PC_LIMS_Report-
ID1-YYYYMMDD-hhmmss.txt.
Selection on | off
Default value off
Validation
Please contact your local Metrohm agent for support in validating instru-
ments and software. Here you can also obtain validation documentation
to provide help for carrying out the Installation Qualification (IQ) and
the Operational Qualification (OQ). IQ and OQ are also offered as a
service by the Metrohm agents. In addition, various application bulletins
are also available on the subject, which also contain Standard Operat-
ing Procedures (SOP) for testing analytical measuring instruments for
reproducibility and correctness.
Maintenance
Electronic and mechanical functional groups in Metrohm instruments can
and should be checked as part of regular maintenance by specialist per-
sonnel from Metrohm. Please ask your local Metrohm agent regarding the
precise terms and conditions involved in concluding a corresponding
maintenance agreement.
Note
9 Troubleshooting
9.1 Karl Fischer titration
Problem Cause Remedy
The drift is very high The coulometer cell is not ■ Check the septum and replace it if neces-
during conditioning. leak-proof. sary.
■ Replace the molecular sieve.
■ Check the ground-joint sleeves for frayed
edges. If necessary, trim the edges cleanly
or replace the ground-joint sleeves.
The diaphragm of the gen- ■ Clean the diaphragm (in accordance with
erator electrode is conta- directions in the leaflet for the generator
minated. electrode).
The gas flow from the KF ■ Reduce the gas flow (if you are working
oven into the coulometer with the oven method with sample vials,
cell is too high. set the gas flow between 40…60 mL/min).
The drift becomes The sample releases water ■ Possibly use a KF oven.
greater after each very slowly. ■ See technical literature.
titration.
The drift is fluctuat- The sample solution is ■ Set the stirring rate in such a way that the
ing. poorly stirred. sample solution will become very well
mixed.
The titration time is The drift during condition- ■ Wait before starting the titration until the
too long. ing is not stable. drift has become stable.
The parameter Stop drift ■ Set the Stop drift higher or use the Rela-
is set too low. tive stop drift.
The water quantity is too ■ Observe the sample size and water con-
high. tents in accordance with Table "Recom-
mended sample sizes", page 31.
The result is too The coulometer cell is not ■ Shake the coulometer cell and wait until
high. yet correctly conditioned. the drift is stable.
The parameter Stop drift ■ Set the Stop drift higher or use the Rela-
is set too low. tive stop drift.
The drift correction is too ■ Start the titration as long as the gas flow
small (e.g. with the use of still exists between the conditioning vial
a KF oven or with manual and the coulometer cell.
drift correction). ■ Set the parameter Drift correction to
auto (= automatic drift correction).
The result is too The sample releases iodine. ■ Possibly use a KF oven.
low. ■ See technical literature.
The results are The sample is nonhomoge- ■ Homogenize the sample if possible.
spread widely. nous. ■ Possibly use a larger sample size.
9.2 Miscellaneous
Problem Cause Remedy
No report is printed. The printer is not recog- ■ Switch the 899 Coulometer off and then
nized by the instrument. back on again.
■ Use a hub on the USB connector and con-
nect the printer to the hub.
The printer model is not Use a printer which fulfills the required specifi-
compatible. cations (see Chapter 10.3.4, page 95).
The USB keyboard The keyboard or mouse is ■ Switch the 899 Coulometer off and then
or the PC mouse not recognized by the back on again.
does not function. instrument. ■ Use a hub on the USB connector and con-
nect the keyboard or mouse to the hub.
The keyboard or the mouse Use a model which fulfills the required specifi-
is not compatible. cations (see Chapter 10.3, page 93).
The display is no The contrast is set incor- Adjust the contrast correctly (see Chapter 6.1,
longer readable. rectly. page 62).
Message 020-511 The USB flash drive is no 1. Connect the USB flash drive.
"Action not possi- longer connected. 2. Switch the instrument off and then back
ble" is displayed. on again.
The USB flash drive is full. ■ Use a different USB flash drive.
■ Delete files with the aid of a PC.
10 Appendix
Example:
Stirring rate set: 8
Rotational speed in rpm = 125 · 8 = 1000
r/min
2000
1500
1000
500
-15 -10 -5 0 5 10 15
Figure 25 Rotational speed depending on stirring rate
10.2 Balance
The sample size and the associated unit can be sent from a connected bal-
ance. The sample size is transmitted as a number with up to ten charac-
ters (including algebraic sign and decimal point).
Sample size and unit are sent as a single character string. They are separa-
ted by a space character. The string is terminated with the ASCII charac-
ters CR and LF.
If the balance sends a negative sample size (e.g. when you are reweighing
a sample), then the algebraic sign is adopted. The algebraic sign is, how-
ever, ignored for the calculations.
Note
With some balances, the sample identification and the method can be
sent in addition to the sample size.
Make sure that the balance does not send the sample size until the end.
Mettler AX
For the Mettler AX balance, the fields that contain the sample identifica-
tion or the method must be designated as follows:
■ Designation for the field with the method name: METHOD
■ Designation for the field with sample identification 1: ID1
■ Designation for the field with sample identification 2: ID2
Note
Note
The lettering of the USB keyboard may differ from above lettering,
depending on the country-specific keyboard used.
10.3.3 PC mouse
In order to make navigating in the dialog of the 899 Coulometer easier, a
PC mouse can be connected.
10.3.4 Printer
The range of USB printers available is extremely varied and constantly
changing. The following points must be taken into account when select-
ing a printer:
■ USB interface necessary
■ Printer language: HP-PCL, Canon BJL Commands, Epson ESC P/2 or
ESC/POS
Note
Inexpensive printers are often designed solely for use with a PC and
may not be equipped with one of the printer languages listed above.
Such models are not suitable for this reason.
Measured value / mV
Ipol = 30 µA
Ipol = 20 µA
Control range
Ipol = 10 µA Endpoint
Ipol = 5 µA
Ipol = 2 µA
Water / µg
Figure 26 Control parameters and polarization current
The diagram shows Karl Fischer titration curves at different polarization
currents (Reagent Coulomat AD). It is clear to see that the position of the
endpoint varies with the polarization current. The curves have different
slopes, i.e. the dynamics must also be adapted. Polarization currents < 10
µA are not suitable for this application. The following table gives you an
idea of the optimal control parameters for various polarization currents.
Stabilizing time 30 s 30 s
>Start conditions
>Titration parameters
Stirring rate 12 12
>Statistics
Statistics on –
Number of determina- 3 –
tions
>Reports
Results on on
Calculations/Statistics on –
Caution
All user data (methods, etc.) are deleted if a system initialization is car-
ried out. Afterwards, the instrument will have the factory settings again.
We recommend creating a backup of the system at regular intervals in
order to avoid data losses.
Note
9 6
6 9
Figure 27 Pin assignment of remote socket and remote plug
The above figure of the pin assignment applies for all Metrohm instru-
ments with 9-pin D-Sub remote connector.
Inputs
+5 V approx. 5 kΩ Pull-up
tp
tp > 100 ms
active = low, inactive = high
Outputs
Open Collector
tp
tp > 200 ms
active = low, inactive = high
IC = 20 mA, VCEO = 40 V
+5 V: maximum load = 20 mA
Output 1
Titr/Determ Output 2
condOK Output 3
Error Output 4
Start Input 0
Stop Input 1
[STOP]
6.2134.040
Interface parameters
We recommend the following parameters for the RS-232 interface
COM2:
■ Baud rate: 19200
■ Data bits: 8
■ Stop bits: 1
■ Parity: none
■ Handshake: software
On the 899 Coulometer, adjust the interface parameters under
Menu ▶ System ▶ External devices ▶ COM2 settings.
Transfer protocol
The data communication is synchronous. On each command there is an
acknowledgement by the instrument.
A command must be sent to the instrument with the control characters
CR LF as terminator. The acknowledgements of the instrument will also
be transferred with CR LF as terminator.
The instrument does not send spontaneous messages.
The values of the variables are only available after the end of a determina-
tion (in the status 'ready').
Acknowledgement of Comment
the instrument
OK Command executed
E1 Method not found
E2 Invalid variable
E3 Invalid command
Rounding-off process
Measured values and results are rounded to the defined number of deci-
mal places (commercial rounding, in accordance with the US Pharmaco-
peia USP). If the digit at the first dropped decimal place is 1, 2, 3 or 4,
then it will be rounded off; if this digit is 5, 6, 7, 8 or 9, then it will be
rounded up. Negative digits will be rounded in accordance with their
amount, i.e. away from zero.
Examples:
2.33 yields 2.3
2.35 yields 2.4
2.47 yields 2.5
–2.38 yields –2.4
–2.45 yields –2.5
Statistics
The arithmetic mean value and the absolute and relative standard devia-
tions of results are calculated:
You can statistically evaluate a maximum of five results (1 ≤ k ≤ 5) calcula-
ted in a determination. A statistical series can contain a maximum of 20
determinations (1 ≤ n ≤ 20).
The following convention applies to the subsequent formulas:
1 ≤ n ≤ 20 and 1 ≤ k ≤ 5.
Mean value:
Explanations
The individual values are incorporated in the statistics with full accuracy.
15 significant places are yielded when the 64 bit numerical format is
applied for the floating-point number in decimal presentation.
The accuracy can be controlled by the selection of the prefix of the unit
(milli, micro) and the number of decimal places.
Example:
The result displayed, 1234.56789158763 mg/L, has 15 significant pla-
ces. It should be rounded off to three decimal places according to the
above rounding-off process:
■ 1234.568 mg/L.
If the same result is expressed in "g/L" (1.23456789158763 g/L), and is
also rounded off to three decimal place, this yields
■ 1.235 g/L.
I.e. you obtain the lowest losses in accuracy with rounding when you
select the application and the numerical format in such a way that the
numbers displayed have as many places before the decimal point as possi-
ble.
A complete recalculation of the statistics using a pocket calculator or PC
calculation programs may exhibit deviations. This can be explained by the
different binary numerical formats used by these computers.
Note
11 Technical specifications
11.1.2 Temperature
One measuring input (Temp.) for one Pt1000-model temperature sensor.
Measuring range –150…+250 °C
Resolution 0.1 °C
Measuring accu- ±0.2 °C
racy (Applies for measuring range –20…+150 °C; ±1 digit; without sensor
error, under reference conditions.)
Design and testing According to EN/IEC/UL 61010-1, CSA-C22.2 No. 61010-1, protection
class III (external power supply unit).
Safety instructions This document contains safety instructions which have to be followed
by the user in order to ensure safe operation of the instrument.
Immunity
Standards fulfil- ■ EN/IEC 61326-1
led ■ EN/IEC 61000-6-2
■ EN/IEC 61000-4-2
■ EN/IEC 61000-4-3
■ EN/IEC 61000-4-4
■ EN/IEC 61000-4-5
■ EN/IEC 61000-4-6
■ EN/IEC 61000-4-11
■ EN/IEC 61000-4-14
■ EN/IEC 61000-4-28
■ NAMUR
11.10 Dimensions
Width 143.5 mm
Height (without 112 mm
titration vessel
holder)
Height (with titra- 195 mm
tion vessel holder)
Depth 281.5 mm
Weight (including 2800 g
power supply unit)
Material
Housing PBT
Material
Base Stainless steel 1.4301
12 Warranty (Guarantee)
Metrohm guarantees that the deliveries and services it provides are free of
errors in materials, design or manufacturing.
The general warranty period is 36 months (exclusions below) from the
date of delivery or 18 months in the event of continuous operation. The
warranty remains valid on the condition that the service is provided by an
authorized Metrohm Service Organization at defined intervals and with a
defined scope.
The warranty period for the suppressors "MSM II" and "MSM-HC" is 120
months from the date of delivery or 60 months in the event of continuous
operation.
The warranty period for IC separation columns is 12 months from the date
of delivery or 6 months in the event of continuous operation. The techni-
cal specifications contained in the manual are authoritative for warranty of
accuracy.
For third-party components that are recognizable as such, the manufac-
turer's warranty regulations apply.
Consumables and materials with limited storage life and glass breakage in
the case of electrodes or other glass parts are excluded from the warranty.
Warranty claims cannot be asserted if the customer has failed to meet his
payment obligations according to schedule.
During the warranty period, Metrohm undertakes either to replace free of
charge or to credit the purchaser for any instruments, assemblies or com-
ponents that can be shown to be faulty. Any transport or customs fees
that may apply are the ordering party’s responsibility.
The precondition for this is that the ordering party must use the Return
Material Authorization (RMA) to report the faulty part, along with specifi-
cation of the article number, the article designation, an adequate error
description, the delivery date and (if applicable) the serial number. In addi-
tion, the ordering party undertakes to store the faulty part for at least 2
years in accordance with current storage directives (in compliance with
ESD guidelines) and to hold it in readiness for onsite inspection or for
return shipment to Metrohm. Metrohm reserves the right to invoice the
ordering party for these articles, including retroactively, in the event of
noncompliance with these pre-conditions.
Deficiencies arising from circumstances that are not the responsibility of
Metrohm, such as improper storage or improper use, etc. are expressly
excluded from the warranty.
13 Accessories
Note
13.1.2 2.899.0110
13.1.3 2.899.1010
13.1.4 2.899.1110
13.1.5 2.899.2110
13.1.6 2.899.3110
Index
A Water standard .................. 29 Instrument diagnosis ................ 71
Adapter Working conditions ............ 33
Connect ............................. 24 Curve ....................................... 56 K
Addition and aspiration tube Karl Fischer
Mounting ........................... 13 D Coulometry ........................ 28
Adsorber tube Determination Karl Fischer oven
Fill ........................................ 9 Cancel ................................ 52 Method examples ............... 97
Application Bulletin .................. 31 Carry out ............................ 49 Using .................................. 14
Result ................................. 56 Karl Fischer titration
B Diagnosis ................................. 72 Troubleshooting ................. 89
Backup ..................................... 66 Dialog language ....................... 62 Keyboard
Balance .............................. 49, 92 Load ................................... 71 Connect ............................. 24
Connect ............................. 22 Dialog type ............................... 63 Key assignment ............ 93, 94
Interface parameters ........... 69 Directory structure .................... 67 Keyboard layout ....................... 68
Balance type ............................. 69 KFC
E Parameters ......................... 73
C Electrical connection
Calculation Power Box .......................... 15 L
Method "Blank" .................. 84 Power supply unit ............... 14 Language ................................. 62
Method "KFC" .................... 82 Electrode Language file
Method "KFC-Blank" .......... 83 Connect ............................. 17 Load ................................... 71
Numerical format ............. 103 Electrode connector Live modifications ..................... 52
Rounding-off process ....... 103 Double Pt wire electrode ...... 7 Live parameters ........................ 55
Catholyte Generator electrode ............. 7
Replacing ........................... 34 Indicator electrode ............... 7 M
Common variable ..................... 65 Electrostatic charge .................... 4 Mains connection ....................... 7
Edit .................................... 65 End of Determination EOD ..... 100 Mains voltage ............................. 4
Common Variable Endpoint Manual control
Delete ................................ 65 Dependency ....................... 95 Stirring ............................... 60
Set to invalid ...................... 65 Expert dialog ............................ 63 Method
Conditioning Delete ................................ 66
Parameters ......................... 73 F Export ................................ 42
Contrast ................................... 64 Formula editor .......................... 39 Import ................................ 66
Control ..................................... 43 Front of the instrument .............. 6 Save ................................... 41
Autostart ............................ 43 Method examples
Sample table ...................... 43 G Karl Fischer oven ................ 97
Control parameters .................. 76 Generator electrode Method template
Control range Filling ................................. 12 Load ................................... 40
Dependency ....................... 95 GLP .......................................... 88 Molecular sieve
Coulometer Graphics width ......................... 68 Replacing ........................... 10
Set up .................................. 8 Guarantee .............................. 110 MSB
Coulometer cell Connector ............................ 7
Equipping ........................... 11 I Multiple determination
Filling ................................. 12 Indicator electrode Statistics calculation ............ 85
Inserting ............................... 9 Warm-up time .................... 34
Coulometry Initialization .............................. 98 N
Drift ................................... 33 Instrument Navigate ................................... 37
Practical tips ....................... 29 Set up .................................. 8 Numerical input ........................ 37
Principle ............................. 28 Switch off ........................... 35
Sample size ........................ 31 Switch on ........................... 35
O Report Stirrer
Operation Print manually .................... 59 Connect ............................. 21
General .............................. 36 Select ................................. 86 Stirring rate .............................. 92
Oven module ........................... 14 Result ....................................... 56 Stop conditions
Recalculate ......................... 57 Parameters ......................... 81
P Rounding-off process ....... 103 Switch off ................................. 35
Parameters Save as a common variable . 65 Switch on ................................. 35
Calculation ......................... 81 Result report System initialization .................. 98
Conditioning ...................... 73 Define ................................ 86
Dependency ....................... 95 Routine dialog .......................... 64 T
KFC .................................... 73 RS-232 Temperature sensor
Modify live ......................... 55 Interface parameters ........... 70 Connect ............................. 17
Start conditions .................. 75 RS-232 connection ................. 101 Text input ................................. 37
Stop conditions .................. 81 Titration cell
Titration ............................. 79 S Equipping ........................... 11
PC/LIMS report ......................... 68 Safety instructions ...................... 3 Filling ................................. 12
Pin assignment ......................... 99 Sample Inserting ............................... 9
Polarization current Liquid ................................. 32 Titration parameters ................. 79
Dependency ....................... 95 Solid ................................... 32 Troubleshooting ....................... 89
Preparation time Sample changer
Generator electrode with dia- Connect ............................. 27 U
phragm .............................. 33 With oven module .............. 14 Update
Generator electrode without Sample data Dialog language ................. 71
diaphragm .......................... 33 Enter .................................. 44 Program version ................. 71
Print ......................................... 59 Modify live ......................... 52 USB .......................................... 93
Printer ................................ 68, 95 Sample size Numerical keypad ............... 93
Connect ............................. 24 Send from a balance ..... 49, 92 PC keyboard ....................... 94
Program crash .......................... 98 Size .................................... 31 PC mouse ........................... 95
Program version Sample table ............................ 45 Printer ................................ 95
Update ............................... 71 Insert line ........................... 48 USB (OTG)
Load ................................... 47 Connector ............................ 7
Q Modify live ......................... 53 USB device
Quality Management ................ 88 Save ................................... 47 Adapter .............................. 24
Sensor Connect ............................. 24
R Connect ............................. 17 USB flash drive
Reagent replacement ................ 34 Sensor connector Directory structure .............. 67
Rear of the instrument ................ 7 Pt1000 ................................. 7 User name ................................ 62
Recalculate ............................... 56 Temperature sensor .............. 7
Remote Service ....................................... 3 V
Connector ............................ 7 Service Agreement ................... 88 Validation ................................. 88
Interface ............................. 99 Start conditions
Pin assignment ................... 99 Parameters ......................... 75 W
Status diagram ................. 100 Statistics ................................... 57 Warranty ................................ 110
Remote connector Statistics calculation .................. 85 Water standard
Sample changer .................. 27 Certified ............................. 29
Remote control ...................... 101