Metrohm Titrino 758 KFD User manual

CH-9101 Herisau/Switzerland
E-Mail [email protected]
Internet www.metrohm.com
758 KFD Titrino
Program version 5.758.0022
Instructions for Use
8.758.1203 11.2001 / pkl

Table of contents
758 KFD Titrino
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 Text input ................................................................................................................... 8
2.4 Configuration, key <CONFIG>................................................................................. 9
2.5 Selection of the mode, key <MODE> .................................................................... 16
2.6 Parameters, key <PARAM>.................................................................................... 17
2.6.1 Parameters for KFT ........................................................................................... 17
2.6.2 Parameters for SET ........................................................................................... 27
2.6.3 Parameters for MEAS........................................................................................ 36
2.6.4 Parameters for CAL........................................................................................... 38
2.6.5 Parameters for TIP ............................................................................................ 40
2.7 Result calculations................................................................................................... 42
2.8 Statistics calculation ................................................................................................ 45
2.9 Common variables................................................................................................... 47
2.10 Data output ............................................................................................................ 48
2.10.1 Reports for the output at the end of a determination...................................... 48
2.10.2 Display of the Curve........................................................................................ 50
2.11 User name, key <USER> ..................................................................................... 51
2.12 TIP, Titration procedure.......................................................................................... 52
2.13 Method memory, keys <USER METH> and <CARD> ....................................... 56
2.13.1 Key <USER METH>....................................................................................... 56
2.13.2 Key <CARD> ................................................................................................. 58
2.14 Calibration data, key <CAL.DATA>...................................................................... 61
2.15 Current sample data, key <SMPL DATA>............................................................ 62
2.16 Silo memory for sample data................................................................................. 63
2.17 Storing determination results and silo calculations ............................................... 66
2.17.1 Storing determination results .......................................................................... 66
2.17.2 Silo calculations .............................................................................................. 67
2.18 Manual dosing and preparation of titration burets ................................................ 70
2.18.1 Manual dosing ................................................................................................ 70
2.18.2 Preparation of the titration burets, key <PREP>............................................ 70
3 Operation via RS232 Interface (green part) ...........................................................71
3.1 General rules............................................................................................................ 71
3.1.1 Call up of objects .............................................................................................. 72
3.1.2 Triggers ............................................................................................................. 73
3.1.3 Status messages .............................................................................................. 74
3.1.4 Error messages................................................................................................. 76
3.2 Remote control commands ..................................................................................... 80
3.2.1 Overview............................................................................................................ 80
3.2.2 Description of the remote control commands .................................................. 99
3.3 Properties of the RS 232 Interface ......................................................................... 130
3.3.1 Handshake...................................................................................................... 130
3.3.2 Pin Assignment ............................................................................................... 133
3.3.3 What can you do if the data transfer does not work? ..................................... 135

Table of contents
758 KFD Titrino
4 Error messages and Troubleshooting .................................................................137
4.1 Error and special messages.................................................................................. 137
4.2 Diagnosis............................................................................................................... 142
4.2.1 General ........................................................................................................... 142
4.2.2 Procedure ....................................................................................................... 142
4.2.3 Equipment required: ....................................................................................... 143
4.2.4 Diagnosis steps .............................................................................................. 143
4.3 Initialize and test RAM ........................................................................................... 154
4.4 Releasing a locked spindle ................................................................................... 155
5 Preparations ...........................................................................................................156
5.1 Setting up and connecting the instruments .......................................................... 156
5.1.1 Titrino with Stirrer or Titration Stand................................................................ 156
5.1.2 Titrino with external burets .............................................................................. 157
5.1.3 Connection of a printer ................................................................................... 158
5.1.4 Connection of a balance................................................................................. 159
5.1.5 Connection of a KF Oven ............................................................................... 160
5.1.6 Connection of a Sample Changer .................................................................. 161
5.1.7 Connection of the 774 Oven Sample Processor ............................................ 162
5.1.8 Connection of a computer.............................................................................. 163
5.1.9 Connection of a Remote Box.......................................................................... 163
5.2 Connection of electrodes and preparing titration vessel....................................... 167
6 Appendix .................................................................................................................170
6.1 Technical specifications ........................................................................................ 170
6.2 Pin assignment of the "Remote" socket................................................................. 173
6.2.1 Lines of the "Remote" socket during the titration............................................ 175
6.2.2 Possible configurations of the activate pulse in SET, KFT and CAL .............. 176
6.3 User methods........................................................................................................ 177
6.3.1 General ........................................................................................................... 177
6.3.2 KF Titer determination with H2O or methanol standard "H2OTiter" ................ 178
6.3.3 KF Titer determination with sodium tartrate "TarTiter"..................................... 179
6.3.4 Blank determination for KFT "Blank_KF"......................................................... 180
6.3.5 KF-titration with blank value subtraction "KF-Blank"....................................... 181
6.3.6 KF-titration without blank value subtraction "KF" ............................................ 183
6.3.7 KF titrations with various KF reagents ............................................................ 185
6.3.8Titer determination of sodium hydroxide "Tit.NaOH" ....................................... 186
6.3.9 Titer determination of hydrochloric acid "Tit.HCl" ........................................... 187
6.3.10 p- and m-Value "p+m val." ........................................................................... 188
6.3.11 Determination of the bromine number "BrNumber" ...................................... 190
6.3.12 Determination of the formaldehyde number "FormolNo".............................. 191
6.4 Titrino validation..................................................................................................... 194
6.4.1 Electronic tests ............................................................................................... 194
6.4.2 Wet tests ......................................................................................................... 194
6.4.3 Maintenance and adjustment of the Titrino .................................................... 194
6.5 Warranty and conformity ........................................................................................ 195
6.5.1 Warranty........................................................................................................... 195
6.5.2 EU Declaration of conformity........................................................................... 196
6.5.3 Certificate of Conformity and System Validation ............................................. 197
6.6 Scope of delivery and ordering designations........................................................ 198
Index ...........................................................................................................................202

Introduction
758 KFD Titrino 1
1 Introduction
1.1 Instrument description
The 758 KFD Titrino is a titrator for fast and precise water determination and endpoint
titration with LCD graphical display. Titration curves can be observed in real-time. The 758
KFD Titrino controls up to three dosing units.
The operator is almost free to define his titrations. All operating modes of the Titrino can
be combined to perform extensive analytical sequences.
Ready-to-start methods for the most common applications are stored in the internal
method memory. The operator is free to modify and overwrite these methods or to create
and store his own titration sequences. The 758 KFD Titrino also provides the opportunity
to store, transfer and load applications and results via memory card.
Data exchange with a PC is possible with the Metrodata VESUV Software and with Metro-
data TiNet Software complete remote control, data acquisition and evaluation via PC is
enabled.

Introduction
758 KFD Titrino
2
1.2 Controls and parts
Front view of instrument:

Introduction
758 KFD Titrino 3
1Exchange Unit
2Display
3Setting of display contrast
4Opening for the memory card
5Controls the dosing rate during manual dosing with <DOS> and
subsequent filling
6Control keys and indicator lamps on the Titrino
Key < > Power switch
Key < > Switching stirrer ON/OFF
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 (5).
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 key-
pad.
Indicator lamps:
"COND." Lamp flashes when conditioning is performed
and the titration vessel is still wet. It is on if condi-
tioning is ok.
"STATISTICS" Lamp is on when the "statistics" function (calcula-
tion of mean and standard deviation) is on.
"SILO" Lamp is on when silo memory (for sample data)
is on.

Introduction
758 KFD Titrino
4
Rear view of instrument:

Introduction
758 KFD Titrino 5
7RS232 interfaces
2 separate interfaces for the connection of printer, balance, and com-
puter
8Remote lines (input/output)
for the connection of the Remote Box, Sample Changers, robots etc.
9Connection of electrodes and temperature sensor
• 2 high-impedance measuring inputs for pH and U measurements.
They can either be used separately or for differential potentiometry,
see page 167.
Important: If you work with both measuring inputs in the same ves-
sel, the same reference electrode must be used.
• 1 measuring input for polarized electrodes, e.g. KF electrode
• 1 measuring input for PT100 or Pt1000 temperature sensor
10 Connection for separate keypad
11 Connection for power cable
With power supplies where the voltage is subject to severe HF distur-
bances, the Titrino should be operated via an additional power filter,
e.g. Metrohm 615 model.
12 Connection for external dosing units D1 and D2
685 Dosimats or 700 Dosinos
13 Connection for stirrer
728 Magnetic Stirrer, 802 Rod Stirrer, 703 or 727 Ti Stand
Supply voltage: 10 VDC (I ≤200 mA)
14 Rating plate
with fabrication, series and instrument number

2.1 Keypad
758 KFD Titrino
6
2 Manual operation
2.1 Keypad
The third functions (inscriptions in the triangle) on the keys of the keypad are used for
formula entry, see page 42.
CONFIG Configuration.
PARAM Parameters.
SMPL DATA Sample data.
STATISTICS ON/OFF switching of statistics calcula-
tions of consecutive determination, see
page 45.
MEAS/HOLD ON/OFF switching of measurements
between titrations and hold during
titrations.
SILO ON/OFF switching of silo memory for
sample data, see page 63.
PREP Preselection of dosing units, see
page 70.
CAL.DATA Calibration data, see page 61.
CARD Management of memory card, see
page 58.
C-FMLA Calculation values, see page 44.
DEF Formulas, data output, sequence for
TIP, see page 42ff and page 52.
USER METH Management of internal method mem-
ory, see page 56.
PRINT Printing of reports, see page 50.
REPORTS Result output.
MODE Mode selection, see page 16.
USER User name, see page 51.
CURVE Switching result/curve display, see
page 50.
←,→Selection of special values (dialog
marked with ":").
↑,↓Cursor key for navigation.
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
758 KFD Titrino 7
2.2 Principle of data input
• If you press a key, you will find a group of inquiries
in the display.
Example key <CONFIG>:
In the first line you see where you are: You pressed
key <CONFIG> and you are now in the inquiries
"configuration".
• The cursor is inverted. In our example the cursor is
on the inquiry ">monitoring". You can move the cur-
sor up and down with keys <↑> and <↓>.
• If a dialog text is marked with ">", it contains a
group of inquiries itself. You go to this group press-
ing <ENTER>.
Example inquiries of "peripheral units":
The first two lines indicate again where you are.
Then you find the inquiries.
If a dialog text of an inquiry is marked with ":", you
can select a value with keys <←> and <→> (for-
ward/backward).
• A value is stored with <ENTER> and the cursor
moves to the next inquiry.
• With key <QUIT> you move one level up, in our ex-
ample you go back to ">peripheral units".
If you press <QUIT> once more, you quit the in-
quiries in "configuration" altogether.
• If you can scroll, "↓" or "↑" appear in the right lower
or upper corner of the display.
configuration
>monitoring
>peripheral units
>auxiliaries
>RS232 settings COM1
>RS232 settings COM2
>common variables
>prep.dosing elements
configuration
>peripheral units
send to COM1: IBM
send to COM2: IBM
man.reports to COM: 1
balance: Sartorius
stirrer control: OFF
remote box: OFF
configuration
>monitoring
>peripheral units
>auxiliaries
>RS232 settings COM1
>RS232 settings COM2
>common variables
>prep.dosing elements

2.3 Text input
758 KFD Titrino
8
2.3 Text input
<CLEAR>
<QUIT>
<ENTER>
Example storing a method:
• Press key <USER METH>.
Place the cursor to ">store method" and press
<ENTER>.
The name of the method which is currently in the
working memory is displayed.
• Delete this name with <CLEAR>.
• Open the "text writing mode" with key <ABC>.
You can now select the desired character by means
of the cursor keys, then confirm this character. Se-
lect the next character...
When you confirmed the last character, i.e. your
name is complete, you quit the text writing mode
with <QUIT>.
Confirm now the name with <ENTER>.
• During text input you can correct typing errors with
<CLEAR>:
<CLEAR> deletes the characters one by one.
• If you wish to modify an existing name, do not de-
lete the existing name before you start the text input
mode. Proceed then as follows:
1. Press <USER METH>, place the cursor to
">store method" and press <ENTER>.
2. Open the text writing mode directly: Press key
<ABC>.
3. <CLEAR> now deletes the characters one by
one or you can add additional characters.
4. If your text is complete, leave the text writing
mode with <QUIT> and confirm the text with
<ENTER>.
REPORTS
ABC
.
user methods
>store method:
method name:
ABCDEFGHIJKLMNOPQRSTUVWXYZ
abcdefghijklmnopqrstuvwxyz
µ°!"#$&'()*+,-./ 0123456789
user methods
>store method
method name: Text
user methods
>store method
method name: ********

2.4 Configuration, key <CONFIG>
758 KFD Titrino 9
2.4 Configuration, key <CONFIG>
Key <CONFIG> serves to enter device specific data.
The set values apply to all modes.
monitoring:
Monitoring of instrument validation, pH calibration, ser-
vice interval and printout of diagnostic report.
peripheral units:
Selection of printer, balance, stirrer control and COM
for manual report output.
auxiliaries:
e.g. setting of dialog language, date, time, type of re-
sult display.
RS232 settings COM1 and 2:
RS parameters for the COM's.
common variables:
Values of common variables.
prep.dosing element:
Parameters for the preparation of the dosing units.
The display texts of the Titrino are shown on the left
side. The values are the default values.
>monitoring
validation: OFF
time interval 365 d
time counter 0 d
calibration: OFF
Monitoring functions
Monitoring the validation interval (ON, OFF)
Monitoring is carried out at the end of the titrations and
when the Titrino is switched on. If the monitoring
responds the message "validate instrument" appears.
The message vanishes with <CLEAR>. At the same
time the counter is reset to zero.
If "ON" has been set:
Time interval for validation (1...9999 d)
see also page 194.
Time counter (0...9999 d)
Counts the number of days since the last time the
counter was reset.
Monitoring the pH calibration interval (ON, OFF)
Monitoring is carried out at the end of the titrations and
when the Titrino is switched on if the measuring input
has a current calibration date. If the monitoring
responds the message "calibrate electrode" appears.
The counter will be reset to zero on the next valid pH
calibration of this input.
configuration
>monitoring
>peripheral units
>auxiliaries
>RS232 settings COM1
>RS232 settings COM2
>common variables
>prep.dosing elements
CONFIG

2.4 Configuration, key <CONFIG>
758 KFD Titrino
10
meas.input: 1
time interval 7 d
time counter 0 d
service: OFF
next service YYYY-MM-DD
system test report: OFF
If "ON" has been set:
Measuring input (1, 2, diff.)
Time interval for validation (1...9999 d)
Time counter (0...9999 d)
Counts the number of days since the last valid
calibration at the selected measuring input.
Monitoring the service interval (ON, OFF)
Monitoring is carried out after the Titrino has been
switched on. If the monitoring responds the message
"Service is due" appears. The message vanishes with
<CLEAR>.
If "ON" has been set:
Date of next service (YYYY-MM-DD)
System test report printout (ON, OFF)
With "ON" the report of the system test is printed out
after the Titrino has been switched on, see also
page 194.
>peripheral units
send to COM1: IBM
send to COM2: IBM
man.reports to COM: 1
balance: Sartorius
Settings for peripheral units
Selection of printer (Epson, Seiko, Citizen, HP, IBM) at
the Titrino COM1
"Epson", for Epson
"Seiko", e.g. for DPU-414
"Citizen", e.g. for iDP 562 RS, Custom DP40-S4N
"HP" e.g. for Desk Jet types. Place curves always at the
beginning of a page as you cannot have them over 2
pages.
"IBM" for all printers with IBM character set Table 437
and IBM graphics, as well as for the data transmission
to a computer or a data system.
COM of Titrino for the output of manually triggered
reports (1, 2, 1&2)
Manually triggered reports (e.g. with <PRINT> ....).
Exception <PRINT><REPORTS>: These reports are
outputted on the COM as defined in the method.
Selection of balance (Sartorius, Mettler, Mettler AT,
AND, Precisa)
Sartorius: Models MP8, MC1
Mettler: Models AM, PM , AX, MX, UMX and
balances with 011, 012, and 016
interfaces
Mettler AT: Model AT
AND: Models ER-60, 120, 180, 182, FR-200, 300
and FX-200, 300, 320
Precisa: Models with RS232C interface

2.4 Configuration, key <CONFIG>
758 KFD Titrino 11
stirrer control: OFF
remote box: OFF
keyboard: US
barcode: input
Automatic switching ON/OFF of the stirrer in the titration
sequence (ON, OFF)
If stirrer control is ON, the stirrer will be switched on at
the beginning and switched OFF at the end of a de-
termination. For SET and KFT with conditioning the
stirrer will be switched off in the inactive state.
In the modes MEAS, CAL, and TIP the stirrer is not
switched automatically.
For stirrer control the red switch on the stirrer unit must
be ON.
Connection of a remote box (ON ,OFF)
To the remote socket for PC keyboard and barcode
reader, see page 163.
If "ON" has been set:
Type of PC keyboard (US, German, French, Spanish,
Swiss.)
The PC keyboard is used as an input aid, see
page 164.
Target for barcode reader (input, method, id1, id2, id3,
smpl size)
The barcode reader is used as an input aid, see
page 163.
Input: The barcode string goes to the entry field in
which the cursor is currently located.
Method: The barcode string goes to the entry field
"Methods" in the silo memory.
Id1: The barcode string goes to the entry field
"Id1". (Similar for Id2 and Id3.)
Smpl size: The barcode string goes to the entry
field "smpl size".
>auxiliaries
dialog: english
date 2001-11-21
time 08:13
run number 0
auto start OFF
General settings
Selection of dialog language (english, deutsch,
français, español, italiano, portugese, svenska)
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...9999)
The sample number is set to 0 when the instrument is
switched on and incremented on every determination.
Automatic start of titrations. (1...9999, OFF)
Number of automatic starts ("number of samples").
Used for instrument interconnections in which the
external instrument does not initiate a start. Not
advisable in connections with Sample Changers.

2.4 Configuration, key <CONFIG>
758 KFD Titrino
12
start delay 0 s
result display: bold
dev.label.
program 758.0022
Start delay (0...999999 s)
Delay time after start of methods. Abort start delay time
with <QUIT>.
Type of result display at the end of the determination
(bold, standard)
bold: The calculated results are displayed in bold
characters.
standard: Displays the whole information, e.g. results,
endpoints, messages etc.
Individual identification of devices (up to 8 ASCII
characters)
Will be printed in the result report, see page 49.
Display of program version
>RS232 settings COM1
baud rate: 9600
data bit: 8
stop bit: 1
parity: none
handshake: HWs
Settings of RS232 interface
see also page 130 Identical for COM2.
Baud rate (300, 600, 1200, 2400, 4800, 9600, 19200,
38400, 57600, 115200)
Data bit (7, 8)
Stop bit (1, 2)
Parity (even, odd, none)
Handshake (HWs, SWline, SWchar, none)
see page 130.
>common variables
C30 0.0
etc.
Values of the common variables
Common variables C30...C39 (0..
± 999999)
The values of all common variables are displayed. For
creating common variables see page 47.
>prep.dosing elements
power ON prep: OFF
report: OFF
Preparation of titration burets, "prep" and "empty"
see also page 70.
Warning after power ON (ON, OFF)
If this function is on, a warning appears after switching
on the Titrino, that a preparation should be executed.
Report of prep (ON, OFF)
With ON, a report will be printed automatically after
prep. The report is outputted on the COM which is
given for manual reports (see also page 10).

2.4 Configuration, key <CONFIG>
758 KFD Titrino 13
dos.element: internal D0
warn.interv.DX OFF min
dos.drive: Dosimat
Selection of the dosing element (internal D0, external
D1, external D2)
internal D0: buret of the Titrino
external D1/2: buret D1, D2, resp.
Warning interval for prep (5...9999 min, OFF)
Selection of the type of dosing element (Dosimat,
Dosino)
The internal buret D0 reacts like a "Dosimat".
volume DX 3.5 ml
cycles DX 2
dos.rate max. ml/min
fill rate max. ml/min
Parameters for the internal buret and for
Dosimats:
Volume, that will be dosed with the preparation
(0...99999.99 mL)
Number of cycles (1...9)
Dosing rate (0.01...150 mL/min, max.)
Filling rate (0.01...150 mL/min, max.)
outlet: tip
len.dos.tub.DX 40.0 cm
diam.dos.tub.DX 2.0 mm
len.asp.tub.DX 25.0 cm
diam.asp.tub.Dx 2.0 mm
dos.rate max. ml/min
fill rate max. ml/min
Parameters for Dosinos:
Location where the liquid will be expelled (tip, flask)
With "flask" the reagent will be re-expelled into the
bottle. In this case, it is possible that the titer will be
changed!
The next 4 entries serve to calculate the volumes which
will be expelled in prep:
Length of the dosing tube (1...999.9 cm)
Diameter of the dosing tube (0.1...9.9 mm)
Length of the aspirating tube (1...999.9 cm)
Diameter of the aspirating tube (0.1...9.9 mm)
Dosing rate (0.01...150 mL/min, max.)
Filling rate (0.01...150 mL/min, max.)

2.4 Configuration, key <CONFIG>
758 KFD Titrino
14
Settings with key <CONFIG> and power ON
Proceed as follows:
1. Switch the Titrino OFF.
2. Press <CONFIG> and keep it pressed during switching the Titrino ON.
The display shows the following:
lock:
Locking keys <CONFIG>, <PARAM> and <SMPL
DATA>, and the functions "recall method", "store
method" and "delete method" of the internal method
memory in the Titrino.
curve:
Changes the appearance of the curve printout.
>lock
<configuration>: OFF
<parameters>: OFF
<smpl data>: OFF
recall method: OFF
store method: OFF
delete method: OFF
lock
"ON" means that the corresponding function is not
accessible anymore.
The corresponding key is locked.
The corresponding function in the internal method
memory of the Titrino is locked.
Setup
>lock
>curve

2.4 Configuration, key <CONFIG>
758 KFD Titrino 15
>curve
grid: ON
frame: ON
scaling: Full
width 0.5
length 0.05
curve
The settings are valid for COM1 and COM2.
If you change the printer type, the following settings are
initialized according to the printer.
Grid drawing (ON, OFF)
Frame drawing (ON, OFF)
Type of scaling (Full, Auto)
Full: The scaling goes from the greatest to the smallest
value.
auto: The scaling from tick to tick, e.g. the
smallest/greatest values lie in between the first/last tick.
Width (0.2...1.00)
1 is greatest width. If you set 1, you may loose the label
at the right margin.
Length (0.01...1.00)
Time axis:
Curve length
0.01 100 cm
0.1 10 cm
0.5 2 cm
1 1 cm

2.5 Selection of the mode, key <MODE>
758 KFD Titrino
16
2.5 Selection of the mode, key <MODE>
Press key <MODE> until the desired mode is
displayed and confirm with <ENTER>.
Select the measured quantity pH, U, Ipol, Upol, (T) with
<←> or <→> and confirm it also with <enter>.
The following modes can be selected:
• KFT: Karl Fischer Titration, the determination of
water content.
• SET: Set Endpoint Titration.
• MEAS: Measuring.
• CAL: pH Calibration.
• TIP: Titration Procedure. Linking of various
commands and methods to a titration procedure.
These standard modes are equipped with a set of
standard parameters. They only need few settings in
order to be ready to work.
TIP is an empty "shell". The TIP sequence has to be
defined with <DEF>, see page 52.
You will find a survey of the modes in the short
Instructions for use.
MODE
;
–
mode
mode: KFT
measured quantity: Ipol