899 Coulometer

Manual
8.899.8001EN / 2020-02-25
Metrohm AG
CH-9100 Herisau
Switzerland
Phone +41 71 353 85 85
Fax +41 71 353 89 01
[email protected]
www.metrohm.com

899 Coulometer

Manual

8.899.8001EN / 2020-02-25
Technical Communication
Metrohm AG
CH-9100 Herisau
[email protected]

This documentation is protected by copyright. All rights reserved.

This documentation has been prepared with great care. However, errors
can never be entirely ruled out. Please send comments regarding possible
errors to the address above.
￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of contents

Table of contents
1 Introduction 1
1.1 Instrument description ......................................................... 1
1.1.1 Connectors .............................................................................. 1
1.1.2 Intended use ........................................................................... 2
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 ........................................... 5
1.3.5 Recycling and disposal ............................................................. 5

2 Overview of the instrument 6

2.1 Front ...................................................................................... 6
2.2 Rear ........................................................................................ 7

3 Installation 8
3.1 Setting up the instrument .................................................... 8
3.1.1 Packaging ................................................................................ 8
3.1.2 Checks .................................................................................... 8
3.1.3 Location .................................................................................. 8
3.2 Setting up the titration cell for coulometry ....................... 9
3.2.1 Inserting the titration cell ......................................................... 9
3.2.2 Preparing the titration cell ........................................................ 9
3.2.3 Mounting the addition and aspiration tube (utilization with Ti
Stand) .................................................................................... 13
3.2.4 Using the titration cell with a Karl Fischer oven ...................... 14
3.2.5 Using the titration cell with a sample changer ........................ 14
3.3 Connecting the coulometer to the power supply ............ 14
3.3.1 Connecting the power supply unit ......................................... 14
3.3.2 Connecting the Power Box .................................................... 15
3.4 Connecting sensors ............................................................ 17
3.4.1 Connecting a generator electrode .......................................... 17
3.4.2 Connecting an indicator electrode ......................................... 18
3.4.3 Connecting a temperature sensor .......................................... 20
3.5 Connecting an additional stirrer ....................................... 21
3.6 Connecting a balance ......................................................... 22
3.7 Connecting a keyboard, printer and other USB devi-
ces ........................................................................................ 24

899 Coulometer ￭￭￭￭￭￭￭￭ III

 Table of contents ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

3.8 Connecting a sample changer to the remote connec-

tor ........................................................................................ 27

4 Coulometric titration 28
4.1 Principle of coulometry according to Karl Fischer ........... 28
4.2 Working with water standards ......................................... 29
4.2.1 Certified water standards ....................................................... 29
4.2.2 Practical recommendations .................................................... 29
4.3 Sample addition .................................................................. 31
4.3.1 Size of the sample size ........................................................... 31
4.3.2 Working with liquid samples .................................................. 31
4.3.3 Working with solid samples ................................................... 32
4.4 Optimum working conditions ........................................... 33
4.4.1 General ................................................................................. 33
4.4.2 Drift ...................................................................................... 33
4.4.3 Reagent replacement ............................................................. 34
4.4.4 Indicator electrode ................................................................ 34

5 Operation 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 ............................................ 36
5.2.3 Navigating in the dialog ......................................................... 37
5.2.4 Entering text and numbers ..................................................... 37
5.2.5 Selecting from a selection list ................................................. 38
5.3 Formula editor .................................................................... 39
5.4 Methods .............................................................................. 40
5.4.1 Method templates ................................................................. 40
5.4.2 Loading a method template ................................................... 40
5.4.3 Saving a method ................................................................... 41
5.4.4 Exporting a method ............................................................... 42
5.5 Control ................................................................................. 43
5.6 Sample data ........................................................................ 44
5.6.1 Entering sample data in the main dialog ................................ 44
5.6.2 Requesting sample data at the start of the determination ...... 45
5.7 Sample table ....................................................................... 45
5.7.1 General ................................................................................. 45
5.7.2 Editing the sample data ......................................................... 47
5.7.3 Sending the sample size from a balance ................................. 49
5.8 Carrying out a determination ............................................ 49
5.9 Live modifications .............................................................. 52
5.9.1 Editing the sample data of the running determination ............ 52
5.9.2 Editing the sample table while a determination is running ...... 53

IV ￭￭￭￭￭￭￭￭ 899 Coulometer

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of contents

5.9.3 Editing the live parameters ..................................................... 55

5.10 Results ................................................................................. 56
5.11 Statistics .............................................................................. 57
5.12 Printing a report manually ................................................. 59
5.13 Manual control ................................................................... 60
5.13.1 Stirring .................................................................................. 60

6 System settings 62
6.1 Basic settings ...................................................................... 62
6.2 Managing common variables ............................................ 65
6.2.1 General ................................................................................. 65
6.2.2 Editing common variables ...................................................... 65
6.3 File management ................................................................ 66
6.4 Configuring external devices ............................................. 68
6.5 Instrument diagnosis .......................................................... 71
6.5.1 Loading program versions and language files ......................... 71
6.5.2 Diagnosis functions ............................................................... 72

7 Parameters 73
7.1 Coulometric Karl Fischer titrations (KFC) .......................... 73
7.1.1 Conditioning ......................................................................... 73
7.1.2 Start conditions ..................................................................... 75
7.1.3 Control parameters ................................................................ 76
7.1.4 Titration parameters .............................................................. 79
7.1.5 Stop conditions ..................................................................... 81
7.1.6 Calculation ............................................................................ 81
7.1.7 Statistics ................................................................................ 85
7.1.8 Reports .................................................................................. 86

8 Troubleshooting 88
8.1 Karl Fischer titration ........................................................... 88
8.2 Miscellaneous ..................................................................... 90

9 Appendix 92
9.1 Stirring rate ......................................................................... 92
9.2 Balance ................................................................................ 92
9.3 USB devices ......................................................................... 93
9.3.1 6.2147.000 numerical USB keypad ........................................ 93
9.3.2 Key assignment of a USB keyboard ........................................ 94
9.3.3 PC mouse .............................................................................. 95
9.3.4 Printer ................................................................................... 95
9.4 Control parameters and polarization current .................. 95

899 Coulometer ￭￭￭￭￭￭￭￭ V

 Table of contents ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

9.5 Method examples for working with the Karl Fischer

oven ..................................................................................... 97
9.6 System initialization ........................................................... 98
9.7 Remote interface ................................................................ 99
9.7.1 Pin assignment of the remote interface .................................. 99
9.7.2 Status diagram of the remote interface ................................ 100
9.8 Remote control via an RS-232 connection ..................... 101
9.8.1 Commands and variables ..................................................... 102
9.9 Arithmetic algorithms in the 899 Coulometer ............... 103

10 Technical specifications 106

10.1 Measuring inputs .............................................................. 106
10.1.1 Indicator electrode .............................................................. 106
10.1.2 Temperature ........................................................................ 106
10.2 Generator connector ........................................................ 106
10.2.1 Generator electrode ............................................................. 106
10.3 Internal stirrer ................................................................... 107
10.4 Interfaces and connectors ............................................... 107
10.5 Power supply .................................................................... 107
10.6 Ambient temperature ....................................................... 108
10.7 Reference conditions ........................................................ 108
10.8 Dimensions ........................................................................ 108

11 Accessories 109
Index 110

VI ￭￭￭￭￭￭￭￭ 899 Coulometer

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ Table of figures

Table of figures
Figure 1 Front 899 Coulometer ....................................................................... 6
Figure 2 Rear 899 Coulometer ........................................................................ 7
Figure 3 Inserting the titration cell (coulometry) .............................................. 9
Figure 4 Filling the adsorber tube .................................................................. 10
Figure 5 Equipping the titration cell (coulometry) .......................................... 11
Figure 6 Mounting the addition and aspiration tube ...................................... 13
Figure 7 Connecting the power supply unit ................................................... 15
Figure 8 Connecting the Power Box .............................................................. 16
Figure 9 Unscrewing the cover from the generator electrode ........................ 17
Figure 10 Screwing the electrode cable to the generator electrode ................. 18
Figure 11 Connecting a generator electrode ................................................... 18
Figure 12 Unscrewing the cover from the indicator electrode .......................... 19
Figure 13 Screwing the electrode cable to the indicator electrode ................... 19
Figure 14 Connecting an indicator electrode ................................................... 19
Figure 15 Connecting a temperature sensor .................................................... 20
Figure 16 Connecting a stirrer ......................................................................... 21
Figure 17 Connecting the balance via RS-232/USB Box .................................... 22
Figure 18 Connecting USB devices .................................................................. 24
Figure 19 Connecting the USB flash drive ........................................................ 26
Figure 20 Connecting the 6.2147.000 USB keyboard with USB flash drive and
printer ............................................................................................. 26
Figure 21 Connecting the USB hub with USB flash drive, printer and 6.2148.030
RS-232/USB Box .............................................................................. 27
Figure 22 Connecting a remote cable .............................................................. 27
Figure 23 Keypad 899 Coulometer .................................................................. 36
Figure 24 Directory structure on the USB flash drive ........................................ 67
Figure 25 Rotational speed depending on the stirring rate ............................... 92
Figure 26 Control parameters and polarization current .................................... 96
Figure 27 Pin assignment of remote socket and remote plug ........................... 99
Figure 28 Remote status diagram .................................................................. 100
Figure 29 Connecting the RS-232/USB Box to the PC .................................... 101

899 Coulometer ￭￭￭￭￭￭￭￭ VII

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1 Introduction

1 Introduction

1.1 Instrument description

The 899 Coulometer is a titrator used for coulometric water content
determination according to Karl Fischer. There are method templates avail-
able which are already configured except for a few parameters. The meth-
ods can be modified and stored under a new name. The methods can be
exported to a connected USB flash drive. This function allows you to copy
methods quickly and easily from one device 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.

1.1.1 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.
￭ Remote connector
For connecting instruments with a remote interface (e.g. 885 Compact
Oven SC).

899 Coulometer ￭￭￭￭￭￭￭￭ 1

 1.2 About the documentation ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

1.1.2 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.
This instrument is suitable for processing chemicals and flammable sam-
ples. Therefore, the use of the 899 Coulometer 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.

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 the user must follow in order to ensure safe opera-
tion of the instrument.

1.2.1 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.
WARNING
This symbol draws attention to a possible hazard due
to electrical current.

2 ￭￭￭￭￭￭￭￭ 899 Coulometer

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1 Introduction

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.

1.3 Safety instructions

1.3.1 General notes on safety

WARNING

Operate this instrument only according to the information contained in

this documentation.

This instrument 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.

899 Coulometer ￭￭￭￭￭￭￭￭ 3

 1.3 Safety instructions ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

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.

Supply voltage

WARNING

An incorrect supply voltage can damage the instrument.

Only operate this instrument with a supply 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 power cord out of the power socket before you
set up or disconnect electrical plug connections at the rear 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 manda-
tory.

4 ￭￭￭￭￭￭￭￭ 899 Coulometer

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 1 Introduction

1.3.4 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.

1.3.5 Recycling and disposal

This product is covered by European Directive 2012/19/EU, WEEE – Waste
Electrical and Electronic Equipment.
The correct disposal of your old instrument will help to prevent negative
effects on the environment and public health.
More details about the disposal of your old instrument can be obtained
from your local authorities, from waste disposal companies or from your
local dealer.

899 Coulometer ￭￭￭￭￭￭￭￭ 5

 2.1 Front ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

2 Overview of the instrument

2.1 Front

Figure 1 Front 899 Coulometer

1 Magnetic stirrer 2 Display

For attaching the titration vessel holder.

3 Keypad

6 ￭￭￭￭￭￭￭￭ 899 Coulometer

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 2 Overview of the instrument

2.2 Rear

1 2 3 4 5 6 7 89
Figure 2 Rear 899 Coulometer

1 Type plate 2 Remote connector

Contains the serial number. For connecting instruments with a remote
interface. D-Sub, 9-pin.

3 Electrode connector (Ind.) 4 Temperature sensor connector (Temp.)

For connecting a metal electrode (double Pt For connecting a temperature sensor of the
wire electrode). Socket F. type Pt1000. Two B sockets, 2 mm.

5 MSB connector (MSB 1) 6 USB (OTG) connector

Metrohm Serial Bus. For connecting an For connecting printers, USB flash drives,
external stirrer. Mini DIN, 8-pin. USB hubs, etc.

7 Mains connection socket (Power) 8 Electrode connector (Gen.)

For connecting the external power supply For connecting a generator electrode.
unit or a Power Box (6.2164.500).

9 Grounding socket
For grounding the Coulometer. Socket B,
4 mm.

899 Coulometer ￭￭￭￭￭￭￭￭ 7

 3.1 Setting up the instrument ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

3 Installation

3.1 Setting up the instrument

3.1.1 Packaging
The instrument is supplied in protective packaging together with the sepa-
rately 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 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.

8 ￭￭￭￭￭￭￭￭ 899 Coulometer

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation

3.2 Setting up the titration cell for coulometry

3.2.1 Inserting the titration cell

6.1464.320

6.2047.030

Figure 3 Inserting the titration cell (coulometry)

Set up the titration cell on the magnetic stirrer as follows:

1 Attach the 6.2047.030 titration vessel holder to the magnetic stirrer.

2 Insert the 6.1464.320 titration cell into the titration vessel holder.

3.2.2 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:

899 Coulometer ￭￭￭￭￭￭￭￭ 9

 3.2 Setting up the titration cell for coulometry ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

6.1403.030

6.2811.000 2

Figure 4 Filling the adsorber tube

1 Insert a small cotton plug into the bottom of the adsorber tube. Do
not pack the cotton too tightly.

2 Fill the molecular sieve up to ¾ of the height.

3 Place a small cotton plug on the molecular sieve. Do not pack the
cotton too tightly.

4 Seal the adsorber tube with the appropriate cover.

NOTICE

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.

10 ￭￭￭￭￭￭￭￭ 899 Coulometer

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation

Equipping the titration cell

3
6.1403.030

2
6.2713.020

5
6.0341.100 4 6.0345.100
6.0344.100

6.2713.000
6.1437.000

6.2701.040 2 2
6.2713.010
6
6.1448.020

6.1464.320
1
6.1903.030

Figure 5 Equipping the titration cell (coulometry)

Equip the titration cell as follows:

1 Place the 6.1903.030 stirring bar in the titration cell.

2 Cut 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.

3 Insert the 6.1403.030 adsorber tube into the generator electrode.

899 Coulometer ￭￭￭￭￭￭￭￭ 11

 3.2 Setting up the titration cell for coulometry ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

4 Insert 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.

5 Insert the 6.0341.100 indicator electrode into the left ground-joint

opening.

6 Place 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:

1 Fill approximately 5 mL of catholyte into the generator electrode.

2 Fill 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.

3 Close 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:

1 Fill approximately 100 mL of reagent into the titration cell with the
aid of the 6.2738.000 funnel.

2 Close the remaining ground-joint opening on the right with the

6.1437.000 ground-joint stopper (with ground-joint sleeve attached).

12 ￭￭￭￭￭￭￭￭ 899 Coulometer

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation

3.2.3 Mounting the addition and aspiration tube (utilization with Ti

Stand)

6.1437.000
2

6.2713.000
1
5
6

6.1439.010

6.2713.000
3

Figure 6 Mounting the addition and aspiration tube

Insert the addition and aspiration tube as follows into the titration cell:

1 Attach the 6.2713.000 ground-joint sleeve that has been cut to size
to the ground joint of the 6.1437.000 stopper.

2 Insert the stopper into the 6.1439.010 addition and aspiration tube.

3 Attach the 6.2713.000 ground-joint sleeve that has been cut to size
to the ground joint of the addition and aspiration tube.

4 Insert this assembly into the ground-joint opening.

5 Connect the tubing for the reagent addition at the upper connector
of the addition and aspiration tube (5).

899 Coulometer ￭￭￭￭￭￭￭￭ 13

 3.3 Connecting the coulometer to the power supply ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

6 Connect the tubing for the aspiration of the titration cell at the lower
connector of the addition and aspiration tube (6).

Details regarding how to connect the addition tubing and the aspiration
tubing can be found in the manual for the 803 Ti Stand.

3.2.4 Using the titration cell with a Karl Fischer oven

When samples release their water only slowly or only at higher tempera-
tures, the oven method is used. The sample is heated in a KF oven (e.g.
860 KF Thermoprep) and the water that is released is transferred to the
titration cell with a carrier gas. You will find recommended parameter set-
tings for determinations with a Karl Fischer oven in chapter 9.5, page 97.
A detailed description of how to set up the titration cell with the KF oven
can be found in the respective manual.

3.2.5 Using the titration cell with a sample changer

If a large number of samples have to be processed, the determination of
the water content can be automated with the aid of a sample changer
with oven module (e.g. 885 Compact Oven SC). You will find recommen-
ded parameter settings for determinations with a Karl Fischer oven in
chapter 9.5, page 97.
A detailed description of how to set up the titration cell with the sample
changer can be found in the respective manual.

3.3 Connecting the coulometer to the power supply

You can supply the 899 Coulometer with electricity in two different ways:
￭ Connect the coulometer directly to the power supply with the aid of
the power supply unit provided.
￭ Connect the coulometer to the 6.2164.500 Power Box if no stable
power supply is available.

3.3.1 Connecting the power supply unit

The 899 Coulometer has an external power supply unit for a 24 V power
supply (DC). This is connected to the power socket of the coulometer.

WARNING

An incorrect supply voltage can damage the instrument.

Operate the instrument only with the supply voltage specified for it. Use
the supplied power supply unit exclusively.

14 ￭￭￭￭￭￭￭￭ 899 Coulometer

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation

Figure 7 Connecting the power supply unit

Proceed as follows:

1 Connect the plug of the external power supply unit with the power
socket (2-7) of the coulometer.

NOTICE

The plug of the power supply unit is protected against accidental

disconnection of the cable by means of a pull-out protection fea-
ture. If you wish to pull out the plug, you first need to pull back
the outer plug sleeve.

2 Connect the power supply cable with the external power supply unit
of the coulometer and with the power supply.

CAUTION

Switch off the 899 Coulometer correctly by pressing the red [STOP] key
before you interrupt the electricity supply. If this is not done, then there
is a danger of data loss.

3.3.2 Connecting the Power Box

As an alternative to the power from the power supply, it is possible to pro-
vide the 899 Coulometer with electricity through the 6.2164.500 Power
Box. This means that you can also use the instrument in environments in
which no stable power supply is available. Details regarding the Power Box
can be found in the respective manual.

899 Coulometer ￭￭￭￭￭￭￭￭ 15

 3.3 Connecting the coulometer to the power supply ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

Figure 8 Connecting the Power Box

Proceed as follows:

1 Connect the plug of the Power Box with the power socket (2-7) of
the coulometer.

NOTICE

The Power Box plug is protected against accidental disconnection

of the cable by means of a pull-out protection feature. If you wish
to pull out the plug, you first need to pull back the outer plug
sleeve.

CAUTION

Switch off the 899 Coulometer correctly by pressing the red [STOP] key
before you interrupt the connection with the Power Box. If this is not
done, then there is a danger of data loss.

16 ￭￭￭￭￭￭￭￭ 899 Coulometer

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation

3.4 Connecting sensors

The measuring interface contains the following measuring inputs:
￭ Gen. for a generator electrode
￭ Ind. for a double Pt electrode
￭ Temp. for a temperature sensor of the Pt1000 type

CAUTION

Under all circumstances, avoid mixing up the electrode cable from the
indicator electrode with the one from the generator electrode. Mark
the screw heads of the cables accordingly.

3.4.1 Connecting a generator electrode

Screwing the electrode cable to the generator electrode

1 Unscrew the cover of the generator electrode.

Figure 9 Unscrewing the cover from the generator electrode

2 Tighten the 6.2104.120 electrode cable to the generator electrode.

899 Coulometer ￭￭￭￭￭￭￭￭ 17

 3.4 Connecting sensors ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

6.2104.120
2

Figure 10 Screwing the electrode cable to the generator electrode

Connecting the electrode cable to the coulometer

1 Plug the electrode plug into the Gen. socket of the coulometer.

Figure 11 Connecting a generator electrode

NOTICE

The electrode cable is protected against accidental disconnection

of the cable by means of a pull-out protection. If you wish to pull
out the plug again, you first need to pull back the outer plug
sleeve.

3.4.2 Connecting an indicator electrode

Screwing the electrode cable to the indicator electrode

1 Unscrew the cover of the indicator electrode.

18 ￭￭￭￭￭￭￭￭ 899 Coulometer

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation

Figure 12 Unscrewing the cover from the indicator electrode

2 Tighten the 6.2104.020 electrode cable to the indicator electrode.

6.2104.020

Figure 13 Screwing the electrode cable to the indicator electrode

Connecting the electrode cable to the coulometer

1 Plug the electrode plug into the Ind. socket of the coulometer.

Figure 14 Connecting an indicator electrode

899 Coulometer ￭￭￭￭￭￭￭￭ 19

 3.4 Connecting sensors ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

NOTICE

The electrode cable is protected against accidental disconnection

of the cable by means of a pull-out protection. If you wish to pull
out the plug again, you first need to pull back the outer plug
sleeve.

3.4.3 Connecting a temperature sensor

A temperature sensor of the Pt1000 type can be connected to the Temp.
connector.
Connect the temperature sensor as follows:

1 Insert the plugs of the temperature sensor into the Temp. sockets of
the coulometer.

Figure 15 Connecting a temperature sensor

NOTICE

Always insert the red plug into the red socket. This is the only way
that shielding against electrical interference can be ensured.

20 ￭￭￭￭￭￭￭￭ 899 Coulometer

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation

3.5 Connecting an additional stirrer

Instead of the built-in magnetic stirrer, you can use the magnetic stirrers
801 Stirrer or 803 Ti Stand.
Proceed as follows:

1 Switch off the coulometer.

2 Connect the connection cable of the magnetic stirrer to MSB 1 on

the rear of the coulometer.

Figure 16 Connecting a stirrer

NOTICE

Make sure that the flat side of the plug matches the marking on
the socket.

3 Switch on the coulometer.

899 Coulometer ￭￭￭￭￭￭￭￭ 21

 3.6 Connecting a balance ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

3.6 Connecting a balance

As a rule, balances are equipped with a serial RS-232 interface. To connect
a balance, you require a 6.2148.030 RS-232/USB Box.

Figure 17 Connecting the balance via RS-232/USB Box

Proceed as follows:

1 Connect the RS-232/USB Box with a 6.2151.020 connecting cable

(USB A - USB B) on the USB (OTG) connector of the coulometer.
You can connect the RS-232/USB Box to the coulometer either via a
USB hub or using a 6.2151.100 USB MINI (OTG) - USB A adapter (see
chapter 3.7, page 24).

2 Connect the 9-pin plug of the respective balance connecting cable to

the RS-232/1 connector. Consult the following list or contact the
balance manufacturer in order to find the correct balance connecting
cable.

NOTICE

The parameters for the RS-232 interfaces on the 899 Coulometer must
match those on the balance (see "Editing the COM1 settings", page
69). Also check the manual for the balance.

The following table offers an overview of the balances that you can use
together with the 899 Coulometer and of which cable you will need for
connection to the RS-232 interface:

22 ￭￭￭￭￭￭￭￭ 899 Coulometer

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation

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
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

899 Coulometer ￭￭￭￭￭￭￭￭ 23

 3.7 Connecting a keyboard, printer and other USB devices ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

3.7 Connecting a keyboard, printer and other USB devi-

ces
The 899 Coulometer has a USB (OTG) connector. Use the 6.2151.100
USB MINI (OTG) - USB A adapter supplied for connecting USB devices.

6.2151.100

Figure 18 Connecting USB devices

CAUTION

Switch the instrument off before connecting or disconnecting a USB

device or a USB flash drive.
The 899 Coulometer can recognize the USB device only immediately
after switching on.

NOTICE

Many USB devices need a so-called USB hub in order to work correctly.
A USB hub is a distributor to which several USB devices can be con-
nected. USB hubs are available in specialty stores in a number of differ-
ent models.
The 6.2147.000 numerical USB keypad can, in addition to its function
as keyboard, also be used as a USB hub. It has two USB connectors.
You cannot however use these two USB connectors to connect any PC
keyboards, barcode readers or additional keypads with numerical key-
pads. These devices are recognized as input devices (like the numerical
USB keypad) and they cannot be switched in series.

24 ￭￭￭￭￭￭￭￭ 899 Coulometer

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation

The following list provides you with an overview of the various USB devi-
ces and how you can connect them to the Coulometer.

USB device Connection options

USB flash drives (for the backup or ￭ With 6.2151.100 adapter USB
storing of methods) MINI (OTG) - USB A
￭ With USB hub
￭ With 6.2147.000 numerical
USB keypad
6.2147.000 numerical USB key- ￭ With 6.2151.100 adapter USB
pad (for comfortable numerical MINI (OTG) - USB A
input and for navigating in the ￭ With USB hub
dialog)
6.2148.030 RS-232/USB Box (for ￭ With 6.2151.100 adapter USB
connecting a balance, a PC or to MINI (OTG) - USB A
the RS-232 remote control) ￭ With USB hub
￭ With 6.2147.000 numerical
USB keypad
USB hub (with or without an own ￭ With 6.2151.100 adapter USB
power supply) MINI (OTG) - USB A
"Custom Neo's" printer with ￭ Directly on the USB (OTG) con-
6.2151.120 cable nector of the 899 Coulometer
"Custom Neo's" printer with ￭ With 6.2151.100 adapter USB
6.2151.020 cable MINI (OTG) - USB A
￭ With USB hub
￭ With 6.2147.000 numerical
USB keypad
USB printer with 6.2151.020 con- Depending on the model of the
necting cable printer:
￭ With 6.2151.100 adapter USB
MINI (OTG) - USB A
or
￭ With USB hub
￭ With 6.2147.000 numerical
USB keypad
PC mouse with USB cable (for ￭ With USB hub
navigating in the dialog) ￭ With 6.2147.000 numerical
USB keypad

899 Coulometer ￭￭￭￭￭￭￭￭ 25

 3.7 Connecting a keyboard, printer and other USB devices ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

USB device Connection options

PC keyboard with USB cable (for ￭ With USB hub
the comfortable input of letters
and numbers)
Barcode reader with USB cable ￭ With USB hub
Keypad with numerical keypad ￭ With USB hub
with USB cable

If you wish to connect several different instruments that do not

have their own power supply, then it is possible you will need to use a
USB hub that does have its own power supply (self powered). The USB
(OTG) connector of the 899 Coulometer is not designed for supplying
power to several devices with elevated electricity requirements.
Also observe the instructions in chapter 9.3, page 93.

Examples:

USB MINI (OTG)-USB

USB stick
6.2151.100

Figure 19 Connecting the USB flash drive

USB stick

USB MINI (OTG)-USB

Printer
6.2151.100 Keypad
6.2147.000

Figure 20 Connecting the 6.2147.000 USB keyboard with USB flash

drive and printer

26 ￭￭￭￭￭￭￭￭ 899 Coulometer

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 3 Installation

USB MINI (OTG)-USB RS-232/USB Box

USB-Hub
6.2151.100
6.2148.030

USB stick
Printer

Figure 21 Connecting the USB hub with USB flash drive, printer and
6.2148.030 RS-232/USB Box

3.8 Connecting a sample changer to the remote connec-

tor
The 899 Coulometer can be connected to a sample changer with oven
module with the aid of the 6.2141.390 remote cable. This makes it possi-
ble to integrate the Coulometer in an automation system.

Figure 22 Connecting a remote cable

Details regarding the use of the sample changer (e.g. 885 Compact Oven
SC) can be found in the respective manual.

899 Coulometer ￭￭￭￭￭￭￭￭ 27

 4.1 Principle of coulometry according to Karl Fischer ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

4 Coulometric titration

4.1 Principle of coulometry according to Karl Fischer

The coulometric Karl Fischer titration is a variation of the classic water
content determination method according to Karl Fischer. The conventional
method works with a methanolic solution of iodine, sulfur dioxide and a
base as buffer substance. If an aqueous sample is titrated, then several
reactions take place that can be summarized in the following sum equa-
tion:

H2O + I2 + [RNH]SO3CH3 + 2 RN ⇄ [RNH]SO4CH3 + 2 [RNH]I

According to the equation above the I2 reacts quantitatively with H2O. This
chemical equation serves as a basis for the water content determination.
With the coulometric Karl Fischer titration, the necessary iodine is
directly and electrochemically generated in the electrolyte containing
iodine ("electronic buret"). Between the amount of electric charge and the
amount of generated iodine, there is a strictly quantitative relationship,
which is used for high-precision dosing of the iodine. Because the coulo-
metric Karl Fischer method is an absolute determination, no titer needs
to be determined. It must only be ensured that the reaction generating
the iodine runs with a 100% current efficiency. All of the reagents avail-
able today ensure this.
The endpoint indication is effected voltametrically by modulating an alter-
nating current of constant strength to a double Pt electrode. This results in
a voltage differential between the Pt wires. This is drastically reduced as
soon as even the slightest amounts of free iodine are present. This circum-
stance is used for detecting the endpoint of the titration.

28 ￭￭￭￭￭￭￭￭ 899 Coulometer

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Coulometric titration

4.2 Working with water standards

4.2.1 Certified water standards
Commercially available, certified water standards with water content of
1.00 ± 0.003 mg/g and/or 0.10 ± 0.005 mg/g should be used for validat-
ing the instrument as a whole, integrated system.

NOTICE

The 1.0 mg/g water standard is easier to handle and is therefore prefer-
red.

Table 1 Recommended weighing ranges

1.0 mg/g water standard 0.2 - 2.0 g
0.1 mg/g water standard 0.5 - 5.0 g

4.2.2 Practical recommendations

For validation, it is essential to work very accurately. In order to minimize
any measurement inaccuracies that could occur, the sample preparation
and the sample processing should proceed in accordance with a defined
scheme:

1 Put on gloves (always for Karl Fischer titration).

2 Use a clean syringe.

NOTICE

If you are working with the 0.1 mg/g water standard, then you
must use a glass syringe. If you are working with the 1.0 mg/g
water standard, then you may use either a plastic syringe or a glass
syringe.

3 Take a new ampoule of water standard and shake it briefly.

4 With a folded paper towel held between thumb and index finger,
break open the ampoule at the marking.

5 Draw approx. 1 mL of the water standard into the syringe.

899 Coulometer ￭￭￭￭￭￭￭￭ 29

 4.2 Working with water standards ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

6 Pull the plunger of the syringe up to the end and shake the syringe
back and forth somewhat.
The inside of the syringe is rinsed by water standard and freed of
water contamination.

7 Dispose of the used water standard in a waste bottle.

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.

11 Place the syringe on the balance and press [TARA].

12 As soon as the drift on the 899 Coulometer is stable, take the syringe
in your 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 cell.
￭ 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 on the Coul-
ometer as the sample size.
If you have connected a balance to the Coulometer, you may trans-
mit the sample size directly from the balance.

30 ￭￭￭￭￭￭￭￭ 899 Coulometer

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Coulometric titration

15 The next determination can be started as soon as the determination

has been finished and the titration cell has been conditioned (drift
stable) again.

4.3 Sample addition

This chapter contains a few notes concerning sample addition. An exhaus-
tive discussion of this topic is not possible here. Further notes can be
found in the literature from the reagent manufacturers and in the follow-
ing Metrohm Application Bulletins:
Bulletin No. Title

No. 142 Karl Fischer water content determination in non-explosive gases

No. 145 Determination of low water contents in plastics using the KF oven method

No. 209 Coulometric water content determinations according to the the Karl
Fischer method in insulating oils, hydrocarbons and their products

4.3.1 Size of the sample size

The sample weight should be small in order to be able to titrate as many
samples as possible in the same electrolyte solution and to keep the titra-
tion time short. However, ensure that the sample contains at least 50 µg
of H2O. The following table helps you determine the appropriate sample
size.

Table 2 Recommended sample sizes

Water content of the sam- Sample size Resulting water content
ple
10,000 ppm = 1% 10 mg - 100 mg 100 µg - 1,000 µg
1,000 ppm = 0.1% 100 mg - 1 g 100 µg - 1,000 µg
100 ppm = 0.01% 1g 100 µg
10 ppm = 0.001% 5g 50 µg

4.3.2 Working with liquid samples

Liquid samples are added with a syringe. The samples can be injected
two different ways:
￭ One uses a syringe with a long needle, which one immerses in the
reagent during the injection.
￭ One uses a syringe with a short needle and aspirates the last drops
back into the needle.

899 Coulometer ￭￭￭￭￭￭￭￭ 31

 4.3 Sample addition ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

The best way for you to determine the injected sample amount is to
reweigh the sample.
Glass syringes should be used for the determination of traces and val-
idations. We recommend obtaining these from a specialized syringe
manufacturer.
Highly volatile samples and samples of low viscosity should be
cooled before sampling. Doing so avoids losses while working. The syringe
must, however, not be cooled directly, as condensation could be formed.
For the same reason, no air may be aspirated into a syringe into which a
cooled sample has been aspirated beforehand.
Samples of high viscosity can be thinned by heating. The syringe must
be heated as well. The same target can be reached by diluting with suit-
able solvents. In this case the water content of the solvent has to be
determined and subtracted as a blank value.
Pastes and fats can be added to the titration cell with a syringe without
needle. You can use the ground-joint opening for this. If you also wish to
aspirate, you can use the opening with the septum stopper. The best way
for you to determine the sample amount is to reweigh the sample.
If samples contain only traces of water, then the syringe has to be pre-
dried well. If possible, the syringe should be rinsed with the sample solu-
tion by filling in and discarding solution several times.

4.3.3 Working with solid samples

If possible, solid samples are to be extracted or dissolved in a suitable sol-
vent. The resulting solution is injected, during which a blank value correc-
tion for the solvent must be carried out.
If no suitable solvent can be found for a solid sample, or if the sample
reacts with the Karl Fischer reagent, then a Karl Fischer oven should be
used.
If solid samples are added directly into the titration cell, then the genera-
tor electrode without diaphragm should be used. The samples can be
added through the ground-joint opening or through the side opening.
While doing so, take care to ensure that
￭ the sample releases its moisture completely.
￭ no side reaction with the Karl Fischer reagent takes place.
￭ the surfaces of the electrodes are not covered by the sample substance
(incomplete KF reaction).
￭ the Pt grid of the generator electrode does not become damaged.
￭ the Pt wires of the indicator electrode do not become damaged.

32 ￭￭￭￭￭￭￭￭ 899 Coulometer

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 4 Coulometric titration

4.4 Optimum working conditions

4.4.1 General
When a titration cell that has been well dried-out beforehand is put into
operation with a generator electrode without diaphragm, the basic drift
will be reached within approx. 30 minutes. It is recommended that the
titration cell be repeatedly and carefully shaken during this time.
For generator electrodes with diaphragms, you should expect a prepara-
tion time of approx. 2 hours.
To obtain precise determinations of amounts of water less than 100 µg, it
may also be of advantage to condition the titration cell overnight before
using it.
If the Coulometer is switched off for extended periods with the titration
cell filled, it will take some time for it to become conditioned again after it
is switched back on.
With continuous use, the Coulometer should not be switched off over-
night.

4.4.2 Drift
A constant drift in the range of ≤ 4 µg/min is all right. Lower values are,
however, quite possible. Higher but stable values will still produce good
results because it is possible to compensate for the drift.
A constantly high drift can be caused by water-containing deposits in
inaccessible parts of the titration cell. In these cases, shaking the cell can
reduce the value. Ensure that there are no drops above the liquid level in
the titration cell.
If you are working with a generator electrode with diaphragm, do not
shake the cell so hard that the catholyte and anolyte mix with one
another. If the drift remains too high for a prolonged time, even after
shaking the cell, then the electrolyte solutions should be replaced. The
catholyte should be replaced once per week.
A wet catholyte can be another reason for the excessively high drift. The
wet catholyte can be dried with a KF one-component reagent.
When you work with a Karl Fischer oven, a drift ≤ of 10 µg/min is all right.
The drift depends on the gas flow (the smaller the gas flow, the lower the
drift) and on the humidity of the surroundings.

899 Coulometer ￭￭￭￭￭￭￭￭ 33

 4.4 Optimum working conditions ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

4.4.3 Reagent replacement

The electrolyte solutions must be replaced in the following cases:
￭ The titration cell is too full.
￭ The KF reagent has reached its capacity limit.
￭ The drift is too high, and cannot be reduced by shaking the titration
cell.
￭ A two-phase-mixture is being formed in the titration cell; in this case it
is also only possible to aspirate the sample phase.
Exhausted electrolyte solution is best disposed of by aspiration. To do this,
you can use, for example, an 803 Ti Stand with built-in membrane pump.
An advantage is that the titration cell does not have to be disassembled.
In the event of severe contamination, the titration cell can be rinsed with a
suitable solvent which is also aspirated.
In the case of a generator electrode with diaphragm, the catholyte should
be replaced once per week. Longer use can cause blackening and yellow
precipitates in the cathode chamber. An unpleasant smell is also a sign of
having used the catholyte for too long.

4.4.4 Indicator electrode

A new indicator electrode can take a certain warm-up time to form the
surface. During this time, unexpectedly long titration times and excessively
high measurement results can occur. These phenomena will, however, dis-
appear after a short time of use. In order to accelerate the setting of a
new indicator electrode, the 899 Coulometer can be conditioned (e.g.
over night).
A contaminated indicator electrode can be carefully cleaned with an abra-
sive agent (6.2802.000 polishing set or toothpaste). After the cleaning,
rinse with ethanol.
The two Pt wires of the indicator electrode should run as parallel as possi-
ble to one another. Check the Pt wires before inserting the electrode.

34 ￭￭￭￭￭￭￭￭ 899 Coulometer

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Operation

5 Operation

5.1 Switching the instrument on and off

Switching on the instrument

Proceed as follows:

1 ￭ Press the red [STOP] key.

The instrument is initialized and a system test performed. This pro-
cess takes some time.
The main dialog is displayed:

Switching off the instrument

The instrument is switched off with the [STOP] key. The fact that the key
needs to be pressed down for an extended time prevents accidental
switch off.
Proceed as follows:

1 ￭ Keep the red [STOP] key pressed down for at least 3 s.

A progress bar is displayed. If the key is released during this time,
then the instrument will not be switched off.

899 Coulometer ￭￭￭￭￭￭￭￭ 35

 5.2 Fundamentals of operation ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

5.2 Fundamentals of operation

5.2.1 The keypad

Figure 23 Keypad 899 Coulometer

BACK Apply the input and exit the dialog.
⇧⇩ Move the selection bar either up or down by one
line at a time. Select the character to be entered
in the text editor.
⇦⇨ Select the character to be entered in the text and
number editor. Select the individual functions in
the function bar.
OK Confirm the selection.
STOP Stop an ongoing method run or a manual func-
tion. Switch the instrument on or off.
START Start a method run or a manual function.

5.2.2 Structure of the dialog windows

The current dialog title is displayed on the left-hand side of the title bar.
The current status of the system is displayed in the upper right-hand cor-
ner:
ready The instrument is in normal status.
cond.busy The working medium is being conditioned.
cond.ok The working medium is conditioned.
busy A method has been started.
hold A method has been paused.

36 ￭￭￭￭￭￭￭￭ 899 Coulometer

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Operation

Some dialogs have a so-called function bar on the bottom line. The func-
tions contained therein can be selected with the arrow keys [⇦] or [⇨] and
executed with [OK].

5.2.3 Navigating in the dialog

The selection bar is displayed in inverted style. Use the arrow keys [⇧] and
[⇩] to move the selection bar upward or downward one line at a time. If a
dialog text is marked with "＞", then additional settings are available in a
subordinate dialog. Use [OK] to access this dialog.
Example: System settings

Use the [BACK] key to return to the next higher level.

5.2.4 Entering text and numbers

In the editing dialog for text input or numerical input, select the individual
characters with the arrow keys. Use [OK] to apply the character in the
input field. The following functions are available:

Editing function Description

Accept The modification is applied and the editing dialog
is exited.
Cancel The editing dialog is exited without applying the
modification.

899 Coulometer ￭￭￭￭￭￭￭￭ 37

 5.2 Fundamentals of operation ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

Editing function Description

Clear The content of the input field is deleted com-
pletely.
The character left of the cursor is deleted (back-
space).
Text editor only
The cursor within the input field is shifted to the
left by one character each time that [OK] is
pressed.
Text editor only
The cursor within the input field is shifted to the
right by one character each time that [OK] is
pressed.
[BACK] The modification is applied and the editing dialog
is exited.

The [BACK] key has the same function as Accept.

A commercially available USB keyboard can be connected to make it eas-
ier to enter text and numbers. The assignment of the keys on the PC key-
board is described in chapter 9.3.2, page 94.

5.2.5 Selecting from a selection list

In a selection list, select the individual entries with the arrow keys [⇧] and
[⇩]. Accept the selection with [OK] or [BACK].

38 ￭￭￭￭￭￭￭￭ 899 Coulometer

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Operation

5.3 Formula editor

The formulas for the calculations are entered with the formula editor. The
formula editor is equipped with an automatic syntax check. This is trig-
gered as soon as a formula is applied. The generally valid rules of priority
apply for the calculation operations.

Variable Description
C00 Sample size
EP# Water quantity at the endpoint EP# (# = 1…9)
CI# Sample identification (# = 1…2)
R# Result (# = 1…5)
CV0# Common variable (# = 1…5)
SMN# Mean value of result R# (# = 1…5)
Var List of additional variables (see "Variables", page 39)

"#" stands for a sequential number that you must enter manually. Exam-
ple: if you apply the variable EP# in the formula, only EP is entered. You
will still need to enter the number yourself.
The meanings of the editing functions are explained in chapter 5.2.4,
page 37.

Variables
Pressing Var displays a list with additional variables. You can enter these
variables either directly into the formula or also by selecting them from the
list and applying them with [OK].

Variable Description
MCQ End quantity, i.e. total amount of removed water at the
end of the titration (in µg)
MCD Duration of the entire titration
MDC Drift for drift correction

899 Coulometer ￭￭￭￭￭￭￭￭ 39

 5.4 Methods ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

Variable Description
DDC Time for drift correction
MIM Initial measured value, i.e. measured value prior to the
processing of the start conditions
MIT Initial temperature, i.e. temperature prior to the process-
ing of the start conditions
MCM End measured value
MCT End temperature
DD Duration of the entire determination

5.4 Methods
5.4.1 Method templates
The 899 Coulometer contains method templates which are already config-
ured except for a few parameters.
The following method templates can be selected:
KFC Coulometric Karl Fischer titration.
The blank value is not taken into account for the
calculation.
KFC-Blank Coulometric Karl Fischer titration minus the blank
value.
Blank Coulometric blank value determination.
The method templates differ only in their calculation formulas.

5.4.2 Loading a method template

Proceed as follows to load a method template:

1 Opening method templates

￭ In the main dialog, select Method and press [OK].
The method table with the stored methods opens:

2 In the function bar, select New and press [OK].

The list with method templates opens:

40 ￭￭￭￭￭￭￭￭ 899 Coulometer

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Operation

3 Loading the method template

￭ Select the desired method template and press [OK].
The method is now loaded and is displayed in the main dialog under
Method.

5.4.3 Saving a method

If you modify method parameters, then you can save these as your own
method. A maximum of 100 methods can be saved.
To save a method, proceed as follows:

1 Opening the method table

￭ In the main dialog, select Method and press [OK].
The method table opens:

2 Modifying/applying the method name

￭ In the function bar, select Store and press [OK].
The name of the method template is suggested as the method
name (e.g. KFC-Blank). If the method has already been saved
once, then the method name already used will be displayed:

Applying the name:

899 Coulometer ￭￭￭￭￭￭￭￭ 41

 5.4 Methods ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

￭ Press [BACK].
The method will be saved and the method table is displayed.
Entering a new name:
￭ Press [OK].
The text editor opens.
￭ Enter a method name (max. 12 characters) and apply with
Accept or [BACK].
￭ Press [BACK].
The method will be saved and the method table is displayed.

5.4.4 Exporting a method

The methods can be exported to a connected USB flash drive.

NOTICE

This function is possible only if a USB flash drive is connected as an

external storage medium.

To export a method, proceed as follows:

1 Opening the method table

￭ In the main dialog, select Method and press [OK].
The method table with the stored methods opens:

2 Selecting the method

￭ Select the desired method.

3 Exporting the method

￭ In the function bar, select Export and press [OK].
The method is being exported. The directory structure on the USB
flash drive is listed in chapter 6.3, page 66.

42 ￭￭￭￭￭￭￭￭ 899 Coulometer

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Operation

5.5 Control
Menu ▶ Control
In the dialog Control, the settings for the execution of a single determi-
nation or of one sample series are defined.

Sample table
If this parameter is activated, the sample data for a sample series can be
entered in a table (see chapter 5.7, page 45).
Selection on | off
Default value off

Autostart
If this parameter is activated, a new determination is started automatically
at the end of a determination. This continues until the number specified
has been reached (see Number of autostarts).
Selection on | off
Default value off

NOTICE

If you are working with a sample changer with oven module (e.g. 885
Compact Oven SC), then the Autostart parameter must be set to off,
because the sample changer starts the titration.

Number of autostarts
This parameter is visible only when Autostart = on.
Number of automatic starts.
Input range 1 - 50
Selection table
Default value table
table
The number of automatic starts corresponds to the number of samples
in the sample table.

899 Coulometer ￭￭￭￭￭￭￭￭ 43

 5.6 Sample data ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

5.6 Sample data

You can enter the sample data (identification, sample size, etc.) in a variety
of ways:
￭ Directly in the main dialog.
￭ Using the sample table. This is particularly useful with sample series.
The sample table is a table in which the sample data for up to 99 sam-
ples can be entered (see chapter 5.7, page 45).
￭ Automatic request immediately after the start of the determination (see
chapter 5.6.2, page 45).
You can also send the sample size and the unit from a connected balance
in any case. With some balances, the sample identification and method
can be also sent (see chapter 9.2, page 92).

5.6.1 Entering sample data in the main dialog

For a sample, you can enter the sample data directly in the main dialog,
even while the determination is running (see chapter 5.9, page 52).

ID1
Sample identification. The sample identification can be used in calculations
as the variable CI1.
Entry max. 10 characters
Default value empty

ID2
Sample identification. The sample identification can be used in calculations
as the variable CI2.
Entry max. 10 characters
Default value empty

Sample size
Sample size. The value of the sample size can be used in calculations as
the variable C00.
Input range –999999999 - 9999999999
Default value 1.0

44 ￭￭￭￭￭￭￭￭ 899 Coulometer

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Operation

Unit
Unit of the sample size.
Selection g | mg | µg | mL | µL | pieces | User-defined
Default value g
User-defined
A user-defined unit can be created. This will be added to the selection
list. The previous entry will be overwritten as soon as the new unit has
been defined.

5.6.2 Requesting sample data at the start of the determination

The sample data can be requested immediately after the start of the deter-
mination in order to ensure that the sample data entry is not forgotten.
This automatic request is indispensable when you reweigh your samples.

The corresponding parameters must be activated under Start conditions

for this purpose. If the parameter Hold at request is activated, then the
run will be paused and must be continued with [START] after the input of
the sample data. If Hold at request is deactivated, then the titration will
be started in the background. This dialog will be displayed until the enter-
ing of the sample data is confirmed with [START], even if the the titration
is already completed. This ensures that the sample data is available for cal-
culations.

5.7 Sample table

5.7.1 General
The sample table is a table in which the sample data for up to 99 samples
can be entered. The sample data can also be entered while a determina-
tion is running (see chapter 5.9.2, page 53).

899 Coulometer ￭￭￭￭￭￭￭￭ 45

 5.7 Sample table ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

Activating the sample table

Proceed as follows to activate the sample table (parameter Sample table

= on).

1 Opening the main menu

￭ In the main dialog, select Menu and press [OK].

2 Opening the control dialog

￭ Select the menu item Control and press [OK].

3 Activating the sample table

￭ Select Sample table and press [OK].
￭ Select the entry on in the selection list and apply with [OK].
￭ Press [BACK].
The menu item Sample table is displayed in the main menu:

The sample table contains numbered lines. The identification (ID1) and
the sample size of each sample are displayed.

46 ￭￭￭￭￭￭￭￭ 899 Coulometer

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Operation

Edit
Edit the data of the selected line, see following chapter.
Delete
Delete the selected line from the sample table.
Insert
Insert a new line above the line selected.
New
Delete the sample table completely. This function is visible only if the
instrument is in ready status.
Store
Save the sample table. The sample table is saved in the internal device
memory.

NOTICE

You can save only one sample table. When you save a sample table,
any previously saved sample table will be overwritten automatically.

Load
Load the sample table from the internal device memory.

5.7.2 Editing the sample data

You will see at the very bottom the line number of the selected line and
the line number of the last line containing data. In this example, the first
line is opened and the sample table contains four lines.
One can scroll between the individual data sets with the keys [⇦] and [⇨].

899 Coulometer ￭￭￭￭￭￭￭￭ 47

 5.7 Sample table ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

Inserting a new line

If you find yourself on the last line (i.e. Line 4 of 4 in the above example),
you can add a new line to the sample table by pressing [⇨] again. The
sample data of the previous sample will be applied thereby.

Method
Method used for processing the sample.
Selection Selection of stored methods | empty
Default value empty
empty
The currently loaded method is used.

ID1
Sample identification. The sample identification can be used in calculations
as the variable CI1.
Entry max. 10 characters
Default value empty

ID2
Sample identification. The sample identification can be used in calculations
as the variable CI2.
Entry max. 10 characters
Default value empty

Sample size
Sample size. The value of the sample size can be used in calculations as
the variable C00.
Input range –999999999 - 9999999999
Default value 1.0

Unit
Unit of the sample size.
Selection g | mg | µg | mL | µL | pieces | User-defined
Default value g
User-defined
A user-defined unit can be created. This will be added to the selection
list. The previous entry will be overwritten as soon as the new unit has
been defined.

48 ￭￭￭￭￭￭￭￭ 899 Coulometer

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Operation

5.7.3 Sending the sample size from a balance

If the sample size is sent directly from the balance, then it will always be
entered in a new line at the end of the sample table. It does not matter
which line is selected or whether the sample table is even opened. In the
above example, the sample size is entered in line 5.

NOTICE

If you would like to enter the sample size in a particular line, then you
must open the corresponding editing dialog (i.e. the Sample data dia-
log is displayed).
If the editing dialog for the sample size is opened, then the sent value
will be ignored.

5.8 Carrying out a determination

The sample size can be entered in the following ways when a determina-
tion is carried out:
￭ Enter manually on the instrument.
￭ Send automatically from a connected balance. For this purpose, check
the manual for the balance.
Proceed as follows to carry out a determination:

1 Loading the method

￭ See Chapter "Methods", Page 40.

2 Starting conditioning
￭ Press [START].
Conditioning starts. Conditioning not OK is displayed until the
endpoint is reached. The working medium is titrated to the endpoint.
This is indicated by Conditioning OK. The status is kept stable.

899 Coulometer ￭￭￭￭￭￭￭￭ 49

 5.8 Carrying out a determination ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

The stirring rate can be modified with the Stirrer function. The fol-
lowing dialog is opened by pressing [OK]:

The stirring rate can be reduced with Stir- and increased with Stir+.
Off switches the stirrer off. On is now displayed instead. This can be
used to switch the stirrer back on. This dialog is exited with [BACK].

3 Adding sample
￭ If Conditioning OK is displayed, press [START].
Conditioning is stopped. The request for adding the sample will
be displayed for 8 s.
The sample must be added during this time.

￭ Add the sample.

Afterward, the request for the sample size appears:

50 ￭￭￭￭￭￭￭￭ 899 Coulometer

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Operation

4 Entering the sample size

￭ Press [OK].
The editing dialog opens.
￭ Enter the sample size and apply with Accept or [BACK].

5 Starting the titration

￭ Press [START].
The titration starts and the curve is displayed:

The axes are scaled automatically.

The stirring rate can be modified during titration with the Stirrer
function. The following dialog is opened by pressing [OK]:

The stirring rate can be reduced with Stir- and increased with Stir+.
Off switches the stirrer off. On is now displayed instead. This can be
used to switch the stirrer back on. This dialog is exited with [BACK].
After the completion of the titration, the results dialog is displayed:

Conditioning is restarted automatically in the background. You can

see the current status of the conditioning in the status display at the
upper right in the dialog window (cond.busy or cond.ok).

899 Coulometer ￭￭￭￭￭￭￭￭ 51

 5.9 Live modifications ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

6 Returning to the conditioning dialog

￭ Press [BACK].
The main dialog with the sample data of the previously ended
titration is displayed.
￭ Select Menu and press [OK].
￭ Select the menu item Live dialog and press [OK].

The current status of the conditioning is displayed (see instruction

step 2).
If you wish to start the next titration, repeat the actions starting with
instruction step 3.

Canceling a determination manually

A determination can be canceled at any time with the [STOP] key.

5.9 Live modifications

5.9.1 Editing the sample data of the running determination
The sample data can be entered or modified in the main dialog while a
determination is running. In calculations always the sample data entered
at the end of the titration in the main dialog is used.
Proceed as follows to edit the sample data:

1 Displaying the main dialog

￭ Press [BACK].
The main dialog is displayed. The determination continues to run in
the background.

2 Editing the sample data

￭ Edit the sample data and apply with Accept or [BACK].

3 Displaying the live dialog

￭ Press [BACK].
or

52 ￭￭￭￭￭￭￭￭ 899 Coulometer

￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Operation

￭ Select Menu and press [OK].

￭ Select the menu item Live dialog and press [OK].

The live dialog is displayed once again.

NOTICE

If the determination is finished while an editing dialog is opened (e.g. of

the sample size), then this will be closed automatically and the results
dialog will be displayed. The value entered must be entered once more
and the determination must be recalculated.
Make sure that the editing dialogs are closed before the determination
is finished.

5.9.2 Editing the sample table while a determination is running

You can insert new lines or delete existing ones or edit sample data while
a determination is running.

NOTICE

We recommend that the editing dialogs always be closed in order to

ensure that no problems occur during the run and that the current data
is always available for calculation purposes.

Editing the sample table

Proceed as follows to edit the sample table:

1 Displaying the main dialog

￭ Press [BACK].
The main dialog is displayed. The determination continues to run in
the background.

2 Opening the main menu

￭ Select Menu and press [OK].

899 Coulometer ￭￭￭￭￭￭￭￭ 53

 5.9 Live modifications ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

3 Selecting the sample data

￭ Select the menu item Sample table and press [OK].
￭ Select the desired line.
￭ In the function bar, select Edit and press [OK].

4 Editing the sample data

￭ Edit the sample data and apply with Accept or [BACK].

NOTICE

In addition to the sample data, the method can also be modified,

except in cases where the determination is running.

5 Displaying the live dialog

￭ Select the menu item Live dialog in the main menu and press
[OK].
or
￭ Press [BACK] in the main dialog.
The live dialog is displayed once again.

Editing the sample data of the running determination

When you use the sample table, the editing of the sample data of the run-
ning determination proceeds as described in chapter 5.9.1, page 52. In
addition, you have the option of editing these in the sample table. The
first line always contains the sample data of the running determination.
Simply select for this purpose the Sample table(see "Editing the sample
table", page 53) menu item in the main menu.

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￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭ 5 Operation

5.9.3 Editing the live parameters

Certain method parameters can be edited while a determination is being
carried out. The only parameters that can be modified are those that can
be selected. Nevertheless, all of the parameters are visible. The modified
parameters are taken into account at once. If, for example, you increase
the parameter Extraction time while the extraction time is still running,
then the new value will be taken into account at once. If however you
change this parameter after the extraction time has already expired, then
the changed value will not be taken into account until the next determina-
tion.
Proceed as follows to edit the parameters:

1 Displaying the main dialog

￭ Press [BACK].
The main dialog is displayed. The determination continues to run in
the background.

2 Opening the main menu

￭ Select Menu and press [OK].

3 Editing the method parameters

￭ Select the menu item Parameters and press [OK].
￭ Change the desired parameters accordingly.

4 Displaying the live dialog

￭ Select the menu item Live dialog in the main menu and press
[OK].
or
￭ Press [BACK] in the main dialog.
The live dialog is displayed once again.

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 5.10 Results ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

5.10 Results
Menu ▶ Results
After the completion of the titration, the results dialog is displayed:

The calculated result and details concerning the drift and the endpoint are
shown in the overview.
Curve
Display the curve of the current determination.
Recalculate
Recalculate the current determination. The procedure will be executed
immediately.
Statistics
Display the statistical overview of a determination series (see chapter 5.11,
page 57).

Displaying the curve

The curve of the current determination can be displayed with the Curve
function.

The arrow keys [⇦] and [⇨] can be used to move to the individual measur-
ing points. A cross hair is used to show the current position on the curve.
The data (water quantity, measured value, time, etc.) for the respective
measuring point is indicated on the right-hand side.

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Recalculating

NOTICE

Recalculation cannot be undone.

All of the results are recalculated with the Recalculate function. This is
necessary if, for example, the calculation or the sample size has been
modified.

5.11 Statistics
Menu ▶ Results ▶ Statistics
The statistical overview of a determination series can be displayed in the
Results dialog with the Statistics function.

NOTICE

This function is visible only if statistics has been activated.

The mean value (Mean), the absolute and the relative standard deviation
(s abs and s rel) are displayed in the overview. For the mean value, the
number of individual results from which it has been calculated is displayed
in parentheses. In this example, it is 3. The Statistics line shows how
many determinations have already been carried out and how many deter-
minations are to be carried out in total. All three determinations were car-
ried out in this example.
Details
Display additional data.
Reset
Delete all statistics data.
Increase
Add a further determination to the determination series.

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 5.11 Statistics ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

Displaying statistical details

Additional data from the determination series can be displayed with the
Details function.

The result and the sample size of each determination are shown.
On/Off
Remove the selected determination from the statistics. The line will then
be marked with an asterisk (*), the statistics will be recalculated automati-
cally. If several calculations are defined in the method, then all the results
will be removed from the statistics.

Deleting statistical data

All statistical data is deleted with the Reset function. The statistics data is
deleted automatically in the following cases:
￭ When all of the determinations of the determination series have been
carried out and a new determination has been started afterwards.
￭ When a new method is loaded.

Adding a determination to a determination series

You can use the function Increase to add an additional sample to a deter-
mination series, e.g. because a determination was faulty and had to be
removed from the statistics. The second number in the Statistics line will
be increased automatically by one.

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5.12 Printing a report manually

Menu ▶ Print reports
Proceed as follows to print a report manually:

1 Opening the main menu

￭ In the main dialog, select Menu and press [OK].

2 Opening the print dialog

￭ Select the menu item Print reports and press [OK].
The dialog window with the available reports opens:

3 Selecting the report

￭ Select the desired report and press [OK].
The report is printed out.

The following reports can be printed out manually:

Results Result report with determination properties,
sample data, calculated results, etc.
Curve Curve report. The width of the curve is defined in
the system settings (see "Graphics width", page
68).
Measuring point Measuring point list report.
list
Parameters Report with all method parameters of the loaded
method.

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 5.13 Manual control ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

System System report with system settings, external

devices, etc.
Calculations/Statis- Calculation report. The statistics are also printed
tics out in the case of multiple determinations. The
individual determinations with the respective
sample size, the mean value, the absolute and
the relative standard deviation are printed out
for each result.
PC/LIMS Machine-readable report with all of the data for
a determination. This report can be saved as a
TXT file to a connected USB flash drive or sent to
a terminal program or a LIMS via an RS-232
interface. The definition is made in the system
settings (see "PC/LIMS report", page 68).
Report as in The reports that are defined in the method will
method be printed out.

5.13 Manual control

Menu ▶ Manual control
The following function is available in the manual control:
￭ Stirring

The available subfunctions are listed in the function bar.

5.13.1 Stirring
Stirrers that are connected or installed in the Coulometer can be control-
led manually.
Proceed as follows:

1 Opening the manual control

￭ In the main dialog, select Menu and press [OK].
The main menu opens.
￭ Select the menu item Manual control and press [OK].
Manual control opens.

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2 Setting the stirring rate

￭
￭ In the function bar, select Stir- or Stir+.
The stirring rate will be increased or decreased by one step each
time the [OK] key is pressed.
The algebraic sign changes the direction in which the stirring is
done. When viewing the stirrer from above, this means:
– "+": counterclockwise rotation
– "–": clockwise rotation

3 Switching on the stirrer

￭ In the function bar, select On and press [OK].
The stirrer is started and stirs at the rate which has been set. Off is
now displayed in the function bar.

4 Switching off the stirrer

￭ In the function bar, select Off and confirm with [OK].
The stirrer is stopped.

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6 System settings

6.1 Basic settings

Menu ▶ System ▶ Settings
This chapter contains a description of general instrument settings.

User name
A user name can be entered here for the report. This parameter will only
be printed if a user has been defined.
Entry max. 12 characters
Default value empty

Instrument name
A instrument name can be entered here for the report. This parameter will
only be printed if a designation has been defined.
Entry max. 10 characters
Default value empty

Serial number
Serial number of the instrument. This is printed as a part of the instrument
identification in the report header.

Program version
Version number of the instrument software. This is printed as a part of the
instrument identification in the report header.

Time
Current time. Only valid numbers can be entered.
Format: hh:mm:ss

Date
Current date. Only valid numbers can be entered.
Format: YYYY:MM:DD

Language
Setting the dialog language. An additional language can be selected
besides English.

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NOTICE

In order to ensure that a second language can be selected, it must first

be installed. This installation must be carried out by specialist personnel.
In chapter Language files, page 71, you will find details regarding the
installation of a second language.

Dialog type
The user dialog can be limited for routine operations. One can operate
normally with methods in the limited dialog. However, no settings can be
made or methods deleted.
The resetting of the dialog will take effect as soon as you exit the main
menu.
The limitation of the dialog results in the following:
￭ The menu items System, Parameters and Control are not shown in
the main menu.
￭ Methods can only be loaded, but not deleted, exported or created.

NOTICE

If the limited dialog for routine operation is activated, then the expert
dialog cannot be activated during ongoing operation. To change the
dialog type, the 899 Coulometer must be switched off and then back
on again. The expert dialog can be forced as soon as the instrument is
started up again. Then it is possible to enter whatever settings one
wishes, e.g. the changing of the dialog type. If the instrument is
switched off again without changing the dialog type, then the routine
dialog will remain activated.

Forcing the expert dialog:

￭ Switch on the instrument.
￭ Wait for the display of the instrument logo with the lettering easy,
safe, precise.
￭ Press the [STOP] key once again and hold it down while also briefly
pressing the [BACK] key.
￭ Release both keys once again.
Selection Expert | Routine
Default value Expert
Expert
Complete dialog.

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Routine
Limited dialog for routine operations.

Contrast
The contrast of the display can be adjusted with the arrow keys [⇦] and
[⇨].
￭ [⇦]: the contrast will be decreased by one step each time the key is
pressed.
￭ [⇨]: the contrast will be increased by one step each time the key is
pressed.
Input range 150 - 240
Default value 212

NOTICE

Alternatively, the contrast can also be modified in the following man-

ner:
Keep the red [STOP] key pressed down. As soon as the progress bar
appears, also press the arrow key [⇩] or [⇧] repeatedly.
This method will, however, cause the contrast to be modified by several
steps.

Beep
If this parameter is activated, then a short beep will sound in the following
cases:
￭ When a key is pressed.
￭ At the end of the determination.
￭ When the system remains conditioned without interruption for 10 sec-
onds.
Selection on | off
Default value on

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6.2 Managing common variables

6.2.1 General
Menu ▶ System ▶ Common variables
The instrument offers the possibility of saving five method-independent
variables, so-called common variables. These variables remain saved in
the instrument and can be used in future calculations. A common variable
is useful, e.g. for the following applications:
￭ Determination of a blank value which will be taken into account during
the content determination of the sample.

The common variables have the non-changeable designation CV01…

CV05. The value is displayed for every variable. No unit can be assigned
to the common variables.
Edit
See the following chapter for editing the data of the selected common
variable.
Delete
Set the selected common variable to invalid.

6.2.2 Editing common variables

The common variables can be modified as follows:
￭ Manually in this dialog.
￭ Automatic assignment from the determination run. A calculation result
must be configured accordingly for this purpose (see below).

Assigning a result automatically to a common variable

Proceed as follows:

1 Opening the editing dialog of the result

￭ Select the menu item Parameters ▶ Calculation and press
[OK].

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￭ Select the result whose value is to be assigned to a common vari-

able.
￭ In the function bar, select Edit and press [OK].

2 Adjusting the result properties

￭ Select the parameter Save as CV and press [OK].
￭ Select the entry on in the selection list and apply with [OK].

The assignment of the result to a common variable occurs automatically

according to the following scheme:
￭ Result R1 ⇨ Common Variable CV01
￭ Result R2 ⇨ Common Variable CV02
￭ etc.

NOTICE

If you have set the parameter Statistics to on, then the mean value of
the results will be assigned to the respective common variable.

6.3 File management

Menu ▶ System ▶ File management

NOTICE

This menu item is visible only if a USB flash drive has been connected as
an external storage medium.

Methods can be imported and deleted from a USB flash drive in this dia-
log. Only methods located in the Files directory are displayed in the list
(see "Directory structure on the USB flash drive", page 67).
A backup of the system can be created (all data and settings). Similarly, an
existing backup can be reloaded.
Import
Import the selected method.

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Delete
Delete the selected method.
Backup
Create a backup of all data and settings on the USB flash drive.

NOTICE

Only one backup can be created on the same USB flash drive.
If a backup is already stored on the flash drive, then this will be over-
written as soon as the function is performed once again.

Restore
Load the backup from a connected USB flash drive.

Directory structure on the USB flash drive

A directory with the instrument number will be created on the USB flash
drive. The structure within this directory appears as follows:

Figure 24 Directory structure on the USB flash drive

Backup All of the files of the backup are stored in this
directory. The directory is created as soon as a
backup is created for the first time.
Files Exported methods are stored in this directory.
The directory is created as soon as a backup is
exported for the first time.
Only methods located in this directory can be
imported.
pc_lims_report PC/LIMS reports are stored in this directory as
TXT files. The directory is created as soon as a
PC/LIMS report is printed for the first time.

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6.4 Configuring external devices

Menu ▶ System ▶ External devices

PC/LIMS report
Specification of the storage location for the PC/LIMS report. The PC/LIMS
report is a machine-readable report with all of the important data for a
determination. It can be saved as follows:
￭ as a TXT file on a USB flash drive.
￭ to a LIMS via an RS-232 interface. The 6.2148.030 RS-232/USB Box is
required for this purpose.
Selection COM2 | USB Stick
Default value USB Stick
COM2
The report is sent via the serial COM2 interface. The interface parame-
ters set in the dialog COM2 settings are used (see "Editing the COM2
settings", page 70).
USB Stick
The report will be saved as a TXT file on the USB flash drive in the
folder pc_lims_report.

Printer
If a printer is connected, then the printer type needs to be defined here in
order for the reports to be printed out correctly.
The printers that have the designation ESC-POS are so-called POS printers
(point-of-sale printers), i.e. they print on continuous paper.
Selection Citizen (ESC-POS) | Custom (ESC-POS) | Epson |
Epson (ESC-POS) | HP DeskJet | HP LaserJet |
Seiko (ESC-POS)
Default value Custom (ESC-POS)

Graphics width
Adjust the width of the curve to be printed out to the paper width of the
printer to be used. The default value depends on the selected printer. The
height of the curve is 2/3 of the width.
Input range 100 - 3000 Pixels

Keyboard layout
A commercially available USB keyboard can be connected to make it eas-
ier to enter text and numbers. Specify the country-specific keyboard lay-
out.

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Selection English US | French FR | German CH | German

DE | Spanish ES
Default value English US

Balance
If you have connected a balance, then you must define the balance type
here.
Selection AND | Mettler | Mettler AT | Mettler AX |
Ohaus | Precisa | Sartorius | Shimadzu
Default value Sartorius
The following table indicates the balance type that needs to be selected
for the balance model:

Balance Balance type

AND AND
Mettler AB, AE, AG, AM, Mettler
AJ, PE, PM, PJ, PR, XP, XS
Mettler AT Mettler AT
Mettler AX, MX, UMX, PG, Mettler AX
AB-S, PB-S
Ohaus Voyager, Explorer, Ohaus
Analytical Plus
Precisa Precisa
Sartorius Sartorius
Shimadzu BX, BW Shimadzu

Editing the COM1 settings

Menu ▶ System ▶ External devices ▶ COM1 settings
The interface parameters for the connected balance are set under COM1
settings.

Baud rate
Transfer rate in characters per second.
Selection 1200 | 2400 | 4800 | 9600 | 19200 | 38400 |
57600 | 115200
Default value 9600

Data bits
Number of data bits.

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Selection 7|8
Default value 8

Stop bits
Number of stop bits.
Selection 1|2
Default value 1

Parity
Type of parity testing.
Selection even | none | odd
Default value none

Handshake
Type of the data transfer protocol.
Selection hardware | software | none
Default value hardware

NOTICE

If communications problems occur, set the parameter Handshake to

software, and make another attempt.

Editing the COM2 settings

Menu ▶ System ▶ External devices ▶ COM2 settings
The interface parameters for instruments connected to the RS-232/2 con-
nector of the RS-232/USB Box (e.g. PC) are set under COM2 settings.
The parameters and input ranges are identical to those for the COM1
interface.

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6.5 Instrument diagnosis

6.5.1 Loading program versions and language files
Menu ▶ System ▶ Diagnosis
New program versions or language files can be loaded from a USB flash
drive. The corresponding file must be saved on the USB flash drive in a
directory with the instrument number (e.g. 899).
You can distinguish between language files and program files by noting
how the file name is constructed.

Program files
They are instrument-specific. The file name has the following structure:
5XXXyyyy.bin where

XXX = Instrument type (e.g. 899 for the 899 Coulometer)

yyyy = Program version

Language files
They can be recognized by means of the two-digit language code in the
file name. A language file contains the dialog texts for various instrument
types. It is not instrument-specific. The file name has the following struc-
ture:
5848xxxxYY.bin where

xxxx = Version number

YY = Language, e.g. DE (German), FR (French), ES (Spanish)

Loading a file

Proceed as follows:

1 Connecting the USB flash drive

￭ Plug in the USB flash drive with the 6.2151.100 adapter (USB
MINI (OTG) - USB A) at the instrument's USB port.
￭ Switch on the instrument.

2 Opening the update dialog

￭ Under Menu ▶ System ▶ Diagnosis, select the menu item
Software update.
￭ Press [OK].

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3 Opening the file selection

￭ Press [OK].
The selection list with the program and language files present on the
USB flash drive opens.

4 Selecting the file

￭ Use the arrow keys to select the required file.
￭ Press [OK].

5 Starting the update

￭ Press [START].
The update process is started, it runs automatically. At the end of the
process, the instrument will be switched off automatically and
switched back on again. No user intervention is required.

6.5.2 Diagnosis functions

Electronic and mechanical functional groups in Metrohm instruments can
and should be checked as part of regular maintenance by specialist per-
sonnel from Metrohm. Please ask your local Metrohm representative
regarding the precise terms and conditions involved in concluding a corre-
sponding maintenance agreement.

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7 Parameters

7.1 Coulometric Karl Fischer titrations (KFC)

7.1.1 Conditioning
Menu ▶ Parameters ▶ Conditioning
Under Conditioning, the conditions required for conditioning are
defined.

Conditioning
If this parameter is activated, then the first time the titration is started the
working medium will be titrated to the endpoint with the specified control
parameters. The status is kept stable. The actual method run does not
begin until [START] has been pressed once more. Conditioning will be
carried out again automatically after the titration.
Selection on | off
Default value on

Start drift
If the measured drift is smaller than this value for a certain time (so-called
stabilizing time), then Conditioning OK will be displayed and the titra-
tion can be started. The stabilizing time is defined under Condition-
ing ▶ Stabilizing time.
Input range 1 - 999 µg/min
Default value 20 µg/min

Drift correction
The end point amount can be drift-corrected. To accomplish this, the drift
is multiplied by the drift correction time and this value is subsequently sub-
tracted from the amount of the end point. The drift correction time is the
time interval between the end of conditioning and the end of the determi-
nation.
Selection auto | manual | off
Default value auto
auto
The value of the current drift is automatically applied at the start of the
titration.
manual
If the drift is known throughout a longer period of time, this can be
entered manually.

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off
No drift correction takes place.

Drift value
This parameter can only be edited with Drift correction = manual.
Drift for manual drift correction.
Input range 0.0 - 99.9 µg/min
Default value 0.0 µg/min

Automatic start
If this parameter is activated, then the determination is automatically
started when the measured voltage suddenly changes. This setting will be
ignored as long as the working medium has not been conditioned.
Selection on | off
Default value off

NOTICE

If you use the automatic start function, then we recommend that the
start drift be reduced and that a stabilizing time be defined.
Recommendation: Start drift ≤ 10 µg/min / Stabilizing time ≥ 30 s

Threshold value
This parameter can only be edited with Automatic start = on.
If the change in voltage is higher than this value, then the determination
will automatically be started.
Input range 0 - 999 mV
Default value 50 mV

Stabilizing time
Waiting time, during which the measured drift has to be smaller than the
start drift defined until Conditioning OK is displayed. The start drift is
defined under Conditioning ▶ Start drift.
Input range 0 - 999999 s
Default value 0s

Cond. stop time

Maximum permissible time over which conditioning may take place. Con-
ditioning is stopped as soon as the specified time has elapsed.
Input range 1 - 999999 s

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Selection off
Default value off

Measured value display

If this parameter is activated, then the currently measured value is dis-
played during the conditioning.
Selection on | off
Default value off

7.1.2 Start conditions

Menu ▶ Parameters ▶ Start conditions
The parameters that are carried out before the start of titration are
defined under Start conditions.

Pause
Waiting time, for example for dissolving the sample. During this time no
iodine is generated.
Input range 0 - 999999 s
Default value 0s

Request sample ID
Selection of the sample identification that is queried in the method run.
Selection ID1 | ID2 | ID1&ID2 | off
Default value off

Request sample size

If this parameter is activated, then the value for the sample size will be
requested.
Selection on | off
Default value on

Request sample unit

If this parameter is activated, then the unit for the sample size will be
requested.
Selection on | off
Default value off

Hold at request
If this parameter is activated, then the run will be paused during the
request. If the parameter is deactivated, then the titration will be started in
the background.

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Selection on | off
Default value on

7.1.3 Control parameters

Menu ▶ Parameters ▶ Control parameters
The control parameters for the endpoint are defined under Control
parameters.

Endpoint at
Measured value for the endpoint.
Input range –1250.0 - 1250.0 mV
Default value 50.0 mV
Selection off

NOTICE

Note that the parameter Endpoint at is linked with the parameters

Dynamics and I(pol). Explanations in this connection can be found in
chapter 9.4 Control parameters and polarization current, page 95.

Titration rate
Three predefined sets of parameters can be selected for the titration rate.
Selection slow | optimal | fast | user
Default value optimal
slow
For samples with a low water content or samples which release their
moisture only slowly.
optimal
For all standard titrations. The parameters have been optimized for the
most frequent applications.
fast
For uncritical samples with high water content.
user
The individual titration parameters can be modified.
The settings of the individual titration rates are listed in table 3, page 77.

Dynamics
This parameter can only be edited with Titration rate = user.
This parameter defines the control range before the specified endpoint.
Within the control range, the iodine is generated step by step, the genera-

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tion is finely controlled. The closer the endpoint, the slower the iodine is
generated until the rate defined under Min. rate is reached. The larger
the control range, the slower the titration. Outside the control range,
iodine is being continuously generated, the rate is defined under Max.
rate.

Input range 0.1 - 1250.0 mV

Default value 70.0 mV
Selection off
off
The generation of iodine is finely controlled during the entire titration.

NOTICE

Note that the parameter Dynamics is linked with the parameters End-
point at and I(pol). Explanations in this connection can be found in
chapter 9.4 Control parameters and polarization current, page 95.

Max. rate
This parameter can only be edited with Titration rate = user.
Rate at which iodine is generated outside the control range.
Input range 1.5 - 2241.0 µg/min
Selection max.
Default value max.

Min. rate
This parameter can only be edited with Titration rate = user.
Rate at which iodine is generated at the very beginning of the titration
and in the control range at the end of the titration. This parameter has a
decisive influence on the titration rate and thus also on the accuracy. The
smaller the selected minimum rate, the slower the titration.
Input range 0.3 - 999.9 µg/min
Default value 15.0 µg/min

Table 3 Default values of the predefined titration rates for KFC

Titration rate
slow optimal fast
Dynamics 120.0 mV 70.0 mV 30.0 mV
Max. rate 1000.0 µg/min maximum maximum
Min. rate 0.3 µg/min 15.0 µg/min 30.0 µg/min

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 7.1 Coulometric Karl Fischer titrations (KFC) ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

Stop criterion
The titration is canceled when the endpoint has been reached and this
stop criterion has been fulfilled. If no stop criterion has been selected then
the titration will not be canceled. The stop conditions (see chapter 7.1.5,
page 81) always lead to a stop, even if the stop criterion has not been
reached.
Selection drift | time | rel. drift | off
Default value rel. drift
drift
The titration is canceled when the stop drift has been reached.
time
The titration is canceled if the endpoint has been exceeded during a
certain time period (Delay time).
rel. drift
The titration is canceled when the sum of the drift at the start of the
titration and the relative stop drift has been reached.
off
The titration will not be canceled until the stop conditions have been
fulfilled.

Stop drift
This parameter can only be edited with Stop criterion = drift.
The titration is canceled when the endpoint and the stop drift have been
reached.
Input range 1 - 999 µg/min
Default value 5 µg/min

Delay time
This parameter can only be edited with Stop criterion = time.
The titration will be canceled if the following criteria are both met simulta-
neously.
￭ The voltage at the indicator electrode lies in the range "endpoint +5
mV and endpoint –2 mV".
￭ The time defined here has expired.
If, for example, the parameter Endpoint at is set to 50 mV and the para-
meter Delay time defined here is 10 s, then the voltage at the indicator
electrode must be between 55 mV and 48 mV for 10 seconds so that the
titration would be canceled.
Input range 0 - 999 s
Default value 10 s

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Relative stop drift

This parameter can only be edited with Stop criterion = rel. drift.
The titration is canceled when the endpoint and the sum of the drift at the
start of the titration and the relative stop drift have been reached.
Input range 1 - 999 µg/min
Default value 5 µg/min

7.1.4 Titration parameters

Menu ▶ Parameters ▶ Titration parameters
Under Titration parameters, the parameters influencing the sequence
of the entire titration are defined.

Extraction time
Minimum duration of the titration. The titration will not be canceled dur-
ing the extraction time, even if the endpoint has already been reached.
The titration is however canceled if a stop condition is fulfilled during this
time (see chapter 7.1.5, page 81). The entering of an extraction time is
e.g. recommended with samples that release water slowly or if a Karl
Fischer oven is used.
Input range 0 - 999999 s
Default value 0s

Generator electr.
Type of generator electrode.
Selection with diaphr. | w/o diaphr.
Default value w/o diaphr.
with diaphr.
Generator electrode with diaphragm.
w/o diaphr.
Generator electrode without diaphragm.

Generator current
Polarization current at the generator electrode.
Selection 100 mA | 200 mA | 400 mA | auto
Default value 400 mA
400 mA
default value, when Generator electr. = w/o diaphr.
auto
The current is adapted to the conductivity of the reagent and automat-
ically reduced near the endpoint. Default value, when Generator
electr. = with diaphr.

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 7.1 Coulometric Karl Fischer titrations (KFC) ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

Stirrer
The stirrer is switched on at the start of the determination when this para-
meter is activated.
Selection on | off
Default value on

Stirring rate
Setting the stirring rate. It can be set in steps of –15 to +15. The default
setting 8 corresponds to 1000 rpm. The formula for calculating the rota-
tional speed is specified in chapter 9.1, page 92. The optimum stirring
rate can be tested in the manual control.
The algebraic sign changes the direction in which the stirring is done.
When viewing the stirrer from above, this means:
￭ "+": counterclockwise rotation
￭ "–": clockwise rotation
Input range –15 - 15
Default value 8

I(pol)
The polarization current is the current that is applied to a polarizable elec-
trode during the voltametric measurement.
Selection 5 µA | 10 µA | 20 µA | 30 µA
Default value 10 µA

NOTICE

Note that the parameter I(pol) is linked with the parameters Dynamics
and Endpoint at. Explanations in this connection can be found in
chapter 9.4 Control parameters and polarization current, page 95.

Electrode test
In the case of polarizable electrodes, an electrode test can be carried out.
A check is made that the electrode is properly connected and that no
short-circuit is present. The electrode test is carried out as soon as the
determination is started.
Selection on | off
Default value off

Time interval MP
Time interval for entering a measuring point in the measuring point list.
The measuring point list is limited to 1000 measuring points.

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Input range 0.1 - 999999.0 s

Default value 2.0 s

Temperature
Temperature entered manually.
Input range –20.0 - 150.0 °C
Default value 25.0 °C

7.1.5 Stop conditions

Menu ▶ Parameters ▶ Stop conditions
The conditions for stopping a titration are defined under Stop condi-
tions, if this does not occur automatically. This could be the case when
the endpoint set is not reached or if the stop criterion (see "Stop crite-
rion", page 78) is not fulfilled.

Stop time
The titration is canceled when the specified time has elapsed since the
start of the titration.
Input range 1 - 999999 s
Selection off
Default value off

7.1.6 Calculation
7.1.6.1 General
Menu ▶ Parameters ▶ Calculation
A maximum of five calculations can be defined in one method. A series of
variables (raw data from the determination, previously calculated results) is
available for the calculations. Definition can be made for each calculation
as to whether the result is to be saved as a common variable.

The result name is specified in the list for each calculation.

The method templates KFC, KFC-Blank and Blank each contains one
calculation. Each of these calculations already bears an appropriate result
name. You can modify these as needed.

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 7.1 Coulometric Karl Fischer titrations (KFC) ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

Edit
See the following chapter for editing the data of the selected calculation.

Delete
Delete the selected calculation.

7.1.6.2 Editing calculations

Method "KFC"

Result name
The result name is the text which will be shown in the results display and
in the report.
Entry 12 characters
Default value R1: Water / R2-R5: empty

Calculation formula "R1"

EP1/C00

R2…R5
Display of the calculation formula. A special editor is opened for the defi-
nition (see chapter 5.3, page 39).
Entry 30 characters
Default value empty

Decimal places
Number of decimal places used to display the result.
Input range 0-5
Default value R1: 1 / R2-R5: 2

Result unit
The result unit is displayed and saved together with the result.
R1
Selection % | mg | mg/piece | mg/g | mg/mL | ppm | µg |
User-defined
Default value ppm
R2-R5
Selection % | mg | mg/piece | mg/g | mg/mL | ppm | µg |
User-defined
Default value %

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User-defined
A user-defined unit can be created. This will be added to the selection
list. The previous entry will be overwritten as soon as the new unit has
been defined. A blank entry can be generated this way as well.

Save as CV
The calculated result can be saved as a method-independent variable, a
so-called common variable. The result is then also available in other meth-
ods for calculations. If Statistics has been activated, then the current mean
value of the determination series will be saved.
Selection on | off
Default value off

Method "KFC-Blank"

Result name
The result name is the text which will be shown in the results display and
in the report.
Entry 12 characters
Default value R1: Water / R2-R5: empty

Calculation formula "R1"

(EP1–CV01)/C00

CV01 is the Common Variable 01 and corresponds to the result from the
calculation of the Method "Blank", page 84.

R2…R5
Display of the calculation formula. A special editor is opened for the defi-
nition (see chapter 5.3, page 39).
Entry 30 characters
Default value empty

Decimal places
Number of decimal places used to display the result.
Input range 0-5
Default value R1: 1 / R2-R5: 2

Result unit
The result unit is displayed and saved together with the result.
R1

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Selection % | mg | mg/piece | mg/g | mg/mL | ppm | µg |

User-defined
Default value ppm
R2-R5
Selection % | mg | mg/piece | mg/g | mg/mL | ppm | µg |
User-defined
Default value %
User-defined
A user-defined unit can be created. This will be added to the selection
list. The previous entry will be overwritten as soon as the new unit has
been defined. A blank entry can be generated this way as well.

Save as CV
The calculated result can be saved as a method-independent variable, a
so-called common variable. The result is then also available in other meth-
ods for calculations. If Statistics has been activated, then the current mean
value of the determination series will be saved.
Selection on | off
Default value off

Method "Blank"

Result name
The result name is the text which will be shown in the results display and
in the report.
Entry 12 characters
Default value R1: Blank / R2-R5: empty

Calculation formula "R1"

EP1

R2…R5
Display of the calculation formula. A special editor is opened for the defi-
nition (see chapter 5.3, page 39).
Entry 30 characters
Default value empty

Decimal places
Number of decimal places used to display the result.
Input range 0-5
Default value 2

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Result unit
The result unit is displayed and saved together with the result.
R1
Selection % | mg | mg/piece | mg/g | mg/mL | ppm | µg |
User-defined
Default value µg
R2-R5
Selection % | mg | mg/piece | mg/g | mg/mL | ppm | µg |
User-defined
Default value %
User-defined
A user-defined unit can be created. This will be added to the selection
list. The previous entry will be overwritten as soon as the new unit has
been defined. A blank entry can be generated this way as well.

Save as CV
The calculated result can be saved as a method-independent variable, a
so-called common variable. The result is then also available in other meth-
ods for calculations. If Statistics has been activated, then the current mean
value of the determination series will be saved.
R1
Selection on | off
Default value on
R2-R5
Selection on | off
Default value off

7.1.7 Statistics
Menu ▶ Parameters ▶ Statistics
The statistics calculation of a multiple determination is activated under
Statistics and definition is made as to how many determinations the
series contains.

Statistics
If this function is activated, then statistics calculations will be carried out
for all of the defined results.
Selection on | off
Default value off

Number of determinations
The number of determinations that are carried out for the statistics calcu-
lations.

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 7.1 Coulometric Karl Fischer titrations (KFC) ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

If an additional determination has to be added to the determination

series, because one determination has been incorrect, for example, then
this can be accomplished in the statistical overview (see chapter 5.11,
page 57).
Input range 2 - 20
Default value 3

7.1.8 Reports
Menu ▶ Parameters ▶ Reports
The reports that will be printed out automatically in connection with a
determination are defined under Reports.

Results
The result report contains the calculated results, endpoints, sample data,
etc.
Selection on | off
Default value off

Curve
Curve report. The width of the curve is defined in the system settings (see
"Graphics width", page 68).
Selection on | off
Default value off

Calculations/Statistics
Output of the calculation formulas for the individual results. Results are
specified with full accuracy. This makes recalculation with an external pro-
gram possible. If Statistics has been activated, then the following data will
be printed out as well:
￭ Result and sample size of the individual determinations
￭ Mean value as well as absolute and relative standard deviation
Selection on | off
Default value off

Measuring point list

Output of the measuring point list.
Selection on | off
Default value off

Parameters
All of the parameters of the current method are printed out in the para-
meter report.

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Selection on | off
Default value off

PC/LIMS
The PC/LIMS report is a machine-readable report with all of the data
important for a determination. The PC/LIMS report can be saved as a TXT
file on a USB storage medium or sent via an RS-232 interface to a LIMS.
The output location is defined in the system settings (see "PC/LIMS
report", page 68).
The file name of the TXT file is constructed as follows: PC_LIMS_Report-
ID1-YYYYMMDD-hhmmss.txt.
Selection on | off
Default value off

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 8.1 Karl Fischer titration ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

8 Troubleshooting
8.1 Karl Fischer titration
Problem Cause Remedy
The drift is very high The titration cell is leaking. ￭ Check the septum and replace it if neces-
during conditioning. sary.
￭ Replace the molecular sieve.
￭ Check the ground-joint sleeves for frayed
edges. If necessary, trim the edges neatly
or replace the ground-joint sleeves.

Deposits containing water ￭ Shake the titration cell.

can be found in the titra-
tion cell.

The reagent is exhausted ￭ Replace the reagent.

or contaminated.

The catholyte is old or ￭ The catholyte must be replaced at least

moist. once per week.
￭ Dry the catholyte with KF one-component
reagent.

The diaphragm of the gen- ￭ Clean the diaphragm (in accordance with
erator electrode is contam- directions in the leaflet for the generator
inated. electrode).

A side reaction is taking ￭ Consider using a KF oven.

place. ￭ See technical literature.

The molecular sieve on the ￭ Replace the molecular sieve.

KF oven has reached its
capacity limit.

The gas flow from the KF ￭ Reduce the gas flow (if you are working
oven into the titration cell with the oven method with sample vials,
is too high. set the gas flow between 40 and 60
mL/min).

The drift becomes The sample releases water ￭ Consider using a KF oven.
greater after each very slowly. ￭ See technical literature.
titration.

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Problem Cause Remedy

The drift is fluctuat- The sample solution is ￭ Set the stirring rate in such a way that the
ing. poorly stirred. sample solution will become very well
mixed.

The Control parameters ￭ Reset the Control parameters to default

are set incorrectly. values.

The titration time is The drift during condition- ￭ Wait before starting the titration until the
too long. ing is not stable. drift has become stable.

The parameter Start drift ￭ Set the Start drift lower.

is set too high. ￭ Adjust the Stop drift or use the Relative
stop drift.

The parameter Stop drift ￭ Set the Stop drift higher or use the Rela-
is set too low. tive stop drift.

The water quantity is too ￭ Observe the sample size and water con-
high. tents in accordance with Table "Recom-
mended sample sizes", page 31.

The Control parameters ￭ Set the parameter Dynamics lower and

are set incorrectly. the parameter Max. rate higher.

The result is too The titration cell is not yet ￭ Shake the titration cell and wait until the
high. correctly conditioned. drift is stable.

The sample contains oxi- ￭ Consider using a KF oven.

dizable substances. ￭ See technical literature.

The parameter Stop drift ￭ Set the Stop drift higher or use the Rela-
is set too low. tive stop drift.

The drift correction is too ￭ Start the titration as long as the gas flow
small (e.g. for the use of a still exists between the conditioning vial
KF oven or for manual drift and the titration cell.
correction). ￭ Set the parameter Drift correction to
auto (= automatic drift correction).

The result is too The sample releases iodine. ￭ Consider using a KF oven.
low. ￭ See technical literature.

The parameter Stop drift ￭ Set the Stop drift lower.

is set too high.

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 8.2 Miscellaneous ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

Problem Cause Remedy

The drift correction is too ￭ Ensure stable and lower drift.
large (e.g. with excessively ￭ Set the parameter Drift correction to
high start drift, with fluctu- auto (= automatic drift correction).
ating drift or with manual
drift correction).

The parameter Min. rate ￭ Set the parameter Min. rate higher.
is set too low. ￭ Reset the Control parameters to default
values.

The results are The sample is nonhomoge- ￭ Homogenize the sample if possible.
spread widely. nous. ￭ Possibly use a larger sample size.

The sample addition is diffi- ￭ Observe the instructions in Chapter 4.3,

cult to reproduce. page 31.

The drift fluctuates. ￭ Ensure stable drift.

8.2 Miscellaneous
Problem Cause Remedy
No report is printed. The printer is not recog- ￭ Switch the 899 Coulometer off and then
nized by the instrument. back on again.
￭ Use a USB hub and connect the printer to
the USB hub.

The printer model is not Use a printer which fulfills the required specifi-
compatible. cations (see chapter 9.3.4, page 95).

The USB keyboard The keyboard or mouse is ￭ Switch the 899 Coulometer off and then
or the PC mouse not recognized by the back on again.
does not function. instrument. ￭ Use a USB hub and connect the keyboard
or mouse to the USB hub.

The keyboard or the mouse Use a model which fulfills the required specifi-
is not compatible. cations (see chapter 9.3, page 93).

The display is no The contrast is set incor- Adjust the contrast correctly (see chapter 6.1,
longer readable. rectly. page 62).

Mettler XP balances The automatic calibration Deactivate the automatic calibration.

send "R" or "O ----" of the balance is activated.
as ID1.

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Problem Cause Remedy

Message 020-511 The USB flash drive is no 1. Connect the USB flash drive.
"Action not possi- longer connected. 2. Switch the instrument off and then back on
ble" is displayed. again.

The USB flash drive is full. ￭ Use a different USB flash drive.
￭ Delete files with the aid of a PC.

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9 Appendix

9.1 Stirring rate

The stirring rate can be adjusted in steps from –15 to +15.
The approximate rotational speed for the internal magnetic stirrer
(depends on the product version) can be calculated with the following for-
mula:

Rotational speed/min (r/min) = 125 · Stirring rate

Example:
Configured stirring rate: 8
Rotational speed in revolutions per minutes = 125 · 8 = 1,000
r/min

2000

1500

1000

500

-15 -10 -5 0 5 10 15
Figure 25 Rotational speed depending on the stirring rate
The information on the separately connectable 802 propeller stirrer can be
found in the "802 Stirrer" manual.

9.2 Balance
The sample size and the associated unit can be sent from a connected bal-
ance. The sample size is transmitted as a number with up to ten characters
(including algebraic sign and decimal point).
Sample size and unit are sent as a single character string. They are separa-
ted by a space character. The string is terminated with the ASCII charac-
ters CR and LF.
If the balance sends a negative sample size (e.g. when you are reweighing
a sample), then the algebraic sign is adopted. The algebraic sign is, how-
ever, ignored for the calculations.

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NOTICE

With some balances, the sample identification and the method can be
sent in addition to the sample size.
Make sure that the balance does not send the sample size until the end.

Mettler AX
For the Mettler AX balance, the fields that contain the sample identifica-
tion or the method must be designated as follows:
￭ Designation for the field with the method name: METHOD
￭ Designation for the field with sample identification 1: ID1
￭ Designation for the field with sample identification 2: ID2

9.3 USB devices

NOTICE

USB peripheral devices that are to be connected must support either

the USB 1.0/1.1 (Full Speed) or the USB 2.0 (High Speed) standard. The
maximum data transfer rate is however in any case 12 MBit/s.
Keyboards, PC mice and barcode readers are so-called HID devices
(Human Interface Device) and can be connected via a USB hub only.
Printers should also be connected via a USB hub. Depending on the
manufacturer or printer type a direct connection is however possible.

9.3.1 6.2147.000 numerical USB keypad

The [Num Lock] key must be pressed for navigating in the dialog. The
arrow keys are effective in conjunction with it.
The respective editing dialog must be opened for the numerical input.

Table 4 Key assignment

Key of the 899 Coulometer or Key on the numerical USB
function in the editing dialog keypad
[BACK] [Home]
[⇧] [⇩] [↑] [↓]
[⇦] [⇨] [←] [→]
[OK] [Enter]

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Key of the 899 Coulometer or Key on the numerical USB

function in the editing dialog keypad
[BS] (backspace)
Clear [Del]
Accept [Home]

9.3.2 Key assignment of a USB keyboard

A commercially available USB keyboard can be connected to make it eas-
ier to enter text and numbers.
The respective editing dialog must be opened for the text input and
numerical input.

Table 5 Key assignment

Key of the 899 Coulometer or Key on the USB keyboard
function in the editing dialog
[BACK] [Esc]
[⇧] [⇩] [↑] [↓]
[⇦] [⇨] [←] [→]
[OK] [↲] (enter key)
or
[Enter] on the numerical keypad
[STOP] [Ctrl] + [S]
[START] [Ctrl] + [G]
[←] (backspace)
Clear [Delete]
Cancel [Ctrl] + [Q]
Accept [Esc]

NOTICE

The lettering of the USB keyboard may differ from above lettering,
depending on the country-specific keyboard used.

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9.3.3 PC mouse
In order to make navigating in the dialog of the 899 Coulometer easier, a
PC mouse can be connected.

Table 6 Mouse functions

Key of the 899 Coulometer Mouse function
[OK] Left mouse button
[BACK] Right mouse button
[⇧] [⇩] [⇦] [⇨] Mouse movement vertical/hori-
zontal
[⇧] [⇩] Scroll wheel vertical

9.3.4 Printer
The range of USB printers available is extremely varied and constantly
changing. The following points must be taken into account when select-
ing a printer:
￭ USB interface necessary
￭ Printer language: HP-PCL, Canon BJL Commands, Epson ESC P/2 or
ESC/POS

NOTICE

Inexpensive printers are often designed solely for use with a PC and
may not be equipped with one of the printer languages listed above.
Such models are not suitable for this reason.

9.4 Control parameters and polarization current

The standard control parameters are optimally set for most determinations
and should not be altered. Should you nevertheless need to change the
control parameters for special reagents and/or samples, please note that
the following parameters are dependent on one another:
￭ The polarization current of the indicator electrode (see parameter
"I(pol)", page 80)
￭ The end point (see parameter "Endpoint at", page 76)
￭ The control range (see parameter "Dynamics", page 76)

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 9.4 Control parameters and polarization current ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

Measured value / mV
Ipol = 30 µA

Ipol = 20 µA

Control range

Ipol = 10 µA Endpoint

Ipol = 5 µA
Ipol = 2 µA

Water / µg
Figure 26 Control parameters and polarization current
The diagram shows Karl Fischer titration curves at different polarization
currents (Reagent Coulomat AD). It is clear to see that the position of the
endpoint varies with the polarization current. The curves have different
slopes, i.e. the dynamics must also be adapted. Polarization currents < 10
µA are not suitable for this application. The following table gives you an
idea of the optimal control parameters for various polarization currents.

Table 7 Optimum control parameters at different polarization currents

I(pol) (polari- 10 µA 20 µA 30 µA
zation cur-
rent)
Endpoint at 50 mV 100 mV 150 mV
Dynamics 70 mV 100 mV 120 mV
Max. rate Default value Default value Default value
Min. rate Default value Default value Default value
Stop drift Default value Default value Default value

The indicator electrode is activated after a certain period of use in the

same reagent, i.e. the titration curve becomes steeper. If the titration
curve is too steep, then slowly fluctuating drift values could occur during
conditioning. You can solve this problem by setting the endpoint lower.
Endpoints that have been set too low could however prolong the titration.
This could have unfavorable effects on the measuring error.

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9.5 Method examples for working with the Karl Fischer

oven
You will find the recommended parameter settings for working with a Karl
Fischer oven in the following table. The methods can be used either with a
sample changer with oven module (e.g. 885 Compact Oven SC) or with a
Karl Fischer oven (e.g. 860 KF Thermoprep). The table contains only para-
meter settings that differ from the default values.

Parameters Blank value Water content

determination determination
(method tem- (method tem-
plate Blank) plate KFC-Blank)
>Conditioning

Start drift 10 µg/min *) 10 µg/min *)

Stabilizing time 30 s 30 s

>Start conditions

Request sample size off off

Hold at request off off

>Titration parameters

Extraction time 180 s 180 s

Stirring rate 12 12

>Statistics

Statistics on –

Number of determina- 3 –
tions
>Reports

Results on on

Calculations/Statistics on –

*) If you work in an environment with high humidity, then we recommend

that the parameter Start drift be set to 20 µg/min.

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 9.6 System initialization ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

9.6 System initialization

In very rare instances, a faulty file system (e.g. because of a program
crash) may lead to an impairment of program functioning. The internal file
system must be initialized in such cases.

CAUTION

All user data (methods, etc.) are deleted if a system initialization is car-
ried out. Afterwards, the instrument will have the factory settings again.
We recommend creating a backup of the system at regular intervals in
order to avoid data losses.

After a system initialization the program versions and language files do

not have to be reloaded. Only the selection of the dialog language may
have to be reset in the system settings.
Proceed as follows for the system initialization:

1 Switching off the instrument

￭ Keep the red [STOP] key pressed down for at least 3 s.
A progress bar is displayed. If the key is released during this time,
then the instrument will not be switched off.

2 Switching on the instrument

￭ Keep the red [STOP] key pressed down for approx. 10 s.
The dialog for confirmation of the initialization is displayed for 8 s.
The initialization must be confirmed during this time.

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3 Confirming the initialization

NOTICE

If the request is not confirmed within 8 s, then the procedure will

be canceled.

￭ Press [BACK] twice.

Initialization is started. The process takes approximately 80 s. The
instrument will be automatically restarted after successful initializa-
tion.

9.7 Remote interface

9.7.1 Pin assignment of the remote interface
5 1
1 5

9 6
6 9
Figure 27 Pin assignment of remote socket and remote plug
The above figure of the pin assignment applies for all Metrohm instru-
ments with 9-pin D-Sub remote connector.

Table 8 Inputs and outputs of the remote interface

Pin No. Assignment Function
1 Output 0 Ready/EOD
2 Output 1 -
3 Output 2 Titration
4 Output 3 Cond OK
5 Output 4 Error
6 0 volt (GND)
7 +5 volts
8 Input 0 Start
9 Input 1 Stop

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 9.7 Remote interface ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

Inputs
+5 V approx. 5 kΩ Pull-up
tp
tp > 100 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

9.7.2 Status diagram of the remote interface

[START] [START]
EOD
ready/EOD Output 0

Output 1

Titr/Determ Output 2

condOK Output 3

Error Output 4

Start Input 0

Stop Input 1
[STOP]

Figure 28 Remote status diagram

EOD = End of Determination

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9.8 Remote control via an RS-232 connection

The 899 Coulometer can be remote controlled via an RS-232 connection.
For this, a 6.2148.030 RS-232/USB Box is necessary. Connect the
RS-232/USB Box to the USB interface of the instrument.
The RS-232/USB Box has two connectors for RS-232 instruments. The
RS-232 remote control functions only through the connector RS-232/2.
The connector RS-232/1 is designed for connection with a balance. Con-
nect the RS-232/2 connector of the RS-232/USB Box to a serial interface
(COM interface marked with the symbol IOIOI) of a PC. Use a
6.2134.040 connection cable.

6.2134.040

Figure 29 Connecting the RS-232/USB Box to the PC

Interface parameters
We recommend the following parameters for the RS-232 interface
COM2:
￭ Baud rate: 19200
￭ Data bits: 8
￭ Stop bits: 1
￭ Parity: none
￭ Handshake: software
On the 899 Coulometer, adjust the interface parameters under
Menu ▶ System ▶ External devices ▶ COM2 settings.

Transfer protocol
The data communication is synchronous. On each command there is an
acknowledgement by the instrument.
A command must be sent to the instrument with the control characters
CR LF as terminator. The acknowledgements of the instrument will also
be transferred with CR LF as terminator.
The instrument does not send spontaneous messages.

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 9.8 Remote control via an RS-232 connection ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

9.8.1 Commands and variables

Command Function Comment
$G Start/Continue Corresponds to the key [START] or [Con-
tinue]
$S Stop Corresponds to the key [STOP]
$H Hold Hold the method run
$D Scan instrument sta- Acknowledgements: Ready;0, Busy;0,
tus Hold;0 or Cond;0 (0 = no message)
If a message on the instrument requires
the interaction of the user, the acknowl-
edgement of the status scan displays the
corresponding message number. Example:
Busy;012-111
= 012-111 Conditioning not OK
The message can be confirmed with [Yes]
or [No], see below.
$A Confirm message Confirm the message on the instrument
with [OK]
A mandatory status scan providing the
message number must take place immedi-
ately before confirming the message, see
above.
$A(OK), $A(CANCEL) Confirm message Confirm the message with [OK] or [Can-
cel]
$A(YES), $A(NO) Confirm message Confirm the message with [Yes] or [No]
$L(method name) Load method The method name has to be known and
unique.
$Q(variable) Request variable value Examples for variables: EP1, R1, C00.
Complete list of the variables, see page
39.

The values of the variables are only available after the end of a determina-
tion (in the status 'ready').

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Acknowledgement of Comment
the instrument
OK Command executed
E1 Method not found
E2 Invalid variable
E3 Invalid command

9.9 Arithmetic algorithms in the 899 Coulometer

Numerical format
The software of the 899 Coulometer calculates in accordance with the
widespread standard IEEE 754 (IEEE Standard for Binary Floating-Point
Arithmetic for Microprocessor Systems). This means that the numbers are
used in calculations in "double precision" (64 bit). Decimal numbers are
converted into binary numbers in the computer and used in this form for
calculations. The output on the display and in reports once again contains
decimal numbers; the binary numbers are thus converted back into deci-
mal numbers. In order to be able to check the internal calculations per-
formed by the computer yourself in accordance with IEEE 754, the num-
bers are reproduced in the calculation report in complete accuracy. A mini-
mal difference may arise between an originally entered decimal number
and the internal computer representation in complete accuracy in the
range of the rear decimal places. This difference results from the fact that
an exact binary equivalent does not exist for every decimal number. If, for
example, you enter the sample size 50.3 mg, this will be depicted in the
calculation report in "double precision" with 5.02999999999999E+01.

Rounding-off process
Measured values and results are rounded to the defined number of deci-
mal places (commercial rounding, in accordance with the US Pharmaco-
peia USP). If the digit at the first dropped decimal place is 1, 2, 3 or 4,
then it will be rounded off; if this digit is 5, 6, 7, 8 or 9, then it will be
rounded up. Negative digits will be rounded in accordance with their
amount, i.e. away from zero.
Examples:
2.33 yields 2.3
2.35 yields 2.4
2.47 yields 2.5
–2.38 yields –2.4
–2.45 yields –2.5

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 9.9 Arithmetic algorithms in the 899 Coulometer ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

Statistics
The arithmetic mean value and the absolute and relative standard devia-
tions of results are calculated:
You can statistically evaluate a maximum of five results (1 ≤ k ≤ 5) calcu-
lated in a determination. A statistical series can contain a maximum of 20
determinations (1 ≤ n ≤ 20).
The following convention applies to the subsequent formulas:
1 ≤ n ≤ 20 and 1 ≤ k ≤ 5.

Mean value:

Absolute standard deviation:

Relative standard deviation (in %):

Explanations
The individual values are incorporated in the statistics with full accuracy.
15 significant places are yielded when the 64 bit numerical format is
applied for the floating-point number in decimal presentation.
The accuracy can be controlled by the selection of the prefix of the unit
(milli, micro) and the number of decimal places.
Example:
The result displayed, 1234.56789158763 mg/L, has 15 significant pla-
ces. It should be rounded off to three decimal places according to the
above rounding-off process:
￭ 1234.568 mg/L.
If the same result is expressed in "g/L" (1.23456789158763 g/L), and is
also rounded off to three decimal place, this yields
￭ 1.235 g/L.
I.e. you obtain the lowest losses in accuracy with rounding when you
select the application and the numerical format in such a way that the
numbers displayed have as many places before the decimal point as possi-
ble.
A complete recalculation of the statistics using a pocket calculator or PC
calculation programs may exhibit deviations. This can be explained by the
different binary numerical formats used by these computers.

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NOTICE

The above losses of accuracy by rounding off in the range of significant

places are only relevant theoretically. They are generally several orders
of magnitude less than measurement technique uncertainties (balance
errors, dosing errors, measuring errors).

899 Coulometer ￭￭￭￭￭￭￭￭ 105

 10.1 Measuring inputs ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

10 Technical specifications

10.1 Measuring inputs

The measuring cycle is 100 ms for the measuring mode Ipol AC.

10.1.1 Indicator electrode

One measuring input (Ind.) for an indicator electrode.
Measuring mode Determination with adjustable polarization current.
Ipol Voltametric endpoint indication with alternating current.
Polarization cur- typical: 5, 10, 20 and 30 µA
rent

10.1.2 Temperature
One measuring input (Temp.) for one Pt1000-model temperature sensor.
Measuring range –150…+250 °C
Resolution 0.1 °C
Measuring accu- ±0.2 °C
racy (Applies for measuring range –20…+150 °C; ±1 digit; without sensor
error, under reference conditions.)

10.2 Generator connector

One electrode connector (Gen.) for a generator electrode.

10.2.1 Generator electrode

Iodine generation with current pulses or continuous current.
Current at the auto: variable direct current
electrode 100, 200, 400 mA: pulsating direct current
Imax 400 mA

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10.3 Internal stirrer

Rotational speed
Maximum rota- ±(1700…1900) rpm
tional speed
Setting of the ±15 steps
rotational
speed
Change in rota- ±(115…125) rpm
tional speed per
step

Fuse Electronic overload protection

10.4 Interfaces and connectors

MSB connector 8-pin Mini DIN socket for connecting an additional stirrer.
MSB1
USB (OTG) connec- For connecting USB peripheral devices.
tor
Remote connector For connecting instruments with a remote interface.

10.5 Power supply

External power 24 V, 65 W
supply unit
Input voltage 20…28 V DC
range
Maximum 36 W
power con-
sumption

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 10.6 Ambient temperature ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

10.6 Ambient temperature

Nominal function +5…+45 °C
range (at a maximum of 85% humidity)
Storage –20…+60 °C
Transport –40…+60 °C

10.7 Reference conditions

Ambient tempera- +25 °C (± 3 °C)
ture
Relative humidity ≤ 60%
Operating temper- Instrument in operation at least 30 min
ature status
Validity of the after calibration
data

10.8 Dimensions
Width 143.5 mm
Height (without 112 mm
titration vessel
holder)
Height (with titra- 195 mm
tion vessel holder)
Depth 281.5 mm
Weight (including 2800 g
power supply unit)
Material
Housing PBT

Material
Base Stainless steel 1.4301

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11 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:

Downloading the accessories list

1 Enter https://www.metrohm.com/ into your Internet browser.

2 Enter the article number (e.g. 899) into the search field.
The search result is displayed.

3 Click on the product.

Detailed information regarding the product is shown on various tabs.

4 On the Included parts tab, click on Download the PDF.

The PDF file with the accessories data is created.

NOTICE

Once you have received your new product, we recommend download-

ing the accessories list from the Internet, printing it out and keeping it
together with the manual for reference purposes.

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 Index ￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭￭

Index
A D Karl Fischer oven
Adapter Determination Method examples ............... 97
Connect ............................. 24 Cancel ................................ 52 Use .................................... 14
Addition and aspiration tube Carry out ............................ 49 Karl Fischer titration
Mount ................................ 13 Result ................................. 56 Troubleshooting ................. 88
Adsorber tube Diagnosis ................................. 72 Keyboard
Fill ........................................ 9 Dialog language ....................... 62 Connect ............................. 24
Application bulletin .................. 31 Load ................................... 71 Key assignment ............ 93, 94
Dialog type ............................... 63 Keyboard layout ....................... 68
B Directory structure .................... 67 KFC
Backup ..................................... 66 Parameters ......................... 73
Balance .............................. 49, 92 E
Connect ............................. 22 Electrical connection L
Interface parameters ........... 69 Power Box .......................... 15 Language ................................. 62
Balance type ............................. 69 Power supply unit ............... 14 Language file
Electrode Load ................................... 71
C Connect ............................. 17 Live modifications ..................... 52
Calculation Electrode connector Live parameters ........................ 55
Method "Blank" .................. 84 Double Pt wire electrode ...... 7
Method "KFC-Blank" .......... 83 Generator electrode ............. 7 M
Method "KFC" .................... 82 Indicator electrode ............... 7 Mains connection ....................... 7
Numerical format ............. 103 Electrostatic charge .................... 4 Manual control
Rounding-off process ....... 103 End of Determination EOD ..... 100 Stirring ............................... 60
Catholyte Endpoint Method
Replace .............................. 34 Dependency ....................... 95 Delete ................................ 66
Common variable ..................... 65 Expert dialog ............................ 63 Export ................................ 42
Edit .................................... 65 Import ................................ 66
Common Variable F Save ................................... 41
Delete ................................ 65 Formula editor .......................... 39 Method examples
Set to invalid ...................... 65 Front of the instrument .............. 6 Karl Fischer oven ................ 97
Conditioning Method template
Parameters ......................... 73 G Load ................................... 40
Contrast ................................... 64 Generator electrode Molecular sieve
Control ..................................... 43 Fill ...................................... 12 Replace .............................. 10
Autostart ............................ 43 Graphics width ......................... 68 MSB
Sample table ...................... 43 Connector ............................ 7
Control parameters ................... 76 I Multiple determination
Control range Indicator electrode Statistics calculation ............ 85
Dependency ....................... 95 Warm-up time .................... 34
Coulometer Initialization .............................. 98 N
Set up .................................. 8 Instrument Navigate ................................... 37
Coulometry Set up .................................. 8 Numerical input ........................ 37
Drift ................................... 33 Switch off ........................... 35
Principle ............................. 28 Switch on ........................... 35 O
Sample size ........................ 31 Instrument diagnosis ................ 71 Operation
Tips for daily practice .......... 29 General .............................. 36
Water standard .................. 29 K Oven module ........................... 14
Working conditions ............ 33 Karl Fischer
Curve ....................................... 56 Coulometry ........................ 28

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P Result ....................................... 56 Stirrer

Parameters Recalculate ......................... 57 Connect ............................. 21
Calculation ......................... 81 Rounding-off process ....... 103 Stirring rate .............................. 92
Conditioning ...................... 73 Save as a common variable . 65 Stop conditions
Dependency ....................... 95 Result report Parameters ......................... 81
KFC .................................... 73 Define ................................ 86 Supply voltage ............................ 4
Modify live ......................... 55 Routine dialog .......................... 64 Switch off ................................. 35
Start conditions .................. 75 RS-232 Switch on ................................. 35
Stop conditions .................. 81 Interface parameters ........... 70 System initialization .................. 98
Titration ............................. 79 RS-232 connection ................. 101
PC/LIMS report ......................... 68 T
Pin assignment ......................... 99 S Temperature sensor
Polarization current Safety instructions ...................... 3 Connect ............................. 17
Dependency ....................... 95 Sample Text input ................................. 37
Preparation time Liquid ................................. 31 Titration cell
Generator electrode with dia- Solid ................................... 32 Equip .................................. 11
phragm .............................. 33 Sample changer Fill ...................................... 12
Generator electrode without Connect ............................. 27 Insert .................................... 9
diaphragm .......................... 33 With oven module .............. 14 Titration parameters ................. 79
Print ......................................... 59 Sample data Troubleshooting ....................... 88
Printer ................................ 68, 95 Enter .................................. 44
Connect ............................. 24 Modify live ......................... 52 U
Program crash .......................... 98 Sample size Update
Program version Send from a balance ..... 49, 92 Dialog language ................. 71
Update ............................... 71 Size .................................... 31 Program version ................. 71
Sample table ............................ 45 USB .......................................... 93
R Insert line ........................... 48 Numerical keypad ............... 93
Reagent replacement ................ 34 Load ................................... 47 PC keyboard ....................... 94
Rear of the instrument ................ 7 Modify live ......................... 53 PC mouse ........................... 95
Recalculate ............................... 56 Save ................................... 47 Printer ................................ 95
Remote Sensor USB (OTG)
Connector ............................ 7 Connect ............................. 17 Connector ............................ 7
Interface ............................. 99 Sensor connector USB device
Pin assignment ................... 99 Pt1000 ................................. 7 Adapter .............................. 24
Status diagram ................. 100 Temperature sensor .............. 7 Connect ............................. 24
Remote connector Service ....................................... 3 USB flash drive
Sample changer .................. 27 Start conditions Directory structure .............. 67
Remote control ...................... 101 Parameters ......................... 75 User name ................................ 62
Report Statistics ................................... 57
Print manually .................... 59 Statistics calculation .................. 85 W
Select ................................. 86 Water standard
Certified ............................. 29

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