89078003EN
89078003EN
89078003EN
Manual
8.907.8003EN / 2022-01-12
Metrohm AG
CH-9100 Herisau
Switzerland
+41 71 353 85 85
[email protected]
www.metrohm.com
907 Titrando
Manual
8.907.8003EN / 2022-01-12 /
Technical Communication
Metrohm AG
CH-9100 Herisau
Disclaimer
Deficiencies arising from circumstances that are not the responsibility of
Metrohm, such as improper storage or improper use, etc., are expressly
excluded from the warranty. Unauthorized modifications to the product
(e.g. conversions or attachments) exclude any liability on the part of the
manufacturer for resulting damage and its consequences. Instructions and
notes in the Metrohm product documentation must be strictly followed.
Otherwise, Metrohm's liability is excluded.
■■■■■■■■■■■■■■■■■■■■■■ Table of contents
Table of contents
1 Introduction 1
1.1 The Titrando system ............................................................. 1
1.2 Instrument description ......................................................... 2
1.3 Titration modes – Measuring modes – Dosing com-
mands .................................................................................... 3
1.4 About the documentation ................................................... 5
1.4.1 Symbols and conventions ........................................................ 5
1.5 Safety instructions ................................................................ 6
1.5.1 General notes on safety ........................................................... 6
1.5.2 Electrical safety ........................................................................ 6
1.5.3 Working with liquids ................................................................ 7
1.5.4 Flammable solvents and chemicals ........................................... 7
1.5.5 Recycling and disposal ............................................................. 7
6 Troubleshooting 44
6.1 General ................................................................................ 44
6.2 Karl Fischer titration ........................................................... 44
6.2.1 ............................................................................................. 44
6.3 SET titration ........................................................................ 46
6.3.1 ............................................................................................. 46
7 Appendix 47
7.1 Remote interface ................................................................ 47
7.1.1 Pin assignment of the remote interface .................................. 47
8 Technical specifications 51
8.1 Measuring interface ........................................................... 51
8.1.1 Potentiometry ........................................................................ 51
8.1.2 Temperature .......................................................................... 51
8.1.3 Polarizer ................................................................................ 52
8.2 Power connection ............................................................... 53
8.3 Ambient temperature ......................................................... 53
8.4 Reference conditions .......................................................... 53
8.5 Dimensions .......................................................................... 53
8.6 Interfaces ............................................................................. 54
9 Accessories 55
Index 56
Table of figures
Figure 1 The Titrando system .......................................................................... 1
Figure 2 Front 907 Titrando ............................................................................ 8
Figure 3 Rear 907 Titrando ............................................................................. 9
Figure 4 Connecting the Touch Control ......................................................... 11
Figure 5 Connecting the computer ................................................................ 14
Figure 6 MSB connections ............................................................................ 15
Figure 7 Connecting a dosing device ............................................................. 17
Figure 8 Connecting an MSB stirrer ............................................................... 18
Figure 9 Connecting the rod stirrer to the titration stand ............................... 18
Figure 10 Connecting the Remote Box ............................................................ 19
Figure 11 Connecting a printer ....................................................................... 21
Figure 12 Schematic configuration of magnetic stirrer, electrode and buret tip
during a titration. a) stirring direction clockwise, b) stirring direction
counterclockwise. ............................................................................ 24
Figure 13 Connecting a pH, metal or ion-selective electrode ........................... 29
Figure 14 Connecting a reference electrode .................................................... 30
Figure 15 Connecting a polarizable electrode .................................................. 30
Figure 16 Connecting a temperature sensor or an electrode with integrated tem-
perature sensor ............................................................................... 31
Figure 17 Plugging in the mini USB adapter cable ........................................... 32
Figure 18 Plugging in the 854 iConnect .......................................................... 32
Figure 19 Removing the protective cap ........................................................... 33
Figure 20 Aligning the guide pin ..................................................................... 33
Figure 21 Attaching the electrode ................................................................... 33
Figure 22 Unplugging the 854 iConnect ......................................................... 34
Figure 23 Connectors of the Remote Box ........................................................ 47
Figure 24 Pin assignment of remote socket and remote plug ........................... 47
1 Introduction
Computer
Sensors
USB Sample Processor
Dosing Interface Robotic Titrosampler Input 1 / 2 Touch Control
Controller
Relay Box
Printer
USB MSB
On Remote Box
PC keyboard
Titrando
r
verte
Con
232
Barcode
/RS-
reader
USB
USB hub
On
Status
80
mDi5
soa
Me
roth
■ KFT
Volumetric water content determination according to Karl Fischer.
Measuring modes:
– Ipol (voltametric measurement with selectable polarization cur-
rent)
– Upol (amperometric measurement with selectable polarization
voltage)
■ MEAS
The following measuring modes can be selected for measurements:
– pH (pH measurement)
– U (potentiometric voltage measurement)
– Ipol (voltametric measurement with selectable polarization cur-
rent)
– Upol (amperometric measurement with selectable polarization
voltage)
– Conc (concentration measurement with or without standard
addition)
– T (temperature measurement)
■ STDADD
The measuring modes for standard addition are listed separately only in
tiamo™. In Touch Control they are integrated in the measuring mode
MEAS Conc.
The following measuring modes can be selected for measurements:
– auto (automatic addition of the standard addition solution by
specifying a potential difference)
– dos (automatic addition of the standard addition solution by
specifying the single volume increments)
– man (manual addition of the standard addition solution)
■ CAL
Electrode calibration.
Measuring mode:
– pH (calibration of pH electrodes)
– Conc (calibration of ion-selective electrodes)
■ ELT
Electrode test for pH electrodes.
This mode is listed separately only in tiamo™. In Touch Control, the
electrode test is a component part of the CAL calibration mode.
■ Dosing commands
The following commands for dosing can be selected:
– PREP (rinsing the cylinder and tubings of an exchange unit or
dosing unit)
– EMPTY (emptying the cylinder and tubings of a dosing unit)
– ADD (dosing a specified volume)
– LQH (carrying out complex dosing tasks with a Dosino)
CAUTION
NOTE
This symbol highlights additional information and
tips.
WARNING
WARNING
WARNING
Supply voltage
WARNING
WARNING
CAUTION
Periodically check all system connections for leaks. Observe the relevant
regulations in respect to working with flammable and/or toxic fluids
and their disposal.
WARNING
On
2
907 Titran
do
iTrode rea
dy
Metrohm
1 6
2
3
7
4 8
9
5 10
11
3 Installation
3.1.2 Checks
Immediately after receipt, check whether the shipment has arrived com-
plete and without damage by comparing it with the delivery note.
3.1.3 Location
The instrument has been developed for operation indoors and may not be
used in explosive environments.
Place the instrument in a location of the laboratory which is suitable for
operation and free of vibrations and which provides protection against
corrosive atmosphere and contamination by chemicals.
The instrument should be protected against excessive temperature fluctua-
tions and direct sunlight.
CAUTION
Take care to ensure that the power cord is pulled out of the power
socket before either setting up or disconnecting connections between
the instruments.
NOTICE
1 ■ Insert the plug of the Touch Control connection cable into the
Controller socket.
CAUTION
The Touch Control must be shut down properly by deactivation with the
power switch on the rear of the instrument before the power supply is
interrupted. If this is not done, then there is a danger of data loss.
Because of the fact that the power supply for the Touch Control is pro-
vided through the Titrando, you must never disconnect the Titrando
from the power grid (e.g. by deactivating with a connector strip) before
you have deactivated the Touch Control.
If you would prefer not to position the Touch Control directly next to the
Titrando, then you can lengthen the connection with the 6.2151.010
cable. The maximum connection length permitted is 5 m.
WARNING
NOTICE
6.2151.000
NOTICE
Stirrer / Ti Stand
MSB
Remote Box
Ti Stand / Stirrer
Relay Box
Dosino / Dosimat
Dosino
Dosimat
Dosimat / Dosino
Figure 6 MSB connections
The control instrument determines which peripheral devices are suppor-
ted.
NOTICE
CAUTION
Exit the control software before you plug in MSB devices. When it is
switched on, the control instrument automatically recognizes which
device is connected to which MSB connector. The operating unit or the
control software enters the connected MSB devices into the system
configuration (device manager).
MSB connections can be extended with the 6.2151.010 cable. The maxi-
mum connection length permitted is 15 m.
CAUTION
If you operate the 907 Titrando with the aid of the Touch Control, take
care to ensure that the Touch Control is switched off when you set up
or disconnect connections between the various instruments. If you use
a PC software to control the 907 Titrando, you should exit the program
before you set up or disconnect the USB connections.
2 With the aid of the 6.2151.020 cable, connect the USB connector of
the 907 Titrando (type A) with the USB connector of the hub (type B,
see manual for the hub).
2 With the aid of the 6.2151.020 cable, connect the USB connector of
the 907 Titrando (type A) with the USB connector of the printer (type
B, see manual for the printer).
Balance Cable
AND ER, FR, FX with RS-232 inter- 6.2125.020 + 6.2125.010
face (OP-03)
Mettler AB, AG, PR (LC-RS9) In the scope of delivery for the
balance
Mettler AM, PM, PE with interface 6.2146.020 + 6.2125.010
option 016
Also from Mettler: ME 47473
or adapter and either ME 42500
hand switch or ME 46278 foot
Mettler AJ, PJ with interface
switch
option 018
Mettler AT 6.2146.020 + 6.2125.010
Also from Mettler: ME 42500
hand switch or ME 46278 foot
switch
Mettler AX, MX, UMX, PG, AB-S, 6.2134.120
PB-S, XP, XS
Balance Cable
Mettler AE with interface option 6.2125.020 + 6.2125.010
011 or 012
Also from Mettler: ME 42500
hand switch or ME 46278 foot
switch
Ohaus Voyager, Explorer, Analyti- Cable AS017-09 from Ohaus
cal Plus
Precisa balances with RS-232-C 6.2125.080 + 6.2125.010
interface
Sartorius MP8, MC, LA, Genius, 6.2134.060
Cubis
Shimadzu BX, BW 6.2125.080 + 6.2125.010
1 Plug in the USB plug of the USB/RS-232 adapter at the USB connec-
tor of the 907 Titrando.
1 Insert the USB plug of the keyboard into one of the USB sockets of
the 907 Titrando.
1 Insert the USB plug of the barcode reader into one of the USB sock-
ets of the 907 Titrando.
2 Specify the desired layout for the keyboard (USA, Germany, France,
Spain, German-speaking Switzerland).
This setting must match the setting in the device manager (see the
Touch Control manual).
3 Make sure that the barcode reader is set in such a way that Ctrl char-
acters (ASCII 00 to 31) can be sent.
4 Program the barcode reader in such a way that the ASCII character
02 (STX or Ctrl B) is sent as the first character. This first character is
normally referred to as the "Preamble" or "Prefix Code".
5 Program the barcode reader in such a way that the ASCII character
04 (EOT or Ctrl D) is sent as the last character. This last character is
normally referred to as the "Postamble", "Record Suffix" or "Postfix
Code".
1 1
2 2
3 3
3 Buret tip
6.1414.030
2
3 4
6.2013.010
1
6.1415.220
6.1903.020
Proceed as follows:
2 Fix the 6.1414.030 vessel lid of the KF titration cell (with correctly
inserted sealing ring from the 6.1244.040 sealing set) to the support
rod. Keep the locking lever pressed down until it can be released at
the desired position.
4 Adjust the height of the KF titration cell by pressing the locking lever.
It should almost touch the surface of the stirrer. The position can
now be fixed by readjusting the clamping ring.
Once the height of the KF titration cell has been adjusted correctly,
the entire cell can be raised and swiveled as required by pressing the
locking lever.
Before insertion, the 6.1403.040 adsorber tube must be filled with the
6.2811.000 molecular sieve. Proceed as follows:
6.2811.000 2
1
6.1403.040
1 Insert a small cotton plug into the bottom of the adsorber tube. Do
not pack the cotton too tightly.
3 Place a small cotton plug on the molecular sieve. Do not pack the
cotton too tightly.
6 6.1805.200
6.1543.060 4 5
6.1543.110 2
3 6.1543.120
6.2730.030 1
1 1
Proceed as follows:
2 Insert the 6.1543.110 dosing tip through the screw nipple in the
middle rear opening.
3 Insert the 6.1543.120 aspiration tip through the screw nipple in the
right rear opening.
When solvent is aspirated, the end of the aspiration tip must touch
the vessel base, but it must not inhibit the action of the stirring bar.
The aspiration tip can, if needed, be pulled out of the solvent.
4 Insert the 6.1543.060 buret tip through the screw nipple in the left
rear opening.
6 Screw the 6.1805.200 PTFE M8 tubing of the solvent bottle onto the
dosing tip.
6.2104.020 5
6 6.1403.040
4
6.0338.100
6.2730.010
6.2730.020
3 1
2
Proceed as follows:
2 Insert the O-rings of the electrode and of the adsorber tube into the
middle openings of the vessel lid.
3 Screw the two 6.2730.010 screw nipples into the openings with the
O-rings. Do not screw too tightly.
6 Insert the filled 6.1403.040 adsorber tube on the right of the elec-
trode into the remaining opening and then tighten the screw nipple
until it seals.
1 Plug the electrode plug into the Ind. socket of the 907 Titrando.
NOTICE
1 Plug the electrode plug into the Ref. socket of the 907 Titrando.
1 Plug the electrode plug into the Pol. socket of the 907 Titrando.
NOTICE
1 Insert the plugs of the temperature sensor into the Temp. sockets of
the Titrando.
NOTICE
Always insert the red plug into the red socket. This is the only way
that shielding against electrical interference can be ensured.
If the mini USB adapter cable is not connected to the instrument yet, pro-
ceed as follows:
1 Plug the mini USB adapter cable (2) into the iConnect connector of
the instrument (1). Observe the correct orientation (markings).
Make sure that the mini USB adapter cable is connected to the instru-
ment.
The 854 iConnect can also be connected while the instrument is switched
on.
1 Plug the plug of the 854 iConnect (3) into the socket of the mini USB
adapter cable (2). Observe the correct orientation (markings).
The 854 iConnect is used as measuring input for iTrodes (electrodes with
integrated memory chip).
2 Align the guide pin (5) of the electrode with the recess in the 854
iConnect (4).
NOTICE
Mount the protective cap again as soon as the 854 iConnect is not in
use anymore and no electrode is connected.
The 854 iConnect can also be removed while the instrument is switched
on.
1 Unplug the 854 iConnect (3) from the socket of the mini USB adapter
cable (2).
2 Leave the mini USB adapter cable (2) plugged into the socket of the
instrument (1).
NOTICE
Position the mini USB adapter cable in such a way that it cannot be
removed by accident.
NOTICE
For further information on the 854 iConnect, see Manual iConnect 854,
article number 8.854.8002.
Two-component reagents
The reactive parts are distributed among two separated solutions. The
titration reagent contains iodine in methanol. The KF solvent is a solution
of sulfur dioxide and a base in methanol. It is used as a working medium
in the KF titration cell.
4 With a folded paper towel held between thumb and index finger,
break open the ampoule at the marking.
6 Pull the piston of the syringe up to the end and swing the syringe
back and forth somewhat.
The inside of the syringe is being rinsed by water standard and freed
from water contamination.
8 Draw the rest of the water standard into the syringe, aspirating as lit-
tle air as possible.
9 Push out any air bubbles that may be present in the syringe.
10 Wipe off the needle with a lint-free paper towel and cover it with the
appropriate cap.
12 As soon as the drift on the 907 Titrando is stable, take the syringe by
hand, press [START] and inject approx. 1 mL of the water standard
through the septum.
There are two possibilities:
■ Version 1:
Inject the water standard without immersing the needle in the
reagent liquid. If a little drop remains on the end of the needle, it
must be aspirated back before pulling the needle out of the sep-
tum.
The water standard should not be sprayed from the syringe onto
the electrode nor onto the wall of the titration vessel.
■ Version 2:
Inject the water standard directly under the surface of the reagent
liquid.
Take care to ensure that you do not aspirate any liquid when you
withdraw the syringe from the reagent liquid.
13 Close the syringe with the same cap and place it back on the bal-
ance.
14 Read off the value displayed by the balance and enter it as sample
size on the Touch Control or in the PC software (e.g. tiamo).
CAUTION
6 Troubleshooting
6.1 General
Problem Cause Remedy
The "On" LED is not The Touch Control or the 1. Check the plug connections.
illuminated, even computer has not been 2. Switch on the Touch Control or the com-
though the instru- switched on yet or the puter.
ment is connected plugs are not correctly
to the power supply. plugged in.
The drift becomes The sample releases water ■ Adjust the method.
greater after each very slowly. ■ Add solubility promoter.
titration. ■ Increase the temperature (possibly using a
KF oven).
■ See technical literature.
The titration will not The titration cell is leaking. ■ Check the seals and the septum. Replace if
be finished. necessary.
■ Replace the molecular sieve.
The stop criterion is unsuit- Adjust the control parameters (see manual/
able. help of the software used):
The sample is over- The increments at the end ■ Select the user-defined titration rate and
titrated. of the titration are too reduce the dosing rate (see manual/help of
high. the software used).
The following experiment provides a clue
for the optimum dosing rate: During condi-
tioning, display the drift and add sample
without starting the titration. Select a value
below the highest drift as dosing rate.
■ Stir faster.
The electrode may be cov- Wipe off the electrode with ethanol or a suit-
ered. able solvent.
The endpoint is The dosing rate outside the Select the user-defined titration rate and
reached too quickly. control range is too high. reduce the dosing rate (see manual/help of the
software used).
The titration times The buffer capacity of the Replace the working medium.
with volumetric solvent may be exhausted
titration are con- with two-component
stantly longer. reagents.
The stop criterion is unsuit- Adjust the control parameters (see manual/
able. help of the software used):
The sample is over- The control parameters are Adjust the control parameters (see manual/
titrated. unsuitable. help of the software used):
The titration time is The control parameters are Adjust the control parameters (see manual/
too long. unsuitable. help of the software used):
The results are The minimum dosing rate is Select user-defined titration rate and decrease
spread widely. too high. the minimum rate (see manual/help of the
software used).
7 Appendix
3
Figure 23 Connectors of the Remote Box
3 Remote connector
For connecting instruments with a remote
interface.
25
14
14
25
Figure 24 Pin assignment of remote socket and remote plug
The above figure of the pin assignment applies for all Metrohm instru-
ments with 25-pin D-Sub remote connector.
Inputs
+5 V approx. 50 kΩ Pull-up
tp
tp > 20 ms
active = low, inactive = high
Outputs
Open Collector
tp
tp > 200 ms
active = low, inactive = high
IC = 20 mA, VCEO = 40 V
+5 V: maximum load = 20 mA
Function Explanation
Warning The line is set for warning message display.
8 Technical specifications
8.1.1 Potentiometry
One high-ohm measuring input (Ind.) for pH, metal or ion-selective elec-
trodes and one measuring input (Ref.) for separate reference electrodes.
Input resistance > 1 · 1012 Ω
Offset current < 1 · 10–12 A (under reference conditions)
Measuring mode
pH
Measuring –13 to +20 pH
range
Resolution 0.001 pH
Measuring ±0.003 pH
accuracy (±1 digit, without sensor error, under reference conditions)
Measuring mode
U
Measuring –1,200 to +1,200 mV
range
Resolution 0.1 mV
Measuring ±0.2 mV
accuracy (±1 digit, without sensor error, under reference conditions)
8.1.2 Temperature
A measuring input (Temp.) for temperature sensors of the Pt1000 or NTC
type with automatic temperature compensation.
R (25 °C) and B value can be configured for NTC sensors.
Measuring range
Pt1000 –150 to +250 °C
NTC –5 to +250 °C
(R (25 °C) = 30,000 Ω and B (25/50) = 4,100 K)
Resolution
Pt1000 0.1 °C
NTC 0.1 °C
Measuring accu-
racy
Pt1000 ±0.2 °C
(Applies for measuring range –20 to +150 °C; ±1 digit; without sensor
error, under reference conditions)
NTC ±0.6 °C
(Applies for measuring range +10 to +40 °C; ±1 digit; without sensor
error, under reference conditions)
8.1.3 Polarizer
One measuring input (Pol.) for polarizable electrodes.
Measuring mode Determination with adjustable polarization current
Ipol
Polarization cur- –122.5 to +122.5 µA (increment: 0.5 µA)
rent –125.0 to +125.0 µA: non-guaranteed values, dependent on reference
voltage +2.5 V
Measuring –1,200 to +1,200 mV
range
Resolution 0.1 mV
Measuring ±0.2 mV
accuracy (±1 digit, without sensor error, under reference conditions)
8.5 Dimensions
Width 142 mm
Height 227 mm
Depth 231 mm
Weight 2.7 kg (without accessories)
Material (housing) Poly(butylene terephthalate) (PBT)
8.6 Interfaces
USB connectors
USB ports 2 USB downstream ports (type A sockets), 500 mA each, for connect-
ing peripheral devices such as printers, keyboards, barcode readers or
RS-232/USB Box (Metrohm order no. 6.2148.020).
"Controller" connector
Controller port USB upstream port with auxiliary power supply (Mini DIN socket) for
connecting Touch Control or computer for controlling the 907
Titrando.
Touch Control With integrated Touch Control cable.
Computer With 6.2151.000 cable.
9 Accessories
Up-to-date information on the scope of delivery and optional accessories
for your product can be found on the Internet. You can download this
information using the article number as follows:
2 Enter the article number (e.g. 907) into the search field.
The search result is displayed.
NOTICE
Index
6.2151.000 controller cable ..... 13 LQH ..................................... 4 P
685 Dosimat plus ..................... 16 PREP ..................................... 4 PC keyboard
700 Dosino .............................. 16 Dosing device Connect ............................. 22
800 Dosino .............................. 16 Connect ............................. 16 Pin assignment ......................... 47
801 Stirrer ................................ 17 Driver software Power connection .......... 9, 12, 13
803 Ti Stand ............................. 17 Install ................................. 13 PREP ........................................... 4
804 Ti Stand ............................. 17 Printer ...................................... 20
805 Dosimat ............................ 16 E
Electrode R
A Connect ............................. 29 Reagent replacement ................ 41
ADD ........................................... 4 Electrode test Remote
ELT ....................................... 4 Interface ............................. 47
B Electrostatic charge .................... 7 Pin assignment ................... 47
Balance .................................... 21 EMPTY ....................................... 4 Remote Box
Barcode reader Connect ............................. 18
Connect ............................. 23 I
Indicator electrode S
C Warm-up time .................... 42 Safety instructions ...................... 6
Calibration mode Installation Sample
CAL ...................................... 4 Driver software ................... 13 Liquid ................................. 40
Computer Instrument description ................ 2 Solid ................................... 41
Connect ............................. 13 Instrument type .......................... 9 Sample size
Connect Size .................................... 39
Balance .............................. 21 K Sensor
Barcode reader ................... 23 Keyboard Connect ............................. 29
Computer ........................... 13 Connect ............................. 22 Serial number ............................. 9
Dosing device ..................... 16 KFT ............................................ 4 Service ....................................... 6
MSB devices ....................... 15 SET ............................................. 3
PC keyboard ....................... 22 L STAT ........................................... 3
Power grid .......................... 12 LED STDADD ..................................... 4
Printer ................................ 20 On ...................................... 44 Stirrer
Remote Box ........................ 18 LQH ........................................... 4 Connect ............................. 17
Stirrer ................................. 17 Stirring direction ....................... 24
Titration stand .................... 17 M Supply voltage ............................ 6
Touch Control ..................... 11 Maintenance ............................ 43 System test ............................... 11
USB hub ............................. 20 MEAS ......................................... 4
Connector Measuring interface ................ 2, 9 T
MSB ..................................... 2 Measuring mode ........................ 3 Temperature sensor
USB ...................................... 2 MEAS ................................... 4 Connect ............................. 29
Controller STDADD ............................... 4 Titrando system .......................... 1
Connector ............................ 9 MET ........................................... 3 Titration mode ............................ 3
Metrohm Serial Bus MSB, see also DET ...................................... 3
D "MSB" ...................................... 15 KFT ....................................... 4
DET ............................................ 3 MSB MET ..................................... 3
Device software Connect devices ................. 15 SET ....................................... 3
Update ................................. 2 Connector ............................ 9 STAT ..................................... 3
Differential potentiometry ......... 34 MSB connector ........................... 2 Titration stand
Dosing command ....................... 3 Connect ............................. 17
ADD ..................................... 4 O Titration vessel
EMPTY .................................. 4 Overview of the instrument ........ 8 Equipping ........................... 24