Metrohm 862 User manual

862 Compact Titrosampler
Manual
8.862.8002EN

Metrohm AG
CH-9101 Herisau
Switzerland
Phone [phone]
Fax [phone]
[email protected]
www.metrohm.com
862 Compact Titrosampler
Manual
8.862.8002EN 10/2009 dm/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
862 Compact Titrosampler ￭￭￭￭￭￭￭￭ III
Table of contents
1Introduction 1
1.1 Instrument description ......................................................... 1
1.1.1 Instrument components .......................................................... 1
1.1.2 Titration and measuring modes ................................................ 2
1.1.3 Intended use ........................................................................... 2
1.2 About the documentation ................................................... 3
1.2.1 Symbols and conventions ........................................................ 3
1.3 Safety instructions ................................................................ 4
1.3.1 General notes on safety ........................................................... 4
1.3.2 Electrical safety ........................................................................ 4
1.3.3 Tubing and capillary connections ............................................. 5
1.3.4 Personnel safety ...................................................................... 5
1.3.5 Flammable solvents and chemicals ........................................... 7
1.3.6 Recycling and disposal ............................................................. 7
2Overview of the instrument 8
3Installation 10
3.1 Setting up the instrument .................................................. 10
3.1.1 Packaging .............................................................................. 10
3.1.2 Checks .................................................................................. 10
3.1.3 Location ................................................................................ 10
3.2 Removing the safety shield and cable cover .................... 11
3.3 Mounting the Dosino ......................................................... 11
3.4 Connecting the Dosino ....................................................... 13
3.5 Setting up the titration head ............................................. 14
3.6 Connecting a stirrer ............................................................ 17
3.7 Connecting keyboard, printer and other USB devices .... 18
3.8 Connecting a balance ......................................................... 20
3.9 Connecting a sensor ........................................................... 21
3.10 Remote connections ........................................................... 23
3.10.1 Miscellaneous remote cables ................................................. 23
3.10.2 Example systems .................................................................... 24
3.11 Mounting the cable cover and the safety shield ............. 26
3.12 Connecting the mains cable .............................................. 27
4Titration and automation sequences 28
4.1 Dynamic equivalence point titration (DET) ....................... 28

Table of contents ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
IV ￭￭￭￭￭￭￭￭ 862 Compact Titrosampler
4.2 Monotonic equivalence point titration (MET) .................. 28
4.3 Endpoint titration (SET) ..................................................... 29
4.4 Automation sequences ...................................................... 29
4.4.1 Dipping in special .................................................................. 29
4.4.2 Dipping in special 2 ............................................................... 30
4.4.3 Double dipping ...................................................................... 31
4.4.4 Rinsing in sample ................................................................... 32
4.4.5 Rinsing in special ................................................................... 32
4.4.6 Pump control ......................................................................... 33
4.4.7 Dosing auxiliary solutions ....................................................... 34
5Operation 35
5.1 Switching the instrument on and off ............................... 35
5.2 Fundamentals of operation ............................................... 36
5.2.1 The keypad ............................................................................ 36
5.2.2 Structure of the dialog windows ............................................ 37
5.2.3 Navigating in the dialog ......................................................... 37
5.2.4 Entering text and numbers ..................................................... 38
5.2.5 Selecting from a selection list ................................................. 39
5.3 Formula editor .................................................................... 39
5.4 Methods .............................................................................. 41
5.4.1 Creating a new method ......................................................... 41
5.4.2 Saving a method ................................................................... 42
5.4.3 Loading a method ................................................................. 43
5.4.4 Exporting a method ............................................................... 44
5.5 Sample data ........................................................................ 45
5.5.1 Sample table ......................................................................... 45
5.5.2 Entering sample data in the main dialog ................................ 48
5.6 Performing a sample series ............................................... 49
5.6.1 Starting the sample series ...................................................... 49
5.6.2 Pausing a sample series and continuing ................................. 50
5.6.3 Status of the sample series ..................................................... 52
5.6.4 Special case: Calibrations ....................................................... 52
5.7 Live modifications .............................................................. 53
5.7.1 Editing the sample data of the running determination ............ 53
5.7.2 Editing the sample table while a determination is running ...... 54
5.7.3 Live parameters ..................................................................... 55
5.8 Results ................................................................................. 56
5.9 Statistics .............................................................................. 58
5.10 Printing a report manually ................................................. 59
5.11 Manual control ................................................................... 61
5.11.1 Rotating the sample rack ....................................................... 61
5.11.2 Moving the lift ....................................................................... 62
5.11.3 Dosing ................................................................................... 62

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862 Compact Titrosampler ￭￭￭￭￭￭￭￭ V
5.11.4 Measuring ............................................................................. 66
5.11.5 Stirring .................................................................................. 67
6System settings 69
6.1 Basic settings ...................................................................... 69
6.2 Lift settings (Lift) ................................................................ 72
6.3 Managing sensors .............................................................. 73
6.3.1 General ................................................................................. 73
6.3.2 Editing the sensor data .......................................................... 74
6.4 Managing solutions ............................................................ 75
6.4.1 General ................................................................................. 75
6.4.2 Editing the solution data ........................................................ 76
6.5 Managing common variables ............................................ 77
6.5.1 General ................................................................................. 77
6.5.2 Editing common variables ...................................................... 78
6.6 File management ................................................................ 79
6.7 Configuring external devices ............................................. 80
6.8 Instrument diagnosis .......................................................... 83
6.8.1 Loading program versions and language files ......................... 83
6.8.2 Diagnosis functions ............................................................... 84
7Parameters 85
7.1 Dynamic equivalence point titrations (DET) ..................... 85
7.1.1 Start conditions ..................................................................... 85
7.1.2 Titration parameters .............................................................. 86
7.1.3 Stop conditions ..................................................................... 91
7.1.4 Evaluation ............................................................................. 93
7.1.5 Calculation ............................................................................ 96
7.1.6 Statistics ................................................................................ 98
7.1.7 Reports .................................................................................. 98
7.2 Monotonic equivalence point titrations (MET) .............. 100
7.2.1 Start conditions ................................................................... 100
7.2.2 Titration parameters ............................................................ 101
7.2.3 Stop conditions ................................................................... 106
7.2.4 Evaluation ........................................................................... 107
7.2.5 Calculation .......................................................................... 110
7.2.6 Statistics .............................................................................. 112
7.2.7 Reports ................................................................................ 112
7.3 Endpoint titrations (SET) .................................................. 114
7.3.1 Conditioning ....................................................................... 114
7.3.2 Start conditions ................................................................... 115
7.3.3 Titration parameters ............................................................ 117
7.3.4 Control parameters EP1 ....................................................... 119
7.3.5 Control parameters EP2 ....................................................... 122
7.3.6 Stop conditions ................................................................... 122

Table of contents ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
VI ￭￭￭￭￭￭￭￭ 862 Compact Titrosampler
7.3.7 Calculation .......................................................................... 123
7.3.8 Statistics .............................................................................. 125
7.3.9 Reports ................................................................................ 125
7.4 pH calibration (CAL) ......................................................... 127
7.4.1 Calibration parameters ........................................................ 127
7.4.2 Buffers ................................................................................ 128
7.4.3 Reports ................................................................................ 129
7.5 Automation: Dipping in special ....................................... 130
7.6 Automation: Dipping in special 2 ................................... 131
7.7 Automation: Double dipping ........................................... 132
7.8 Automation: Rinsing in sample ....................................... 133
7.9 Automation: Rinsing in special ....................................... 134
8Handling and maintenance 135
8.1 General .............................................................................. 135
8.2 Quality Management and validation with Metrohm .... 135
9Troubleshooting 137
9.1 SET titration ...................................................................... 137
9.2 Miscellaneous ................................................................... 138
10 Appendix 139
10.1 Dosing unit ........................................................................ 139
10.1.1 Maximum dosing and filling rate .......................................... 139
10.1.2 Parameters for preparing (PREP) and emptying (EMPTY) ....... 139
10.2 Stirring rate ....................................................................... 140
10.3 Balance .............................................................................. 140
10.4 USB devices ....................................................................... 141
10.4.1 Numerical USB keypad 6.2147.000 ...................................... 141
10.4.2 Key assignment of a USB keyboard ...................................... 142
10.4.3 PC mouse ............................................................................ 142
10.4.4 Printer ................................................................................. 143
10.5 System initialization ......................................................... 143
10.6 Remote interface .............................................................. 145
10.6.1 Pin assignment of the remote interface ................................ 145
10.6.2 Status diagram of the remote interface ................................ 146
11 Technical specifications 147
11.1 Measuring inputs .............................................................. 147
11.1.1 Potentiometry ...................................................................... 147
11.1.2 Polarizer .............................................................................. 147
11.1.3 Temperature ........................................................................ 148

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862 Compact Titrosampler ￭￭￭￭￭￭￭￭ VII
11.2 Dosing drive ...................................................................... 149
11.3 Lift ..................................................................................... 149
11.4 Turntable ........................................................................... 149
11.5 Interfaces and connectors ............................................... 149
11.6 Mains connection ............................................................. 150
11.7 Safety specifications ........................................................ 150
11.8 Electromagnetic compatibility (EMC) ............................. 150
11.9 Ambient temperature ...................................................... 151
11.10 Reference conditions ........................................................ 151
11.11 Dimensions ........................................................................ 151
12 Conformity and warranty 152
12.1 Declaration of Conformity ............................................... 152
12.2 Warranty (guarantee) ....................................................... 153
12.3 Quality Management Principles ...................................... 154
13 Accessories 156
13.1 Scope of delivery 2.862.0010 ......................................... 156
13.2 Optional accessories ........................................................ 160
Index 163

Table of figures ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
VIII ￭￭￭￭￭￭￭￭ 862 Compact Titrosampler
Table of figures
Figure 1 Front 862 Compact Titrosampler ....................................................... 8
Figure 2 Rear 862 Compact Titrosampler ........................................................ 9
Figure 3 Removing shields ............................................................................. 11
Figure 4 Mounting the Dosino ...................................................................... 12
Figure 5 Connecting the Dosino .................................................................... 13
Figure 6 Equip the titration head ................................................................... 14
Figure 7 Installing rinsing nozzles and aspiration tip ...................................... 15
Figure 8 Setting up the distributor ................................................................. 16
Figure 9 Rod stirrer 802 Stirrer ...................................................................... 17
Figure 10 Connecting a stirrer ......................................................................... 17
Figure 11 Connecting USB devices ................................................................. 18
Figure 12 Connecting the USB stick ................................................................ 19
Figure 13 Connecting the 6.2147.000 USB keyboard with USB stick and
printer ............................................................................................. 20
Figure 14 Connecting the USB hub with USB stick, printer and the 6.2148.030
RS-232/USB Box (for connecting balances). ..................................... 20
Figure 15 Connecting a balance ...................................................................... 20
Figure 16 Connecting pH or redox electrodes ................................................. 21
Figure 17 Connecting a reference electrode .................................................... 22
Figure 18 Connecting a temperature sensor .................................................... 22
Figure 19 Connecting a polarizable electrode .................................................. 23
Figure 20 Remote cable with lettering ............................................................. 24
Figure 21 Remote connection 862 Compact Titrosampler - 843 Pump Station -
Dosimat plus ................................................................................... 24
Figure 22 Remote connection 862 Compact Titrosampler - Dosimat ............... 25
Figure 23 Mounting the shields ....................................................................... 26
Figure 24 Connecting the mains cable ............................................................ 27
Figure 25 Reagent dosing for DET ................................................................... 28
Figure 26 Reagent dosing for MET .................................................................. 28
Figure 27 Reagent dosing for SET ................................................................... 29
Figure 28 Keypad 862 Compact Titrosampler .................................................. 36
Figure 29 Directory structure on the USB stick ................................................. 80
Figure 30 Tubbs method for determining the equivalence point ...................... 96
Figure 31 Rotational speed depending on stirring rate .................................. 140
Figure 32 Pin assignment of remote socket and plug .................................... 145
Figure 33 Remote status diagram .................................................................. 146

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862 Compact Titrosampler ￭￭￭￭￭￭￭￭ 1
1 Introduction
1.1 Instrument description
The 862 Compact Titrosampler is a versatile analysis instrument which
combines a titrator and a compact sample changer in a single unit. It is
the central control instrument in an automation system that can also
include, in addition to a Dosimat (for adding auxiliary solutions), a pump
for rinsing and aspirating the sample vessels.
Given automation sequences and titration modes can be individually para-
meterized and saved as sample-specific methods. Methods can be expor-
ted on a USB stick and then copied onto another instrument quickly and
easily.
1.1.1 Instrument components
The 862 Compact Titrosampler has the following components:
￭Turntable
Permanently mounted sample rack with 11 positions for sample beak-
ers and one position for a rinsing beaker.
￭Lift with titration head
For two electrodes, one rod stirrer, two dosing tips, one aspiration tip
and three rinsing nozzles.
￭Sensor connectors
Four connectors for the following sensor types:
– pH or redox electrodes
– reference electrodes
– polarizable electrodes
– temperature sensors (Pt1000 or NTC)
￭Stirrer connector
For a rod stirrer with propeller stirrer.
￭MSB connector (Metrohm Serial Bus)
For connecting a Dosino.
￭USB (OTG) connector
The 6.2151.100 adapter can be used to connect, for example, a USB
hub or a USB stick (for system backup or method export).
￭Remote connector
For connecting a Dosimat and/or an 843 Pump Station as well as other
instruments with a remote interface.

1.1 Instrument description ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
2￭￭￭￭￭￭￭￭ 862 Compact Titrosampler
1.1.2 Titration and measuring modes
The following titration and measuring modes are supported:
￭DET
Dynamic equivalence point titration. The reagent is added in variable
volume steps.
Measuring modes:
–pH (potentiometric pH measurement)
–U (potentiometric voltage measurement)
–Ipol (voltametric measurement with adjustable polarization cur-
rent)
–Upol (amperometric measurement with adjustable polarization
voltage)
￭MET
Monotonic equivalence point titration. The reagent is added in con-
stant volume steps.
Measuring modes:
–pH (potentiometric pH measurement)
–U (potentiometric voltage measurement)
–Ipol (voltametric measurement with adjustable polarization cur-
rent)
–Upol (amperometric measurement with adjustable polarization
voltage)
￭SET
Endpoint titration at one or two specified endpoints.
Measuring modes:
–pH (potentiometric pH measurement)
–U (potentiometric voltage measurement)
–Ipol (voltametric measurement with adjustable polarization cur-
rent)
–Upol (amperometric measurement with adjustable polarization
voltage)
￭CAL
Electrode calibration.
Measuring mode:
–pH (calibration of pH electrodes)
1.1.3 Intended use
The 862 Compact Titrosampler is designed for usage as an automation
system in analytical laboratories. It is not suitable for usage in biochemi-
cal, biological or medical environments in its basic equipment version.
This instrument is suitable for dosing chemicals and flammable solvents.
The usage of the 862 Compact Titrosampler 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

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862 Compact Titrosampler ￭￭￭￭￭￭￭￭ 3
prevention measures prescribed for laboratories or production plants is
also mandatory.
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
second 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.

1.3 Safety instructions ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
4￭￭￭￭￭￭￭￭ 862 Compact Titrosampler
Caution
This symbol draws attention to a possible damage of
instruments or instrument parts.
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
damaged 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.

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862 Compact Titrosampler ￭￭￭￭￭￭￭￭ 5
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).
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
connections. 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 manda-
tory.
1.3.4 Personnel safety
Warning
Wear protective goggles and working clothes suitable for laboratory
work while operating the 862 Compact Titrosampler. It is also advisable
to wear gloves when caustic liquids are used or in situations where
glass vessels could break.

1.3 Safety instructions ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
6￭￭￭￭￭￭￭￭ 862 Compact Titrosampler
Warning
Always install the safety shield supplied with the equipment before
using the instrument for the first time. Pre-installed safety shields are
not allowed to be removed.
The 862 Compact Titrosampler may not be operated without a safety
shield!
Warning
Personnel are not permitted to reach into the working area of the
instrument while operations are running!
A considerable risk of injury exists for the user.
Warning
In the event of a possible blockage of a drive, the mains plug must be
pulled out of the socket immediately. Do not attempt to free jammed
sample vessels or other parts while the device is switched on. Blockages
can only be cleared when the instrument is in a voltage-free status; this
action generally involves a considerable risk of injury.
Warning
The 862 Compact Titrosampler is not suitable for utilization in bio-
chemical, biological or medical environments in its basic equipment ver-
sion.
Appropriate protective measures must be implemented in the event
that potentially infectious samples or reagents are being processed.

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862 Compact Titrosampler ￭￭￭￭￭￭￭￭ 7
1.3.5 Flammable solvents and chemicals
Warning
All relevant safety measures are to be observed when working with
flammable solvents and chemicals.
￭Set up the instrument in a well-ventilated location.
￭Keep all sources of flame far from the workplace.
￭Clean up spilled fluids and solids immediately.
￭Follow the safety instructions of the chemical manufacturer.
1.3.6 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.
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.

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8￭￭￭￭￭￭￭￭ 862 Compact Titrosampler
2 Overview of the instrument
1
2
3
4
5
6
7
Figure 1 Front 862 Compact Titrosampler
1Safety shield (6.2751.130)
With knurled screws for mounting. The
safety shield can be folded up.
2Titration head
With two retracted dosing tips and four
stoppers.
3Sample rack
For 11 sample beakers and one rinsing
beaker (6.1459.300, 120 mL)
4Display
5Keypad 6Dosino holder (6.2057.110)
For fixing the dosing drive and the titrant
bottle (1 L).
7Special position
For a rinsing beaker

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862 Compact Titrosampler ￭￭￭￭￭￭￭￭ 9
1
2
3 4 5 6 7 8 9 10 11 12
Figure 2 Rear 862 Compact Titrosampler
1Warning symbol
(see Chapter 1.3.4, page 5)
2Tubing and cable cover
3Electrode connector (Ind.)
For connecting pH or redox electrodes with
integrated or separate reference electrode.
Socket F.
4Electrode connector (Ref.)
For connecting reference electrodes. Socket
B, 4 mm.
5Temperature sensor connector
For connecting temperature sensors of the
Pt1000 or NTC types. Two B sockets, 2 mm.
6Electrode connector (Pol.)
For connecting polarizable electrodes, e g.
double Pt electrodes. Socket F.
7Remote connector
For connecting instruments with a remote
interface. D-Sub, 9-pin.
8MSB connector
Metrohm Serial Bus.
For connecting the 800 Dosino. Mini DIN,
9-pin.
9USB (OTG) connector
For connecting printers, USB sticks, USB
hubs, etc.
10 Stirrer connection
For 802 Stirrer (rod stirrer).
11 Mains connection socket 12 Type plate
Contains specifications concerning mains
voltage and serial number.

3.1 Setting up the instrument ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
10 ￭￭￭￭￭￭￭￭ 862 Compact Titrosampler
3 Installation
3.1 Setting up the instrument
3.1.1 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.
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, free of vibrations, protected from corrosive atmosphere, and
contamination by chemicals.
The instrument should be protected against excessive temperature fluctu-
ations and direct sunlight.