Metrohm 899 Coulometer User manual

899 Coulometer
Manual – Short Instructions
8.899.8002EN / 2014-10-24

Metrohm AG
CH-9100 Herisau
Switzerland
Phone [phone]
Fax [phone]
[email protected]
www.metrohm.com
899 Coulometer
Manual – Short Instructions
8.899.8002EN / 2014-10-24 ebe

Technische Dokumentation
Metrohm AG
CH-9100 Herisau
[email protected]
This documentation is protected by copyright. All rights reserved.
This document has been prepared with great care. However, errors can
never be entirely ruled out. Please send comments regarding possible
errors to the address above.
Documentation in additional languages can be found on
http://documents.metrohm.com.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of contents
899 Coulometer ￭￭￭￭￭￭￭￭ III
Table of contents
1 About these short instructions 1
2 Introduction 2
2.1 Instrument description ......................................................... 2
2.1.1 Connectors .............................................................................. 2
2.1.2 Intended use ........................................................................... 3
2.2 About the documentation ................................................... 3
2.2.1 Symbols and conventions ........................................................ 3
2.3 Safety instructions ................................................................ 4
2.3.1 General notes on safety ........................................................... 4
2.3.2 Electrical safety ........................................................................ 4
2.3.3 Tubing and capillary connections ............................................. 5
2.3.4 Flammable solvents and chemicals ........................................... 6
2.3.5 Recycling and disposal ............................................................. 6
3 Overview of the instrument 7
3.1 Front ...................................................................................... 7
3.2 Rear ........................................................................................ 8
4 Installation 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 Setting up the titration cell for coulometry ..................... 10
4.2.1 Inserting the titration cell ....................................................... 10
4.2.2 Preparing the titration cell ...................................................... 10
4.2.3 Mounting the addition and aspiration tube (utilization with Ti
Stand) ................................................................................... 14
4.2.4 Using the titration cell with a Karl Fischer oven ...................... 15
4.2.5 Using the titration cell with a sample changer ........................ 15
4.3 Connecting the coulometer to the power supply ............ 15
4.3.1 Connecting the power supply unit ......................................... 15
4.3.2 Connecting the Power Box .................................................... 16
4.4 Connecting sensors ............................................................ 18
4.4.1 Connecting a generator electrode .......................................... 18
4.4.2 Connecting an indicator electrode ......................................... 19
4.4.3 Connecting a temperature sensor .......................................... 21
4.5 Connecting an additional stirrer ....................................... 22
4.6 Connecting a balance ......................................................... 23

Table of contents ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
IV ￭￭￭￭￭￭￭￭ 899 Coulometer
4.7 Connecting a keyboard, printer and other USB devi-
ces ........................................................................................ 25
4.8 Connecting a sample changer to the remote connec-
tor ........................................................................................ 28
5 Operation 29
5.1 Switching the instrument on and off ............................... 29
5.2 Fundamentals of operation ............................................... 30
5.2.1 The keypad ............................................................................ 30
5.2.2 Structure of the dialog windows ............................................ 30
5.2.3 Navigating in the dialog ......................................................... 31
5.2.4 Entering text and numbers ..................................................... 31
5.2.5 Selecting from a selection list ................................................. 32
5.3 Formula editor .................................................................... 33
5.4 Methods .............................................................................. 34
5.4.1 Method templates ................................................................. 34
5.4.2 Loading a method template ................................................... 34
5.4.3 Saving a method ................................................................... 35
5.4.4 Exporting a method ............................................................... 36
5.5 Control ................................................................................. 37
5.6 Sample data ........................................................................ 38
5.6.1 Entering sample data in the main dialog ................................ 38
5.6.2 Requesting sample data at the start of the determination ...... 39
5.7 Sample table ....................................................................... 40
5.7.1 General ................................................................................. 40
5.7.2 Editing the sample data ......................................................... 42
5.7.3 Sending the sample size from a balance ................................. 43
5.8 Carrying out a determination ............................................ 44
5.9 Live modifications .............................................................. 47
5.9.1 Editing the sample data of the running determination ............ 47
5.9.2 Editing the sample table while a determination is running ...... 48
5.9.3 Editing the live parameters ..................................................... 49
5.10 Results ................................................................................. 50
5.11 Statistics .............................................................................. 51
5.12 Printing a report manually ................................................. 53
5.13 Manual control ................................................................... 54
5.13.1 Stirring .................................................................................. 54
Index 56

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1 About these short instructions
899 Coulometer ￭￭￭￭￭￭￭￭ 1
1 About these short instructions
The present short instructions contain important chapters from the more
detailed manual. In addition to an introduction, safety instructions and an
overview of the instruments, you will also find information about the
installation and operation of the 899 Coulometer in addition to informa-
tion regarding the warranty. You will find the detailed manual as a PDF
file at http://products.metrohm.com under Literature/Technical docu-
mentation.

2.1 Instrument description ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
2￭￭￭￭￭￭￭￭ 899 Coulometer
2 Introduction
2.1 Instrument description
The 899 Coulometer is a titrator used for coulometric water content
determination according to Karl Fischer. There are method templates
available which are already configured except for a few parameters. The
methods can be modified and stored under a new name. The methods
can be exported to a connected USB flash drive. This function makes it
possible for you to copy methods quickly and easily from one instrument
to another.
The 899 Coulometer has an integrated magnetic stirrer that is visible on
the top side of the housing. The titration cell (coulometry) can easily be
attached to the magnetic stirrer. Thanks to its compact construction, you
can use the instrument in a small space as a stand-alone titrator. Further-
more, the remote interface permits you to connect a sample changer with
oven module and to perform automated determinations.
As an alternative to the power supply with the power supply unit provi-
ded, the 899 Coulometer can also be operated by means of an accumula-
tor (a so-called Power Box). The Power Box is available as optional equip-
ment. It is particularly appropriate for use in environments where the
power supply is either unstable or absent.
2.1.1 Connectors
The instrument is equipped with the following connectors:
￭Electrical connection
For connecting to the power supply with the aid of the power supply
unit provided or for connecting to the 6.2164.500 Power Box.
￭MSB connector (Metrohm Serial Bus)
For connecting an additional stirrer.
￭USB (OTG) connector
The 6.2151.100 adapter can be used to connect, for example, a
printer, a USB flash drive or a USB keyboard.
￭Sensor connectors
Three connectors for the following sensor types:
– Double Pt electrode
– Generator electrode
– Temperature sensor (Pt1000)
￭Grounding socket
For grounding the coulometer.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2 Introduction
899 Coulometer ￭￭￭￭￭￭￭￭ 3
￭Remote connector
For connecting instruments with a remote interface (e.g. 885 Compact
Oven SC).
2.1.2 Intended use
The 899 Coulometer is designed for usage as a titrator in analytical labora-
tories. Its application field is coulometric water content determination
according to Karl Fischer.
The present instrument is suitable for processing chemicals and flammable
samples. Usage of the 899 Coulometer therefore requires the user to have
basic knowledge and experience in handling toxic and caustic substances.
Knowledge with respect to the application of the fire prevention measures
prescribed for laboratories is also mandatory.
2.2 About the documentation
CAUTION
Please read through this documentation carefully before putting the
instrument into operation. The documentation contains information
and warnings which the user must follow in order to ensure safe opera-
tion of the instrument.
2.2.1 Symbols and conventions
The following symbols and formatting may appear 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-threat-
ening hazard or risk of injury.

2.3 Safety instructions ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
4￭￭￭￭￭￭￭￭ 899 Coulometer
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 possible damage to
instruments or instrument parts.
NOTE
This symbol highlights additional information and
tips.
2.3 Safety instructions
2.3.1 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.
2.3.2 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.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2 Introduction
899 Coulometer ￭￭￭￭￭￭￭￭ 5
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.
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.
Do not fail to pull the mains cable out of the mains connection socket
before you set up or disconnect electrical plug connections at the rear
of the instrument.
2.3.3 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.

2.3 Safety instructions ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
6￭￭￭￭￭￭￭￭ 899 Coulometer
2.3.4 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 (e.g. fume cup-
board).
￭Keep all sources of flame far from the workplace.
￭Clean up spilled liquids and solids immediately.
￭Follow the safety instructions of the chemical manufacturer.
2.3.5 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.
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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899 Coulometer ￭￭￭￭￭￭￭￭ 7
3 Overview of the instrument
3.1 Front
1
2
3
Figure 1 Front 899 Coulometer
1Magnetic stirrer
For attaching the titration vessel holder.
2Display
3Keypad

3.2 Rear ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
8￭￭￭￭￭￭￭￭ 899 Coulometer
3.2 Rear
1 2 345 6 78 9
Figure 2 Rear 899 Coulometer
1Type plate
Contains the serial number.
2Remote connector
For connecting instruments with a remote
interface. D-Sub, 9-pin.
3Electrode connector (Ind.)
For connecting a metal electrode (double Pt
wire electrode). Socket F.
4Temperature sensor connector (Temp.)
For connecting a temperature sensor of the
type Pt1000. Two B sockets, 2 mm.
5MSB connector (MSB 1)
Metrohm Serial Bus. For connecting an
external stirrer. Mini DIN, 8-pin.
6USB (OTG) connector
For connecting printers, USB flash drives,
USB hubs, etc.
7Mains connection socket (Power)
For connecting the external power supply
unit or a Power Box (6.2164.500).
8Electrode connector (Gen.)
For connecting a generator electrode.
9Grounding socket
For grounding the Coulometer. Socket B,
4 mm.

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899 Coulometer ￭￭￭￭￭￭￭￭ 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 com-
plete 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 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.

4.2 Setting up the titration cell for coulometry ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
10 ￭￭￭￭￭￭￭￭ 899 Coulometer
4.2 Setting up the titration cell for coulometry
4.2.1 Inserting the titration cell
6.2047.030
6.1464.320
1
2
Figure 3 Inserting the titration cell (coulometry)
Set up the titration cell on the magnetic stirrer as follows:
1Attach the 6.2047.030 titration vessel holder to the magnetic stirrer.
2Insert the 6.1464.320 titration cell into the titration vessel holder.
4.2.2 Preparing the titration cell
Filling the adsorber tube
Before setting up the titration cell, the 6.1403.030 adsorber tube has to
be filled with 6.2811.000 molecular sieve. Proceed as follows:

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Installation
899 Coulometer ￭￭￭￭￭￭￭￭ 11
6.1403.030
6.2811.000
1
2
3
4
Figure 4 Filling the adsorber tube
1Insert a small cotton plug into the bottom of the adsorber tube. Do
not pack the cotton too tightly.
2Fill the molecular sieve up to ¾ of the height.
3Place a small cotton plug on the molecular sieve. Do not pack the
cotton too tightly.
4Seal the adsorber tube with the appropriate cover.
NOTE
Note that the molecular sieve must be replaced at regular intervals.
Each time you refill the adsorber tube with molecular sieve, you can, for
example, write the date directly on the adsorber tube.

4.2 Setting up the titration cell for coulometry ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
12 ￭￭￭￭￭￭￭￭ 899 Coulometer
Equipping the titration cell
6.1903.030
6.1464.320
6.2713.010
6.1437.000
6.0345.100
6.2713.020
6.1403.030
6.1448.020
6.2701.040
6.2713.000
6.0341.100
2
1
2
5
2
3
4
6
6.0344.100
Figure 5 Equipping the titration cell (coulometry)
Equip the titration cell as follows:
1Place the 6.1903.030 stirring bar in the titration cell.
2Cut the 6.2713.0x0 ground-joint sleeves to the correct length and
attach them to the ground joints of the inserts (electrodes, adsorber
tube, etc.).
Make sure that the edges of the ground-joint sleeves are cut to size
cleanly and that there are no fringes. The ground-joint sleeves must
not protrude at the lower edge of the ground-joint opening.
3Insert the 6.1403.030 adsorber tube into the generator electrode.

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Installation
899 Coulometer ￭￭￭￭￭￭￭￭ 13
4Insert the 6.0345.100 generator electrode without diaphragm or the
6.0344.100 generator electrode with diaphragm together with the
adsorber tube into the large ground-joint opening at the rear.
5Insert the 6.0341.100 indicator electrode into the left ground-joint
opening.
6Place the 6.1448.020 septum on the front opening of the titration
cell and screw it shut with the 6.2701.040 screw cap.
Tighten the screw cap only enough so that it seals. The septum is not
permitted to bend.
Filling the titration cell (generator electrode with dia-
phragm)
Proceed as follows when using a generator electrode with a diaphragm:
1Fill approximately 5 mL of catholyte into the generator electrode.
2Fill approximately 100 mL of anolyte into the titration cell with the
aid of the 6.2738.000 funnel. The level of the anolyte should be
roughly 1 - 2 mm above the level of the catholyte.
3Close the remaining ground-joint opening on the right with the
6.1437.000 ground-joint stopper (with ground-joint sleeve attached).
Filling the titration cell (generator electrode without dia-
phragm)
Proceed as follows when using a generator electrode without a dia-
phragm:
1Fill approximately 100 mL of reagent into the titration cell with the
aid of the 6.2738.000 funnel.
2Close the remaining ground-joint opening on the right with the
6.1437.000 ground-joint stopper (with ground-joint sleeve attached).

4.2 Setting up the titration cell for coulometry ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭
14 ￭￭￭￭￭￭￭￭ 899 Coulometer
4.2.3 Mounting the addition and aspiration tube (utilization with Ti
Stand)
6.1437.000
6.2713.000
6.2713.000
6.1439.010
1
2
4
5
6
3
Figure 6 Mounting the addition and aspiration tube
Insert the addition and aspiration tube as follows into the titration cell:
1Attach the 6.2713.000 ground-joint sleeve that has been cut to size
to the ground joint of the 6.1437.000 stopper.
2Insert the stopper into the 6.1439.010 addition and aspiration tube.
3Attach the 6.2713.000 ground-joint sleeve that has been cut to size
to the ground joint of the addition and aspiration tube.
4Insert this assembly into the ground-joint opening.
5Connect the tubing for the reagent addition at the upper connector
of the addition and aspiration tube (5).