Metrohm 787KF User Manual

CH-9101 Herisau/Switzerland E-Mail info@metrohm.com Internet www.metrohm.com
787 KF Titrino
Program version 5.787.0010
Instructions for Use
Table of contens

Table of contents

1 Introduction ..........................................................................................................1
1.1 Instrument description...........................................................................................1
1.2 Controls and parts................................................................................................. 2
2
Manual operation..................................................................................................6
2.1 Keypad ..................................................................................................................6
2.2 Principle of data input............................................................................................ 7
2.3 Tutorial ................................................................................................................... 8
2.3.1 Entering data, setting the dialog language....................................................8
2.3.2 Titer determination .......................................................................................10
2.3.3 Karl Fischer titration .....................................................................................15
2.3.4 Drift...............................................................................................................16
2.4 Selection of the mode, key <MODE> ................................................................ 18
2.5 Configuration, key <CONFIG>...........................................................................19
2.6 Parameters, key <PARAM> ............................................................................... 22
2.6.1 Parameters for SET ...................................................................................... 22
2.8 Result calculations............................................................................................... 31
2.9 Drift display, key <DRIFT> ................................................................................. 36
2.10 Data output ...................................................................................................... 37
3
Error messages, Troubleshooting.....................................................................39
3.1 Error and special messages................................................................................ 39
3.2 What can you do if the data transfer does not work?.......................................... 41
3.3 Diagnosis............................................................................................................. 42
3.3.1 General......................................................................................................... 42
3.3.2 Procedure..................................................................................................... 42
3.3.3 Equipment required: ....................................................................................43
3.3.4 Diagnosis steps ...........................................................................................43
3.4 Initialise and test RAM ......................................................................................... 52
3.5 Releasing a locked spindle with inserted Exchange Unit.................................... 53
4
Preparations .......................................................................................................53
4.1 Setting up and connecting the instruments ........................................................53
4.1.1 Titrino with Titration Stand or Stirrer .............................................................53
4.1.2 Connection of a printer ................................................................................54
4.1.3 Connection of a balance..............................................................................55
4.1.4 Connection of a KF Oven............................................................................. 57
4.1.5 Connection of the 774 Oven Sample Processor.......................................... 57
4.1.6 Connection of a Sample Changer ...............................................................58
4.1.7 Connection of a recorder ............................................................................. 59
4.1.8 Connection of a computer ........................................................................... 60
4.2 Connection of electrodes, preparing titration vessel...........................................61
5
Appendix.............................................................................................................63
5.1 Technical specifications ......................................................................................63
5.2 Pin assignment of the "Remote" socket............................................................... 65
5.2.1 Lines of the "Remote" socket during the titration ......................................... 67
5.3 RS232 interface ...................................................................................................68
787 KF Titrino
Table of contents
5.4 Validation / GLP................................................................................................... 69
5.5 Warranty and conformity ..................................................................................... 70
5.5.1 Warranty....................................................................................................... 70
5.5.2 EU Declaration of conformity....................................................................... 71
5.5.3 Certificate of Conformity and System Validation ......................................... 72
5.6 Scope of delivery and ordering designations ..................................................... 73
Index...........................................................................................................................77
787 KF Titrino
1.1 Instrument description

1 Introduction

1.1 Instrument description

The 787 KF Titrino is a fast and precise titrator for the water determination according to Karl Fischer. With the Metrodata VESUV Software determination data can be saved on a PC.
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1.2 Controls and parts

1.2 Controls and parts

Front view of instrument:
787 KF Titrino
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1.2 Controls and parts
1 Exchange Unit
2 Display
3 Setting of display contrast
4 Controls the dosing rate during manual dosing with <DOS> and subse-
quent filling
5 Control keys and indicator lamps on the Titrino
Key <DOS> Dosing key. Dispensing is performed as long as <DOS> is being
pressed. Used e.g. to prepare the Exchange Unit. The dispensing rate can be set with potentiometer (4).
Key <STOP/FILL> - Stops procedures, e.g. titrations, conditioning.
- Filling after manual dosing with <DOS>.
Key <START> Starts procedures, e.g. titrations, conditioning.
Identical with key <START> of the separate keypad. Indicator lamp: "Cond." Lamp flashes during conditioning. Lamp is on when the titration
cell is conditioned.
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1.2 Controls and parts
Rear view of instrument:
787 KF Titrino
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1.2 Controls and parts
6 RS232 interface
for the connection of printer, balance or a computer
7 Remote lines
(input/output) for the connection of Sample Changers, robots etc.
8 Connection for the KF electrode
9 Connection for separate keypad
10 Analog output for the connection of a recorder
11 Connection for power cable
With power supplies where the voltage is subject to severe HF disturbances, the Ti­trino should be operated via an additional power filter, e.g. Metrohm 615 model.
12 Mains switch
13 Earthing socket
14 Connection for Ti Stand or stirrer
703 Ti Stand or 728 Magnetic Stirrer Supply voltage: 9 VDC (I 200 mA)
15 Display of the set mains voltage
Before switching on for the first time, check that the set mains voltage matches the voltage of your power supply. If this is not the case, disconnect mains cable and change voltage.
16 Rating plate
with fabrication, series and instrument number
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2.1. Keypad

2 Manual operation

2.1 Keypad

CONFIG Configuration, see page 19. PARAM Parameters, see page 22. CALC DATA Result calculation, see page 31. These keys are opening the corresponding menus.
For the principle of data input see page 7.
DRIFT ON/OFF switching of the drift display,
see page 36.
UNIT Unit of result and sample size, see
page 34.
SELECT Selection of special values (dialog
marked with ":") MODE Mode selection, see page 18. PRINT Printing of reports, see page 37. CLEAR Clears values, set special values. ENTER Stores values. STOP Stops methods. QUIT Quits inquiries, waiting times, printing. START Starts methods.
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2.2 Principle of data input

2.2 Principle of data input

KFT ********
KFT ******** >KF device settings
KFT ******** >peripheral units
KFT ******** send to: IBM
KFT ******** >auxiliaries
KFT ********
The first line of the display always shows the active mode (in this case "KFT") and the state of the Titrino. "********" means the Titrinos is in its standby state.
The keys <CONFIG>, <PARAM> and <CALC DATA> are opening the corresponding menus.
Pressing one of this keys shows the first group of inquiries of the corresponding menu in the second line of the display.
Example key <CONFIG>: You opened the configuration menu, the second line of the display shows the first group of inquiries of this menu ">KF device settings".
By pressing <CONFIG> repeatedly you can move to the other titles of this menu. With pressing <CONFIG> 2 times you go to the group of inquiries "peripheral units".
If a dialog text is marked with ">", it contains a group of inquiries. You branch into this group by pressing <ENTER>.
Example first inquiry of the group "peripheral units": Now you opened the first inquiry of the group pe­ripheral units in the configuration menu and you can change the setting.
If a dialog text of an inquiry is marked with ":", you can select a value with the key <SELECT>.
A value is stored with <ENTER> and the cursor moves to the next inquiry.
Repeated pressing of <ENTER> moves you through the inquiries of the group ">peripheral units“, after the last inquiry of this group you leave this group and return to the level above. The next group of the menu "configuration“ appears: ">auxiliaries“
With key <QUIT> you leave an inquiry or a group of inquiries, it always
In this example you leave the menu "configuration" by pressing <QUIT> and return to the standby state with the display of the titration mode.
moves you one level up.
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2.3. Tutorial

2.3 Tutorial

This short operating course teaches you to work quick and efficient with the 787 KF Ti­trino, by means of the most important applications.
Set up your Titrino and connect the peripheral devices needed, see chapter 4.

2.3.1 Entering data, setting the dialog language

We can thus make a start and first take a look at the fundamentals of the entry of data. We change the dialog language.
KFT ********
<CONFIG>
KFT ******** >KF device settings
3 × <CONFIG>
KFT ******** >auxilliaries
<ENTER>
KFT ******** dialog: english
<SELECT>
KFT ******** dialog: español
<ENTER>
KFT ******** fecha 2002-03-27
Switch on the Titrino. It is now in the standby state, it shows you the active mode.
Press the key <CONFIG>, the display shows:
This is the title of the group "KF device settings". This group contains various inquiries for the KF titra­ton.
Press <CONFIG> 3 times. You see the titles of the other groups of inquiries in the configuration menu. The display shows
This "auxiliaries" group contains the inquiry for the dialog language.
Pressing the <ENTER> key takes you to the inquir­ies of the group "auxiliaries". Note the ">" sign. All ti­tles of inquiry groups are prefixed by this sign.
This is the first inquiry of the "auxiliaries" group: the selection of the dialog language.
You select the various dialog languages with the <SELECT> key. Press <SELECT> repeatedly until "español" appears in the display. Note the sign ":". It appears if the values can be se­lected with the key <SELECT>.
Accept the new "value" with <ENTER>. The next inquiry "fecha" (date) of the group "ajustes varios" (auxiliaries) is shown.
You can open this inquiry by pressing <ENTER> too and go through all the inquiries of this group this
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2.3 Tutorial
<QUIT>
KFT ******** >ajustes varios
<QUIT>
KFT ********
way. Because this inquiry follows no colon ":" the value can't be selected by <SELECT>, the date "fecha" has to be entered with the numeric keys.
Exit the inquiries with <QUIT>. You are one level higher in the "configuration" menu showing the title "ajustes varios" (auxiliaries).
Press <QUIT> once again to exit the "configuration" menu and return to the standby state.
All the dialog texts will now be displayed in Spanish. If you prefer English as the displayed dialog lan­guage, proceed as before and select "English".
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2.3. Tutorial

2.3.2 Titer determination

Set up your titration vessel, see page 61f and plug your KF electrode into the measuring input ('KF electr.'). Put a Exchange Unit with KF reagent on the Titrino and rinse the tubing and the buret tip with <DOS>. Fill the buret again with <STOP/FILL>. Fill your titration vessel with solvent, put a stirrer bar in the titration vessel and switch on the stirrer.
For the titer determination you need water and a syringe that allows the exact dispensing of 30 µL.
Selection of the mode
<MODE>
KFT ******** TITER with H2O or Std.
<ENTER>
TITER ********
Briefly check a few settings under the <PARAM> key:
2 × <PARAM>
TITER ******** >preselections
<ENTER>
TITER ******** conditioning: ON
<ENTER>
TITER ******** req.ident: OFF
<ENTER>
TITER ******** req.smpl size: ON
<ENTER>
TITER ******** report: OFF
Press <MODE> repeatedly until "TITER with H2O or std." appears in the display.
Confirm "TITER with H2O or std." with <ENTER>.
The mode "TITER" is active and instrument is in its standby state
Press <PARAM> twice so that the title "preselec­tions" appears in the display:
View the individual inquiries of this group with <ENTER>. The following values should be set:
Automatic drying of the titration cell before and be­tween titrations: "ON".
Request of the sample identification after the titration start: "OFF".
Request of the sample size after the titration start: "ON".
If no printer is attached, the report printout after the titration must be switched off.
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2.3 Tutorial
or
TITER ******** report: short
With a connected printer, the short report, for example, can be selected.
<ENTER>
If you have to alter one of these settings, you can do this with the <SELECT> key.
Your titration vessel already contains solvent. Start with <START>. First the titrations cell is dried. The display shows
TITER wait
as long as the vessel is still wet and the green "Cond." lamp flashes. As soon as the titra­tion vessel is dry and hence ready for operation, this is shown by
TITER conditioning
an the "Cond."-LED lights continuously.
To determine the titer we shall perform several titrations and store the mean value as "titer".
Calculating the mean value and standard deviation
Check that the mean value calculation is switched on:
2 × <CALC DATA>
TITER ******** >statistics
<ENTER>
TITER ******** mean: n= 20
2 × <QUIT>
Press <CALC DATA> twice until the display shows
the title of the group is "statistics". Press <ENTER>.
Number of single determinations for the calculation of the mean value. Since the mean value is recalculated after every determination, the maximum value can re­main set at 20. The mean calculation is terminated when the operating mode is changed.
Exit the inquiry.
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2.3. Tutorial
Determination
<START>
KFR volume 0.000 ml smpl size 1.0 g
0.03
<ENTER>
KFR volume 1.426 ml #======
KFR volume 5.632 ml titer 5.3267 mg/ml
Now prepare the sample, e.g. 30 µL water and start the titration with <START>. The display shows
Inject the sample and enter the weight in g:
If you have connected a balance, you can also back­weigh the syringe.
The titration now runs. The first line of the display shows the current volume. In addition, a "" appears when dispensing is being per­formed. A "control bar" appears on the second line and shows the control deviation of the current measured value from the set endpoint.
On completion of the titration, the first line shows the dispensed volume and the second the calculated titer.
If you have connected a printer, a report is also printed:
date 2002-03-27 time 13:55:10 3 smpl size 0.03 g titer 5.3267 mg/ml ============
Perform another determination.
On completion of the titration, the mean value of the two determinations is calculated. The report on the printer has the following appearance:
date 2002-03-27 time 13:55:10 3 smpl size 0.03 g titer 5.3686 mg/ml mean (2) 5.3477 mg/ml +/-s 0.02973 mg/ml s(rel) 0.56 %
============
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2.3 Tutorial
Viewing the statistics data
If you have not connected a printer, you can view the statistics data on the display with <SELECT>.
KFR volume 5.676 ml titer 5.3686 mg/ml
<SELECT>
KFR volume 5.676 ml mean (2) 5.3477 mg/ml
<SELECT>
KFR volume 5.676 ml +/-s 0.02973 mg/ml
<SELECT>
KFR volume 5.676 ml s(rel) 0.56 %
<SELECT>
From the result display "titer", switch to the display of the mean value with <SELECT>.
Mean value of 2 determinations.
Press <SELECT> again and the standard deviation is shown.
Absolute standard deviation.
Pressing <SELECT> once more leads to the
relative standard deviation.
<SELECT> returns you to the result display.
Repeat the titer determination once more.
With a connected printer you may want a printout of the single results that are used for the statistics calculation: press the key sequence <PRINT><1><ENTER>.
Let us assume that you have discovered that one of the values is an "outlier" and you would like to delete it.
Deleting a result in the mean value calculation
2 × <CALC DATA>
KFR volume 5.676 ml >statistics
2× <ENTER>
KFR volume 5.676 ml res.tab: original
<SELECT>
KFR volume 5.676 ml res.tab: delete n
<ENTER>
787 KF Titrino
In our example, the deviation of the second result is excessive. We thus wish to delete it:
Press <CALC DATA> twice. The display shows:
Open with <ENTER> the inquiry of the result table
"res.tab:"
Press <SELECT> to display "delete n". This means that you wish to delete a single result with the index n in the result table.
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2.3. Tutorial
KFR volume 5.676 ml delete n= 1
<2>
<ENTER>
2 × <QUIT>
Enter the index of the result you wish to delete, in our case the second:
Exit the inquiry with <QUIT>.
Mean value and standard deviation are recalculated and can be viewed in the display.
If you have connected a printer, a new report is printed out.
Following this titer determination, you now decide to perform Karl Fischer determinations. The titer just determined will be automatically used here.
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2.3 Tutorial

2.3.3 Karl Fischer titration

<MODE>
KFR volume 5.676 ml KFT
<ENTER>
KFT conditioning
<CALC DATA>
3 × <ENTER>
KFT conditioning titer 5.3326 mg/ml
2 × <QUIT>
Now prepare your sample and titrate it.
Select the "KFT" mode: Press <MODE> repeatedly until the display shows
Accept this mode with <ENTER>
The instrument is in the KFT mode and the titration cell is ready for operation.
Check briefly that the titer just determined has also been adopted: Press <CALC DATA>, branch to the group "calculation" with <ENTER> and then press <ENTER> two times more to display the following inquiry.
Exit the inquiry by pressing <QUIT> twice.
Result calculation and unit of the result
The result is calculated by the following formula:
=
)content(water
<UNIT>
KFT volume 3.459 ml result unit: %
2 × <SELECT>
<ENTER>
KFT volume 3.459 ml result unit: mg/ml;3
<1>
<ENTER>
Change the unit of the result to mg/mL: Press <UNIT>. The display shows:
You wish to have your result in mg/mL. Press <SELECT> repeatedly until "mg/ml" appears in the display.
Press <ENTER>. The number of decimal places is shown after the separator ";". The "3" flashes to show you that you can now enter a number. Enter here, e.g. 1 decimal place and exit the inquiry by pressing <QUIT> twice.
<QUIT>
The result is outputted in the new unit.
××
factortiter)blank)KFR(volume(
×
divisorsmplsize
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2.3. Tutorial
It is now necessary to match the factor to the new result unit. A table with a selection of matched quantities for factor, divisor and unit of the sample size can be found in the quick reference.
<CALC DATA>
4 × <ENTER>
KFT volume 3.459 ml factor 0.1
<1>
<ENTER>
KFT volume 3.459 ml divisor 1
<ENTER>
2 × <QUIT>
Enter a new factor: Press <CALC DATA> and enter the inquiries of the "calculation" group with <ENTER>. Proceed with 3 times <ENTER> to the display:
Enter "1".
As divisor enter the density of the sample.
Exit the inquiry by pressing <QUIT> twice. The re-
sult is recalculated and outputted.

2.3.4 Drift

The drift is measured in µL/min. It specifies how much KF reagent is consumed per unit time to keep the titration cell dry. The reagent is needed,
to titrate moisture in the titration cell.
to compensate the iodine consumption of slow side reactions.
The drift value is generally of the order of a few µL/min for "dry conditioned" titration cells.
Checking the condition of the solvent
The drift can be displayed during the conditioning of the titration cell with the <DRIFT> key:
<DRIFT>
Drift 4.3 µl/min
<DRIFT>
Press <DRIFT>. The first line of the display shows
You can follow the progress of the drift. In fresh solvent the drift value should drop to less than 10 µL/min after a few minutes.
Pressing <DRIFT> once again switches the drift display off.
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2.3 Tutorial
Drift correction of the results
You can correct your results by the drift. This is primarily necessary if you wish to deter­mine very small amounts of moisture or when you have very long titration times. For the correction "drift value titration time" is subtracted form the dispensed volume:
corrected volume = dispensed volume – (drift value titration time)
The drift value can be determined automatically or entered manually. In the automatic determination the current drift value at the start of the titration is stored and used for the correction. In the manual entry you yourself enter a fixed value, e.g. the stable drift value that you have read off from the display during conditioning.
<CALC DATA>
7 × <ENTER>
KFT volume 3.459 ml drift corr.: OFF
2 × <SELECT>
<ENTER>
KFT volume 3.459 ml drift value 0.0 µl/min
2.2
<ENTER>
<QUIT>
KFT-Vol -d 2.365 ml
Activate the drift correction: Press <CALC DATA> and enter the inquiries of the "calculation" group with <ENTER>. Proceed with <ENTER> until the dis­play shows:
Make your selection with <SELECT>, e.g. "man.".
Enter a drift value, e.g. 2.2 µL/min and exit the in-
quiry.
The result is recalculated and the first line of the display shows
-d means that a drift correction has been performed.
If you have connected a printer, the full report provides you with all data for recalculation of the result:
date 2002-03-27 time 13:55:10 3 smpl size 0.03 g KFR volume 3.459 ml drift man. 2.2 µl/min (-d)time 1.03 water 922.2 mg/ml
============
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2.4. Selection of the mode, key <MODE>

2.4 Selection of the mode, key <MODE>

MODE
Press key <MODE> until the desired mode is displayed and confirm with <ENTER>.
The following modes can be selected:
KFT: Karl Fischer titration
TITER with H2O or std.: Titer determination with water or water-containing standard.
TITER with Na2Tart*2H2O: titer determination with sodium tartrate.
BLANK determination: determination of the blank value
The set values under the <CONFIG> and <PARAM> keys apply to all modes, whereas the calculations differ for each mode. Once values have been set they remain effective even if the instrument is switched off.
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2.5 Configuration, key <CONFIG>

2.5 Configuration, key <CONFIG>

CONFIG
KFT ******** >KF device settings
>KF device settings
limit KF reag. OFF ml
actual KF reag. 0 ml
polarizer: I(pol)
I(pol) 50 µA EP 250 mV cond.
U(pol) 400 mV EP 25 µA cond.
Key <CONFIG> serves to enter device specific data. The set values apply to all modes. The quantities marked with "cond." are also accessible during the conditioning
KF device settings:
Settings for the monitoring of the reagent supply, the measuring input, the endpoint and the filling rate.
peripheral units:
Selection of printer, balance and the curve at the ana­log output.
auxiliaries:
e.g. setting of dialog language, date, time, etc.
RS232 settings:
RS parameters for the COM interface.
The display texts of the Titrino are shown to the left. The values are the default values.
KF device settings for all modes
KF reagent volume counter (0...999 mL, OFF)
is used for monitoring of the
reagent supply
the buffer capacity of the solvent with 2-component
reagents <CLEAR> sets "OFF". If the KF reagent volume counter is activated, the inquiry of the current counter status follows.
Current counter status (0...999 mL)
Selection of the polarization mode (I(pol), U(pol))
Polarization current(-127...127 µA) Endpoint voltage(-1500 mV...1500 mV)
Polarization voltage(-1270...1270 mV, in steps of 10 mV) Endpoint current (-150...150 µA)
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2.5. Configuration, key <CONFIG>
filling rate max. ml/min
cond.
>RS232 settings
baud rate: 9600
data bit: 8
stop bit: 1
parity: none
handshake: HWs
RS control: ON
>peripheral units
send to: IBM
balance: Sartorius
record: V vs. t
Filling rate after the titration (0.01...150 mL/min, max.)
<CLEAR> sets "max.". The maximum rate depends on the Exchange unit: Exchange unit max. 5 mL 15 mL/min 10 mL 30 mL/min 20 mL 60 mL/min 50 mL 150 mL/min
Settings of RS232 interface
see also page 68.
Baud rate (300, 600, 1200, 2400, 4800, 9600)
Data bit (7, 8)
Stop bit (1, 2)
Parity (even, odd, none)
Handshake (HWs, HWf, SWline, SWchar, none)
see page 68.
Control via RS232 interface (ON, OFF)
"OFF" means that the receipt of commands via the RS232 interface is blocked. Data output
is possible.
Settings for peripheral units
Selection of printer (Epson, Seiko, IBM) at the Titrino RS232 interface.
"Epson", for Epson Mode, e.g. Epson LX 300+,
Citizen iDP 562 RS, Custom DP40-S4N
"Seiko", e.g. for DPU-414 "IBM", e.g. for HP DeskJet types, for all printers with IBM character set Table 437 and IBM graphics, as well as for the data transmission to a computer with Metrodata software VESUV.
Selection of balance (Sartorius, Mettler, AND, Precisa)
Sartorius: Models MP8, MC1 Mettler: Models AT, AM, PM, AX, MX, UMX and
balances with 011, 012, or 016 interface
AND: Models ER-60, 120, 180, 182, FR-200, 300
and FX-200, 300, 320
Precisa: Models with RS232C interface
Selection of the curve for the output at the analog output (V vs. t, dV/dt vs. t, U vs. t, -U vs. t)
V vs. t: Volume vs. time curve dV/dt vs. t: Drift vs. time curve U vs. t: Control deviation (current value – EP) vs.
time curve
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2.5 Configuration, key <CONFIG>
>auxiliaries
dialog: english
date 2001-03-27
time 08:13
run number 0
electrode test: ON
display KFR vol.: ON
device label
program 787.0010
General settings
Selection of dialog language (english, deutsch, francais, español)
Current date (YYYY-MM-DD)
Format: Year-month-day, entry with leading zeros.
Current time (HH-MM)
Format: Hours-minutes, entry with leading zeros.
Current run number for result output (0...999)
The sample number is set to 0 when the instrument is switched on and incremented on every determination.
Electrode test (ON, OFF)
Test for polarized electrodes. Performed on changeover from the inactive state to a measurement. "OFF" means that the test is not performed.
Display the dispensed KFR volume in the result display (ON, OFF)
"ON" means the dispensed KFR volume will be displayed in the result output on the first line.
Individual identification of devices (up to 8 ASCII characters)
Display of program version
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