Metrohm 787 KF Titrino User manual

CH-9101 Herisau/Switzerland
E-Mail [email protected]
Internet www.metrohm.com
787 KF Titrino
Program version 5.787.0010
Instructions for Use
8.787.1003 03.2002 / pkl

Table of contens
787 KF Titrino
Table of contents
1Introduction ..........................................................................................................1
1.1 Instrument description...........................................................................................1
1.2 Controls and parts................................................................................................. 2
2Manual 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
3Error 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
4Preparations .......................................................................................................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
5Appendix.............................................................................................................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

Table of contents
787 KF Titrino
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

1.1 Instrument description
787 KF Titrino 1
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.

1.2 Controls and parts
787 KF Titrino
2
1.2 Controls and parts
Front view of instrument:

1.2 Controls and parts
787 KF Titrino 3
1Exchange Unit
2Display
3Setting of display contrast
4Controls the dosing rate during manual dosing with <DOS> and subse-
quent filling
5Control 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.

1.2 Controls and parts
787 KF Titrino
4
Rear view of instrument:

1.2 Controls and parts
787 KF Titrino 5
6RS232 interface
for the connection of printer, balance or a computer
7Remote lines
(input/output)
for the connection of Sample Changers, robots etc.
8Connection for the KF electrode
9Connection 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 Ti-
trino 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

2.1. Keypad
787 KF Titrino
6
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.

2.2 Principle of data input
787 KF Titrino 7
2.2 Principle of data input
• 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 pe-
ripheral 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 moves you one level up.
• In this example you leave the menu "configuration"
by pressing <QUIT> and return to the standby
state with the display of the titration mode.
KFT ********
send to: IBM
KFT ********
>auxiliaries
KFT ********
KFT ********
>KF device settings
KFT ********
KFT ********
>peripheral units

2.3. Tutorial
787 KF Titrino
8
2.3 Tutorial
This short operating course teaches you to work quick and efficient with the 787 KF Ti-
trino, 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.
<CONFIG>
3 ×<CONFIG>
<ENTER>
<SELECT>
<ENTER>
• 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 titra-
ton.
• 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 inquir-
ies of the group "auxiliaries". Note the ">" sign. All ti-
tles 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 se-
lected 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
KFT ********
>KF device settings
KFT ********
>auxilliaries
KFT ********
dialog: english
KFT ********
dialog: español
KFT ********
KFT ********
fecha 2002-03-27

2.3 Tutorial
787 KF Titrino 9
2 ×<QUIT>
<QUIT>
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 lan-
guage, proceed as before and select "English".
KFT ********
KFT ********
>ajustes varios

2.3. Tutorial
787 KF Titrino
10
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>
<ENTER>
• 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
Briefly check a few settings under the <PARAM> key:
2 ×<PARAM>
<ENTER>
<ENTER>
<ENTER>
<ENTER>
• Press <PARAM> twice so that the title "preselec-
tions" 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 be-
tween 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.
KFT ********
TITER with H2O or Std.
TITER ********
TITER ********
>preselections
TITER ********
conditioning: ON
TITER ********
req.ident: OFF
TITER ********
req.smpl size: ON
TITER ********
report: OFF

2.3 Tutorial
787 KF Titrino 11
or
<ENTER>
With a connected printer, the short report, for example,
can be selected.
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
as long as the vessel is still wet and the green "Cond." lamp flashes. As soon as the titra-
tion vessel is dry and hence ready for operation, this is shown by
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>
<ENTER>
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 re-
main set at 20. The mean calculation is terminated
when the operating mode is changed.
• Exit the inquiry.
TITER ********
report: short
TITER wait
TITER conditioning
TITER ********
>statistics
TITER ********
mean: n= 20

2.3. Tutorial
787 KF Titrino
12
Determination
<START>
0.03
<ENTER>
• 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 back-
weigh the syringe.
The titration now runs.
The first line of the display shows the current volume. In
addition, a "↑" appears when dispensing is being per-
formed.
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:
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:
KFR volume 0.000 ml
smpl size 1.0 g
KFR volume ↑1.426 ml
#======
KFR volume 5.632 ml
titer 5.3267 mg/ml
date 2002-03-27 time 13:55:10 3
smpl size 0.03 g
titer 5.3267 mg/ml
============
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 %
============

2.3 Tutorial
787 KF Titrino 13
Viewing the statistics data
If you have not connected a printer, you can view the statistics data on the display with
<SELECT>.
<SELECT>
<SELECT>
<SELECT>
<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>
2×<ENTER>
<SELECT>
<ENTER>
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.
KFR volume 5.676 ml
titer 5.3686 mg/ml
KFR volume 5.676 ml
res.tab: original
KFR volume 5.676 ml
res.tab: delete n
KFR volume 5.676 ml
mean (2) 5.3477 mg/ml
KFR volume 5.676 ml
+/-s 0.02973 mg/ml
KFR volume 5.676 ml
s(rel) 0.56 %
KFR volume 5.676 ml
>statistics

2.3. Tutorial
787 KF Titrino
14
<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.
KFR volume 5.676 ml
delete n= 1

2.3 Tutorial
787 KF Titrino 15
2.3.3 Karl Fischer titration
<MODE>
<ENTER>
• 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.
<CALC DATA>
3 ×<ENTER>
2 ×<QUIT>
• 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.
Now prepare your sample and titrate it.
Result calculation and unit of the result
The result is calculated by the following formula:
divisorsmplsize
factortiter)blank)KFR(volume(
)content(water ×
××−
=
<UNIT>
2 ×<SELECT>
<ENTER>
<1>
<ENTER>
<QUIT>
• 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.
The result is outputted in the new unit.
KFR volume 5.676 ml
KFT
KFT conditioning
KFT conditioning
titer 5.3326 mg/ml
KFT volume 3.459 ml
result unit: mg/ml;3
KFT volume 3.459 ml
result unit: %

2.3. Tutorial
787 KF Titrino
16
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>
<1>
<ENTER>
<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>
• 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.
KFT volume 3.459 ml
factor 0.1
KFT volume 3.459 ml
divisor 1
Drift 4.3 µl/min