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.
787 KF Titrino
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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
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.
787 KF Titrino
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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.
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 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
787 KF Titrino
5
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.
787 KF Titrino
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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.
787 KF Titrino
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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
787 KF Titrino
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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".
787 KF Titrino
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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.
787 KF Titrino
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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.
787 KF Titrino
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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 %
============
787 KF Titrino
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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.
13
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.
787 KF Titrino
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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
787 KF Titrino
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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.
787 KF Titrino
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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:
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
============
787 KF Titrino
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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.
787 KF Titrino
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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 voltage(-1270...1270 mV, in steps of 10 mV)
Endpoint current (-150...150 µA)
787 KF Titrino
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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)