Metrohm 870 KF Titrino plus User manual

870 KF Titrino plus
Manual
8.870.8003EN

Metrohm AG
CH-9101 Herisau
Switzerland
Phone [phone]
Fax [phone]
[email protected]
www.metrohm.com
870 KF Titrino plus
Manual
8.870.8003EN 10.2009 jb

Teachware
Metrohm AG
CH-9101 Herisau
[email protected]
This documentation is protected by copyright. All rights reserved.
Although all the information given in this documentation has been checked
with great care, errors cannot be entirely excluded. Should you notice any
mistakes please send us your comments using the address given above.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of contents
870 KF Titrino plus ￭￭￭￭￭￭￭￭ III
Table of contents
1Introduction 1
1.1 Instrument description ......................................................... 1
1.1.1 Titration and measuring modes ................................................ 1
1.1.2 Connectors .............................................................................. 1
1.1.3 Intended use ........................................................................... 1
1.2 About the documentation ................................................... 2
1.2.1 Symbols and conventions ........................................................ 2
1.3 Safety instructions ................................................................ 3
1.3.1 General notes on safety ........................................................... 3
1.3.2 Electrical safety ........................................................................ 3
1.3.3 Tubing and capillary connections ............................................. 4
1.3.4 Flammable solvents and chemicals ........................................... 4
1.3.5 Recycling and disposal ............................................................. 4
2Overview of the instrument 6
3Water determination according to Karl Fischer (KFT) 8
4Installation 9
4.1 Setting up the instrument .................................................... 9
4.1.1 Packaging ................................................................................ 9
4.1.2 Checks .................................................................................... 9
4.1.3 Location .................................................................................. 9
4.2 Connecting a sensor ............................................................. 9
4.3 Connecting a stirrer ............................................................ 10
4.4 Connecting a balance ......................................................... 10
4.5 Connecting keyboard, printer and other USB devi-
ces ........................................................................................ 11
4.6 Connecting instruments to the remote connector .......... 14
4.7 Attaching the exchange unit ............................................. 14
5Operation 16
5.1 Switching the instrument on and off ............................... 16
5.2 Fundamentals of operation ............................................... 17
5.2.1 The keypad ............................................................................ 17
5.2.2 Structure of the dialog windows ............................................ 17
5.2.3 Navigating in the dialog ......................................................... 18
5.2.4 Entering text and numbers ..................................................... 18
5.2.5 Selecting from a selection list ................................................. 19

Table of contents ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
IV ￭￭￭￭￭￭￭￭ 870 KF Titrino plus
5.3 Methods .............................................................................. 20
5.3.1 Method templates ................................................................. 20
5.3.2 Loading a method ................................................................. 20
5.3.3 Saving a method ................................................................... 21
5.3.4 Exporting a method ............................................................... 21
5.4 Sample data ........................................................................ 22
5.4.1 Entering sample data in the main dialog ................................ 22
5.4.2 Requesting sample data at the time of determination
start ...................................................................................... 23
5.5 Carrying out a determination ............................................ 24
5.6 Live modifications .............................................................. 27
5.6.1 Editing the sample data of the running determination ............ 27
5.6.2 Live parameters ..................................................................... 28
5.7 Results ................................................................................. 29
5.8 Statistics .............................................................................. 30
5.9 Printing a report manually ................................................. 31
5.10 Manual Control ................................................................... 33
5.10.1 Dosing ................................................................................... 33
5.10.2 Stirring .................................................................................. 37
6System settings 39
6.1 Basic settings ...................................................................... 39
6.2 Managing solutions ............................................................ 42
6.2.1 General ................................................................................. 42
6.2.2 Editing the solution data ........................................................ 43
6.3 File management ................................................................ 44
6.4 Configuring external devices ............................................. 46
6.5 Instrument diagnosis .......................................................... 48
6.5.1 Loading program versions and language files ......................... 48
6.5.2 Diagnosis functions ............................................................... 50
7Parameters 51
7.1 Karl Fischer Titrations (KFT) .............................................. 51
7.1.1 Conditioning ......................................................................... 51
7.1.2 Start conditions ..................................................................... 52
7.1.3 Control parameters ................................................................ 53
7.1.4 Titration parameters .............................................................. 56
7.1.5 Stop conditions ..................................................................... 58
7.1.6 Calculations - Methods "Blank Ipol/Upol" ............................... 59
7.1.7 Calculations - Methods "Titer Ipol/Upol" ................................ 60
7.1.8 Calculations - Methods "KFT Ipol/Upol", "KFT Ipol/Upol–
Blank" ................................................................................... 61
7.1.9 Statistics ................................................................................ 63
7.1.10 Reports .................................................................................. 63

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of contents
870 KF Titrino plus ￭￭￭￭￭￭￭￭ V
8Handling and maintenance 65
8.1 Quality Management and validation with Metrohm ....... 65
9Troubleshooting 66
9.1 Karl Fischer titration .......................................................... 66
9.2 Miscellaneous ..................................................................... 67
10 Appendix 69
10.1 Exchange unit ..................................................................... 69
10.1.1 Maximum dosing and filling rate ............................................ 69
10.1.2 Parameters for the preparing (PREP) ....................................... 69
10.2 Stirring rate ......................................................................... 69
10.3 Balance ................................................................................ 70
10.4 USB devices ......................................................................... 71
10.4.1 Numerical USB keypad 6.2147.000 ........................................ 71
10.4.2 Key assignment of a USB keyboard ........................................ 71
10.4.3 PC mouse .............................................................................. 72
10.4.4 Printer ................................................................................... 73
10.5 System initialization ........................................................... 73
10.6 Remote interface ................................................................ 74
10.6.1 Pin assignment of the remote interface .................................. 74
10.6.2 Status diagram of the remote interface .................................. 75
10.7 Remote control via an RS-232 connection ....................... 76
10.7.1 Commands and variables ....................................................... 77
11 Technical specifications 79
11.1 Measuring inputs ................................................................ 79
11.1.1 Polarizer ................................................................................ 79
11.2 Dosing drive ........................................................................ 80
11.3 Interfaces ............................................................................. 80
11.4 Mains connection ............................................................... 80
11.5 Safety specification ............................................................ 80
11.6 Electromagnetic compatibility (EMC) ................................ 81
11.7 Ambient temperature ......................................................... 81
11.8 Reference conditions .......................................................... 81
11.9 Dimensions .......................................................................... 82
12 Conformity and warranty 83
12.1 Declaration of Conformity ................................................. 83
12.2 Quality Management Principles ........................................ 84

Table of contents ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
VI ￭￭￭￭￭￭￭￭ 870 KF Titrino plus
12.3 Warranty (guarantee) ......................................................... 85
13 Accessories 86
13.1 Scope of delivery ................................................................ 86
13.2 Optional accessories ........................................................... 91
Index 93

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of figures
870 KF Titrino plus ￭￭￭￭￭￭￭￭ VII
Table of figures
Figure 1 Front 870 KF Titrino plus ................................................................... 6
Figure 2 Rear 870 KF Titrino plus .................................................................... 7
Figure 3 Reagent dosing for KFT ..................................................................... 8
Figure 4 Connecting a polarizable electrode .................................................... 9
Figure 5 Connecting a stirrer ......................................................................... 10
Figure 6 Connecting a balance ...................................................................... 11
Figure 7 Connecting USB devices ................................................................. 11
Figure 8 Connecting the USB stick ................................................................ 13
Figure 9 Connecting the 6.2147.000 USB keyboard with USB stick and
printer ............................................................................................. 13
Figure 10 Connecting the USB hub with USB stick, printer and the 6.2148.030
RS-232/USB Box (for connecting balances). ..................................... 13
Figure 11 Connecting a remote cable ............................................................. 14
Figure 12 Attaching the exchange unit ........................................................... 14
Figure 13 Keypad 870 KF Titrino plus .............................................................. 17
Figure 14 Directory structure on the USB stick ................................................. 45
Figure 15 Rotational speed depending on stirring rate .................................... 70
Figure 16 Pin assignment of remote socket and plug ...................................... 74
Figure 17 Remote status diagram .................................................................... 75
Figure 18 Connecting the RS-232/USB Box to the PC ...................................... 76

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1 Introduction
870 KF Titrino plus ￭￭￭￭￭￭￭￭ 1
1 Introduction
1.1 Instrument description
The 870 KF Titrino plus is an instrument used for volumetric water determi-
nation according to Karl Fischer. There are method templates available
which are already configured except for a few parameters. If parameters are
changed, then these will be saved automatically. The methods can be expor-
ted on a connected USB stick. This function makes it possible for you to copy
methods quickly and easily from one instrument to another.
1.1.1 Titration and measuring modes
The following titration and measuring modes are supported:
￭KFT
Volumetric water determination according to Karl Fischer.
Measuring modes:
–Ipol (voltametric measurement with adjustable polarization cur-
rent)
–Upol (amperometric measurement with adjustable polarization
voltage)
1.1.2 Connectors
The instrument is equipped with the following connectors:
￭MSB connector (Metrohm Serial Bus)
For connecting a stirrer.
￭USB (OTG) connector
The 6.2151.100 adapter can be used to connect, for example, a printer,
a USB Stick or a USB keyboard.
￭Electrode connector
For connecting polarizable electrodes.
￭Remote connector
For connecting instruments with a remote interface.
1.1.3 Intended use
The 870 KF Titrino plus is designed for usage as a titrator in analytical labo-
ratories. Its main application field is volumetric titration.
The present instrument is suitable for processing chemicals and flammable
samples. The usage of the 870 KF Titrino plus therefore requires that the
user has basic knowledge and experience in the handling of toxic and caustic
substances. Knowledge with respect to the application of the fire prevention
measures prescribed for laboratories is also mandatory.

1.2 About the documentation ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
2￭￭￭￭￭￭￭￭ 870 KF Titrino plus
1.2 About the documentation
Caution
Please read through this documentation carefully before putting the
instrument into operation. The documentation contains information and
warnings which have to be followed by the user in order to ensure safe
operation of the instrument.
1.2.1 Symbols and conventions
The following symbols and styles are used in this documentation:
Cross-reference to figure legend
The first number refers to the figure number, the sec-
ond to the instrument part in the figure.
Instruction step
Carry out these steps in the sequence shown.
Method Dialog text, parameter in the software
File ▶ New Menu or menu item
[Next] Button or key
Warning
This symbol draws attention to a possible life hazard
or risk of injury.
Warning
This symbol draws attention to a possible hazard due
to electrical current.
Warning
This symbol draws attention to a possible hazard due
to heat or hot instrument parts.
Warning
This symbol draws attention to a possible biological
hazard.
Caution
This symbol draws attention to a possible damage of
instruments or instrument parts.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1 Introduction
870 KF Titrino plus ￭￭￭￭￭￭￭￭ 3
Note
This symbol marks additional information and tips.
1.3 Safety instructions
1.3.1 General notes on safety
Warning
This instrument may only be operated in accordance with the specifica-
tions in this documentation.
This instrument has left the factory in a flawless state in terms of technical
safety. To maintain this state and ensure non-hazardous operation of the
instrument, the following instructions must be observed carefully.
1.3.2 Electrical safety
The electrical safety when working with the instrument is ensured as part of
the international standard IEC 61010.
Warning
Only personnel qualified by Metrohm are authorized to carry out service
work on electronic components.
Warning
Never open the housing of the instrument. The instrument could be dam-
aged by this. There is also a risk of serious injury if live components are
touched.
There are no parts inside the housing which can be serviced or replaced
by the user.
Mains voltage
Warning
An incorrect mains voltage can damage the instrument.
Only operate this instrument with a mains voltage specified for it (see rear
panel of the instrument).

1.3 Safety instructions ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
4￭￭￭￭￭￭￭￭ 870 KF Titrino plus
Protection against electrostatic charges
Warning
Electronic components are sensitive to electrostatic charges and can be
destroyed by discharges.
Always pull the mains cable out of the mains connection socket before
connecting or disconnecting electrical appliances on the rear panel of the
instrument.
1.3.3 Tubing and capillary connections
Caution
Leaks in tubing and capillary connections are a safety risk. Tighten all
connections well by hand. Avoid applying excessive force to tubing con-
nections. Damaged tubing ends lead to leakage. Appropriate tools can
be used to loosen connections.
Check the connections regularly for leakage. If the instrument is used
mainly in unattended operation, then weekly inspections are mandatory.
1.3.4 Flammable solvents and chemicals
Warning
All relevant safety measures are to be observed when working with flam-
mable solvents and chemicals.
￭Set up the instrument in a well-ventilated location (e.g. laboratory
flue).
￭Keep all sources of flame far from the workplace.
￭Clean up spilled fluids and solids immediately.
￭Follow the safety instructions of the chemical manufacturer.
1.3.5 Recycling and disposal
This product is covered by European Directive 2002/96/EC, WEEE – Waste
from Electrical and Electronic Equipment.
The correct disposal of your old equipment will help to prevent negative
effects on the environment and public health.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1 Introduction
870 KF Titrino plus ￭￭￭￭￭￭￭￭ 5
More details about the disposal of your old equipment can be obtained from
your local authorities, from waste disposal companies or from your local
dealer.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
6￭￭￭￭￭￭￭￭ 870 KF Titrino plus
2 Overview of the instrument
2
5
4
3
1
Figure 1 Front 870 KF Titrino plus
1Piston rod
Of the dosing drive.
2Contact pins
For the data chip.
3Coupling
For switching the flat stopcock.
4Display
5Keypad

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2 Overview of the instrument
870 KF Titrino plus ￭￭￭￭￭￭￭￭ 7
1
25
4
3
6
Figure 2 Rear 870 KF Titrino plus
1Type plate
Contains specifications concerning mains
voltage and serial number.
2Mains connection socket
3USB (OTG) connector
For connecting printers, USB sticks, USB hubs,
etc.
4MSB connector
Metrohm Serial Bus.
For connecting a stirrer. Mini DIN, 9-pin.
5Remote connector
For connecting instruments with a remote
interface. D-Sub, 9-pin.
6Electrode connector (Pol.)
For connecting polarizable electrodes, e.g.
double Pt electrodes. Socket F.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
8￭￭￭￭￭￭￭￭ 870 KF Titrino plus
3 Water determination according to Karl Fischer
(KFT)
Karl Fischer Titration is a method for volumetric water determination. Con-
ditioning is carried out automatically both before and after the actual
titration. The reagent dosing is controlled in such a way that a predefined
endpoint is reached as quickly and as accurately as possible. The volume
steps and the rate of reagent dosing are regulated by the difference between
the current measured value and the predefined endpoint. This means that
titration is performed more slowly in the control range and that smaller vol-
umes are added. The titration is stopped at the endpoint either drift-
controlled or after a waiting time. The volume dosed until the endpoint is
used to calculate the water content of the sample.
EP
KFT Ipol
KFT Upol EP
V/mL
Continuous
dosing
Initial
dosing
V/mL
V/mL
U/mV
t/s
I/µA
Control range
Control range
Figure 3 Reagent dosing for KFT

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Installation
870 KF Titrino plus ￭￭￭￭￭￭￭￭ 9
4 Installation
4.1 Setting up the instrument
4.1.1 Packaging
The instrument is supplied in highly protective special packaging together
with the separately packed accessories. Keep this packaging, as only this
ensures safe transportation of the instrument.
4.1.2 Checks
Immediately after receipt, check whether the shipment has arrived complete
and without damage by comparing it with the delivery note.
4.1.3 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 suitable for operation
and free of vibrations, if possible protected from corrosive atmospheres and
contamination by chemicals.
The instrument should be protected against excessive temperature fluctua-
tions and direct sunlight.
4.2 Connecting a sensor
Connecting a polarizable electrode
Figure 4 Connecting a polarizable electrode

4.3 Connecting a stirrer ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
10 ￭￭￭￭￭￭￭￭ 870 KF Titrino plus
Note
The electrode cable is protected against accidental disconnection of the
cable by means of a pull-out protection feature. If you wish to remove
the plug, then you must first retract the outer plug sleeve.
4.3 Connecting a stirrer
You can connect the following stirrers:
￭801 Stirrer
￭803 Ti Stand
￭804 Ti Stand (requires rod stirrer)
Figure 5 Connecting a stirrer
Caution
Make sure that the flat side of the plug matches the marking on the
socket.
4.4 Connecting a balance
Balances are equipped with a serial RS-232 interface as a rule. To connect a
balance, you require a 6.2148.030 RS-232/USB Box.