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899 Coulometer: Manual

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0% found this document useful (0 votes)
435 views178 pages

899 Coulometer: Manual

Uploaded by

kaddouri
Copyright
© © All Rights Reserved
We take content rights seriously. If you suspect this is your content, claim it here.
Available Formats
Download as PDF, TXT or read online on Scribd
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899 Coulometer

Manual
8.899.8001EN
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 04.2012 ebe


Teachware
Metrohm AG
CH-9100 Herisau
[email protected]

This documentation is protected by copyright. All rights reserved.


Although all the information given in this documentation has been
checked with great care, errors cannot be entirely excluded. Should you
notice any mistakes please send us your comments using the address
given above.
Documentation in additional languages can be found on
http://products.metrohm.com under Literature/Technical documenta-
tion.
■■■■■■■■■■■■■■■■■■■■■■ 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 coulometer cell ............................................ 9
3.2.1 Inserting the coulometer cell .................................................... 9
3.2.2 Preparing the coulometer cell .................................................. 9
3.2.3 Mounting the addition and aspiration tube (utilization with Ti
Stand) ................................................................................... 13
3.2.4 Using the coulometer cell with a Karl Fischer oven ................. 14
3.2.5 Using the coulometer 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 .................................................. 32
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 Operation and maintenance 88


8.1 Quality Management and validation with Metrohm ....... 88

9 Troubleshooting 89
9.1 Karl Fischer titration .......................................................... 89
9.2 Miscellaneous ..................................................................... 91

10 Appendix 92
10.1 Stirring rate ......................................................................... 92
10.2 Balance ................................................................................ 92
10.3 USB devices ......................................................................... 93
10.3.1 6.2147.000 numerical USB keypad ........................................ 93
10.3.2 Key assignment of a USB keyboard ........................................ 94
10.3.3 PC mouse .............................................................................. 95

899 Coulometer ■■■■■■■■ V


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

10.3.4 Printer ................................................................................... 95


10.4 Control parameters and polarization current .................. 95
10.5 Method examples for working with the Karl Fischer
oven ..................................................................................... 97
10.6 System initialization ........................................................... 98
10.7 Remote interface ................................................................ 99
10.7.1 Pin assignment of the remote interface .................................. 99
10.7.2 Status diagram of the remote interface ................................ 100
10.8 Remote control via an RS-232 connection ..................... 101
10.8.1 Commands and variables ..................................................... 102
10.9 Arithmetic algorithms in the 899 Coulometer ............... 103

11 Technical specifications 106


11.1 Measuring inputs .............................................................. 106
11.1.1 Indicator electrode .............................................................. 106
11.1.2 Temperature ........................................................................ 106
11.2 Generator connector ........................................................ 106
11.2.1 Generator electrode ............................................................ 106
11.3 Internal stirrer ................................................................... 107
11.4 Interfaces and connectors ............................................... 107
11.5 Power supply .................................................................... 107
11.6 Safety specifications ........................................................ 108
11.7 Electromagnetic compatibility (EMC) ............................. 108
11.8 Ambient temperature ...................................................... 109
11.9 Reference conditions ........................................................ 109
11.10 Dimensions ........................................................................ 109

12 Warranty (Guarantee) 110


13 Accessories 112
13.1 Scope of delivery .............................................................. 112
13.1.1 2.899.0010 ......................................................................... 112
13.1.2 2.899.0110 ......................................................................... 119
13.1.3 2.899.1010 ......................................................................... 125
13.1.4 2.899.1110 ......................................................................... 132
13.1.5 2.899.2110 ......................................................................... 139
13.1.6 2.899.3110 ......................................................................... 152
13.2 Optional accessories ........................................................ 164

Index 167

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 coulometer cell ............................................................. 9
Figure 4 Filling the adsorber tube .................................................................. 10
Figure 5 Equipping the coulometer cell ......................................................... 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 general electrode ..................... 18
Figure 11 Connecting a generator electrode ................................................... 18
Figure 12 Unscrew the cover from the indicator electrode .............................. 19
Figure 13 Screwing on 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 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
available which are already configured except for a few parameters. The
methods can be modified and stored under a new name. The methods
can be exported to a connected USB flash drive. This function makes it
possible for you to copy methods quickly and easily from one instrument
to another.
The 899 Coulometer has an integrated magnetic stirrer that is visible on
the top side of the housing. The coulometer cell can easily be attached to
the magnetic stirrer. Thanks to its compact construction, you can use the
device in a small space as a stand-alone titrator. Furthermore, 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 power
supplies are either unstable or absent.

1.1.1 Connectors
The instrument is equipped with the following connectors:
■ Electrical connection
For connecting to the mains supply with the aid of the power supply
unit provided or for connection 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.

899 Coulometer ■■■■■■■■ 1


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

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

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. The usage of the 899 Coulometer therefore requires that the user
have basic knowledge and experience in the handling of toxic and caustic
substances. Knowledge with respect to the application of the fire preven-
tion 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 hazard
or risk of injury.

2 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 1 Introduction

Warning
This symbol draws attention to a possible hazard due
to electrical current.
Warning
This symbol draws attention to a possible hazard due
to heat or hot instrument parts.
Warning
This symbol draws attention to a possible biological
hazard.
Caution
This symbol draws attention to a possible damage of
instruments or instrument parts.
Note
This symbol marks additional information and tips.

1.3 Safety instructions


1.3.1 General notes on safety

Warning

This instrument may only be operated in accordance with the specifica-


tions in this documentation.

This instrument has left the factory in a flawless state in terms of technical
safety. To maintain this state and ensure non-hazardous operation of the
instrument, the following instructions must be observed carefully.

1.3.2 Electrical safety


The electrical safety when working with the instrument is ensured as part
of the international standard IEC 61010.

Warning

Only personnel qualified by Metrohm are authorized to carry out service


work on electronic components.

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.

Mains voltage

Warning

An incorrect mains voltage can damage the instrument.


Only operate this instrument with a mains voltage specified for it (see
rear panel of the instrument).

Protection against electrostatic charges

Warning

Electronic components are sensitive to electrostatic charges and can be


destroyed by discharges.
Do not fail to pull the mains cable out of the mains connection socket
before you set up or disconnect electrical plug connections at the rear
of the instrument.

1.3.3 Tubing and capillary connections

Caution

Leaks in tubing and capillary connections are a safety risk. Tighten all
connections well by hand. Avoid applying excessive force to tubing
connections. Damaged tubing ends lead to leakage. Appropriate tools
can be used to loosen connections.
Check the connections regularly for leakage. If the instrument is used
mainly in unattended operation, then weekly inspections are manda-
tory.

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. laboratory
flue).
■ Keep all sources of flame far from the workplace.
■ Clean up spilled fluids and solids immediately.
■ Follow the safety instructions of the chemical manufacturer.

1.3.5 Recycling and disposal


This product is covered by European Directive 2002/96/EC, WEEE – Waste
from Electrical and Electronic Equipment.
The correct disposal of your old equipment will help to prevent negative
effects on the environment and public health.
More details about the disposal of your old equipment can be obtained
from your local authorities, from waste disposal companies or from your
local dealer.

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 highly protective special packaging together
with the separately packed accessories. Keep this packaging, as only this
ensures safe transportation of the instrument.

3.1.2 Checks
Immediately after receipt, check whether the shipment has arrived com-
plete and without damage by comparing it with the delivery note.

3.1.3 Location
The instrument has been developed for operation indoors and may not be
used in explosive environments.
Place the instrument in a location of the laboratory which is suitable for
operation, free of vibrations, protected from corrosive atmosphere, and
contamination by chemicals.
The instrument should be protected against excessive temperature fluctu-
ations and direct sunlight.

8 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 3 Installation

3.2 Setting up the coulometer cell


3.2.1 Inserting the coulometer cell

6.1464.320

6.2047.030

Figure 3 Inserting the coulometer cell


Set up the coulometer 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 coulometer cell into the titration vessel holder.

3.2.2 Preparing the coulometer cell

Filling the adsorber tube

Before setting up the coulometer 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 coulometer cell ■■■■■■■■■■■■■■■■■■■■■■

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 the ¾ level.

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.

Note

Note that the molecular sieve must be replaced at regular intervals.


Each time you refill the adsorber tube with molecular sieve, you can, for
example, write the date directly on the adsorber tube.

10 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 3 Installation

Equipping the coulometer 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 coulometer cell


Equip the coulometer cell as follows:

1 Place the 6.1903.030 stirring bar in the coulometer 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.).
Take care to ensure that the edges of the ground-joint sleeves are
cut to size cleanly and that there are no fringes. The ground-joint
sleeves are not permitted to 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 coulometer cell ■■■■■■■■■■■■■■■■■■■■■■

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 coulome-


ter 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 coulometer 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 coulometer 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 coulometer cell (generator electrode without


diaphragm)

Proceed as follows when using a generator electrode without a dia-


phragm:

1 Fill approximately 100 mL of reagent into the coulometer 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 coulometer 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 everything together 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 coulometer 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 coulometer 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 guided with a carrier
gas into the coulometer cell. You will find recommended parameter set-
tings for determinations with a Karl Fischer oven in chapter 10.5, page
97.
A detailed description of setting up the coulometer cell with the KF oven
can be found in the respective manual.

3.2.5 Using the coulometer cell with a sample changer


When there is a large number of samples, 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 recommended para-
meter settings for determinations with a Karl Fischer oven in chapter 10.5,
page 97.
A detailed description of setting up the coulometer 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 two different ways:
■ Connect the coulometer directly to the mains supply with the aid of
the power supply unit provided.
■ Connect the coulometer to the 6.2164.500 Power Box if no stable
mains 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 mains connection of the Coulometer.

Warning

An incorrect mains voltage can damage the instrument.


Operate the instrument only with the mains 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 mains
connection (2-7) of the Coulometer.

Note

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 will first need to pull
back the outer plug sleeve.

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

Caution

Switch off the 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 supply from the mains supply, the option
exists of providing 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 mains 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 mains connection (2-7)
of the Coulometer.

Note

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 will first need to pull back the outer
plug sleeve.

Caution

Switch off the 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. Attach
corresponding markings on the screw heads of the cables.

3.4.1 Connecting a generator electrode

Screwing the electrode cable to the general electrode

1 Unscrew the cover of the generator electrode.

Figure 9 Unscrewing the cover from the generator electrode

2 Screw the 6.2104.120 electrode cable tightly onto the generator


electrode.

899 Coulometer ■■■■■■■■ 17


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

6.2104.120
2

Figure 10 Screwing the electrode cable to the general 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

Note

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 will first need to pull back the outer plug
sleeve.

3.4.2 Connecting an indicator electrode

Screwing on the electrode cable to the indicator electrode

1 Unscrew the cover of the indicator electrode.

18 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 3 Installation

Figure 12 Unscrew the cover from the indicator electrode

2 Screw the 6.2104.020 electrode cable tightly onto the indicator elec-
trode.

6.2104.020

Figure 13 Screwing on the electrode cable to the indicator elec-


trode

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 ■■■■■■■■■■■■■■■■■■■■■■

Note

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 will 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

Note

Always insert the red plug into the red socket. It is only this way that
the shielding against electrical interferences is 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

Note

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 con-
nect 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 either with via a USB hub or
using a 6.2151.100 USB MINI (OTG) - USB A adapter (see Chapter
3.7, page 24) on the Coulometer.

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


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

Note

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.

Note

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 connec-
ted. USB hubs are available in specialty stores in a number of different
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 10.3, 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 con-
ventional method works with a methanolic solution of iodine, sulfur diox-
ide 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
equation:

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 determina-
tion.
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 availa-
ble 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
For validating the instrument as a whole, integrated system, commercially
available, certified water standards with water contents of 1.00 ± 0.003
mg/g and/or 0.10 ± 0.005 mg/g should be used.

Note

The 1.0 mg/g water standard is easier to handle and therefore to be


preferred.

Table 1 Recommended sample sizes


Water standard 1.0 mg/g 0.2…2.0 g
Water standard 0.1 mg/g 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 with Karl Fischer titration).

2 Use a clean syringe.

Note

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 piston of the syringe up to the end and swing the syringe
back and forth somewhat.
The inside of the syringe is being rinsed by water standard and freed
from water contamination.

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
by hand, press [START] and inject approx. 1 mL of the water stand-
ard through the septum.
There are two possibilities:

13 ■ 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 coulometer cell.
or
■ 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 out of the reagent liquid.

14 Close the syringe with the same cap and place it back on the bal-
ance.

15 Read off the value displayed by the balance and enter it on the Coul-
ometer as the sample size.

30 ■■■■■■■■ 899 Coulometer


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

If you have connected a balance to the Coulometer, you may trans-


mit the sample size directly from the balance.

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


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

4.3 Sample addition


This chapter contains a few notes concerning sample addition. A com-
plete description of this topic is not possible here. Further notes can be
found in the publications from the reagent manufacturers and in the fol-
lowing Metrohm Application Bulletins:
Bulletin No. Title

No. 142 Karl Fischer water content determinations in gaseous samples

No. 145 The determination of small water contents in plastics

No. 209 Water content determinations in insulating oils, hydrocarbons and their
products

No. 273 Validation of KF coulometers according to GLP / ISO 9001

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 in order to keep
the titration time short. However, ensure that the sample contains at least
50 µg of H2O. The following table provides clues for the sample size.

Table 2 Recommended sample sizes


Content of the sample Sample size H2O, to be determined
(Water content)
10000 ppm = 1% 10 mg…100 mg 100 µg…1000 µg
1000 ppm = 0.1% 100 mg…1 g 100 µg…1000 µg
100 ppm = 0.01% 1g 100 µg
10 ppm = 0.001% 5g 50 µg

899 Coulometer ■■■■■■■■ 31


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

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.
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, however, must not be cooled directly, as condensates could form.
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 suita-
ble solvents. In this case the water content of the solvent has to be deter-
mined and subtracted as blank value.
Paste and fats can be added to the coulometer cell with a syringe with-
out 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 by reweighing the sam-
ple.
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 coulometer cell, then the gen-
erator 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

32 ■■■■■■■■ 899 Coulometer


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

■ 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.

4.4 Optimum working conditions


4.4.1 General
When a coulometer 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 coulometer cell be repeatedly and carefully shaken during this time.
For generator electrodes with diaphragm, you should expect a preparation
time of approx. 2 hours.
To obtain precise determinations of amounts of water smaller than 100
µg, it may also be of advantage to condition the coulometer cell overnight
before using it.
If the Coulometer is switched off for extended periods with the coulome-
ter 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, how-
ever, are quite possible. Higher but stable values will still produce good
results, because the drift can be compensated.
A constantly high drift can be caused by water-containing deposits in
inaccessible parts of the coulometer cell. In these cases, shaking the cell
can reduce the value. Ensure that there are no drops above the liquid level
in the coulometer cell.
If you are working with a generator electrode with diaphragm, shake the
cell only hard enough that the catholyte and anolyte do not 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 single-component reagent.

899 Coulometer ■■■■■■■■ 33


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

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.

4.4.3 Reagent replacement


The electrolyte solutions must be replaced in the following cases:
■ The coulometer cell is too full.
■ The KF reagent has reached its capacity limit.
■ The drift is too high, and cannot be reduced by shaking the coulometer
cell.
■ A two-phase-mixture is being formed in the coulometer cell; in this
case it is also possible to aspirate the sample phase only.
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 coulometer cell does not have to be disassem-
bled.
In the event of severe contamination, the coulometer cell can be rinsed
with a suitable solvent which is also aspirated.
In the case of the generator electrode with diaphragm, the catholyte
should be replaced once per week. Longer use can cause blackening and
yellow precipitates in the cathode chamber. A discernable stench 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 for forming
the surface. During this time unexpectedly long titration times and high
measurement results can occur. This phenomenon will, however, disap-
pear 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
process 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 10.3.2, 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:

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■■■■■■■■■■■■■■■■■■■■■■ 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.

Note

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.

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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

Note

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 vari-
ety 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 10.2, 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

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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
entering of the sample data is confirmed with [START], even if the the
titration is already completed. This ensures that the sample data is availa-
ble for calculations.

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.

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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.

Note

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.

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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.

Note

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:

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■■■■■■■■■■■■■■■■■■■■■■ 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.

Note

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.

Note

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].

Note

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.

54 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 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.

899 Coulometer ■■■■■■■■ 55


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.

56 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 5 Operation

Recalculating

Note

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.

Note

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.

899 Coulometer ■■■■■■■■ 57


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
determination 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.

899 Coulometer ■■■■■■■■ 59


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.

899 Coulometer ■■■■■■■■ 61


6.1 Basic settings ■■■■■■■■■■■■■■■■■■■■■■

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.

62 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 6 System settings

Note

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.

Note

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.

899 Coulometer ■■■■■■■■ 63


6.1 Basic settings ■■■■■■■■■■■■■■■■■■■■■■

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

Note

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 System settings

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].

899 Coulometer ■■■■■■■■ 65


6.3 File management ■■■■■■■■■■■■■■■■■■■■■■

■ 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.

Note

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

Note

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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■■■■■■■■■■■■■■■■■■■■■■ 6 System settings

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

Note

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.

899 Coulometer ■■■■■■■■ 67


6.4 Configuring external devices ■■■■■■■■■■■■■■■■■■■■■■

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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■■■■■■■■■■■■■■■■■■■■■■ 6 System settings

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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6.4 Configuring external devices ■■■■■■■■■■■■■■■■■■■■■■

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

Note

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 System settings

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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6.5 Instrument diagnosis ■■■■■■■■■■■■■■■■■■■■■■

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 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 star-
ted 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

Note

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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■■■■■■■■■■■■■■■■■■■■■■ 7 Parameters

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

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

Note

Note that the parameter Endpoint at is linked with the parameters


Dynamics and I(pol). Explanations in this connection can be found in
chapter 10.4 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.

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■■■■■■■■■■■■■■■■■■■■■■ 7 Parameters

This parameter defines the control range before the specified endpoint.
Within the control range, the iodine is generated step by step, the genera-
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.

Note

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 10.4 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

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

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

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.

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■■■■■■■■■■■■■■■■■■■■■■ 7 Parameters

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

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.

899 Coulometer ■■■■■■■■ 79


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

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.

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 10.1, 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

Note

Note that the parameter I(pol) is linked with the parameters Dynamics
and Endpoint at. Explanations in this connection can be found in
chapter 10.4 Control parameters and polarization current, page 95.

80 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 7 Parameters

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.
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.

899 Coulometer ■■■■■■■■ 81


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

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.

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

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■■■■■■■■■■■■■■■■■■■■■■ 7 Parameters

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 %
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

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

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 %
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).

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■■■■■■■■■■■■■■■■■■■■■■ 7 Parameters

Entry 30 characters
Default value empty

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

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

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.
If an additional determination has to be added to the determination ser-
ies, 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 (see Chapter 10.9, page 103). If Statistics has been activa-
ted, 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

86 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 7 Parameters

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.
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

899 Coulometer ■■■■■■■■ 87


8.1 Quality Management and validation with Metrohm ■■■■■■■■■■■■■■■■■■■■■■

8 Operation and maintenance

8.1 Quality Management and validation with Metrohm


Quality Management
Metrohm offers you comprehensive support in implementing quality man-
agement measures for instruments and software. Further information on
this can be found in the brochure «Quality Management with
Metrohm» available from your local Metrohm agent.

Validation
Please contact your local Metrohm agent for support in validating instru-
ments and software. Here you can also obtain validation documentation
to provide help for carrying out the Installation Qualification (IQ) and
the Operational Qualification (OQ). IQ and OQ are also offered as a
service by the Metrohm agents. In addition, various application bulletins
are also available on the subject, which also contain Standard Operat-
ing Procedures (SOP) for testing analytical measuring instruments for
reproducibility and correctness.

Maintenance
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 agent regarding the
precise terms and conditions involved in concluding a corresponding
maintenance agreement.

Note

You can find information on the subjects of quality management, vali-


dation and maintenance as well as an overview of the documents cur-
rently available at www.metrohm.com/com/ under Support.

88 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 9 Troubleshooting

9 Troubleshooting
9.1 Karl Fischer titration
Problem Cause Remedy
The drift is very high The coulometer cell is not ■ Check the septum and replace it if neces-
during conditioning. leak-proof. sary.
■ Replace the molecular sieve.
■ Check the ground-joint sleeves for frayed
edges. If necessary, trim the edges cleanly
or replace the ground-joint sleeves.

Aqueous deposits are to be ■ Shake the coulometer cell.


found in the coulometer
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 single-compo-
nent reagent.

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

A side reaction is taking ■ Possibly use 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 coulometer with the oven method with sample vials,
cell is too high. set the gas flow between 40…60 mL/min).

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

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.

899 Coulometer ■■■■■■■■ 89


9.1 Karl Fischer titration ■■■■■■■■■■■■■■■■■■■■■■

Problem Cause Remedy


The Control parameters ■ Reset the Control parameters to default
are not set correctly. 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 coulometer cell is not ■ Shake the coulometer cell and wait until
high. yet correctly conditioned. the drift is stable.

The sample contains oxi- ■ Possibly use 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. with the use of still exists between the conditioning vial
a KF oven or with manual and the coulometer cell.
drift correction). ■ Set the parameter Drift correction to
auto (= automatic drift correction).

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

The parameter Stop drift ■ Set the Stop drift lower.


is set too high.

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).

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■■■■■■■■■■■■■■■■■■■■■■ 9 Troubleshooting

Problem Cause Remedy


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 ■ Observe the instructions in chapter 4.3,


poorly reproducible. page 31.

The drift fluctuates. ■ Ensure stable drift.

9.2 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 hub on the USB connector and con-
nect the printer to the hub.

The printer model is not Use a printer which fulfills the required specifi-
compatible. cations (see Chapter 10.3.4, 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 hub on the USB connector and con-
nect the keyboard or mouse to the hub.

The keyboard or the mouse Use a model which fulfills the required specifi-
is not compatible. cations (see Chapter 10.3, 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.

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
ble" is displayed. on again.

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

899 Coulometer ■■■■■■■■ 91


10.1 Stirring rate ■■■■■■■■■■■■■■■■■■■■■■

10 Appendix

10.1 Stirring rate


The stirring rate can be adjusted in steps of –15 to +15.
The approximate rotational speed can be calculated with the following
formula:

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

Example:
Stirring rate set: 8
Rotational speed in rpm = 125 · 8 = 1000
r/min

2000

1500

1000

500

-15 -10 -5 0 5 10 15
Figure 25 Rotational speed depending on stirring rate

10.2 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 charac-
ters (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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■■■■■■■■■■■■■■■■■■■■■■ 10 Appendix

Note

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

10.3 USB devices

Note

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.

10.3.1 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]

899 Coulometer ■■■■■■■■ 93


10.3 USB devices ■■■■■■■■■■■■■■■■■■■■■■

Key of the 899 Coulometer or Key on the numerical USB


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

10.3.2 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]

Note

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

94 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 10 Appendix

10.3.3 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

10.3.4 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

Note

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.

10.4 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)

899 Coulometer ■■■■■■■■ 95


10.4 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.

96 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 10 Appendix

10.5 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.

899 Coulometer ■■■■■■■■ 97


10.6 System initialization ■■■■■■■■■■■■■■■■■■■■■■

10.6 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.

98 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 10 Appendix

3 Confirming the initialization

Note

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.

10.7 Remote interface


10.7.1 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

899 Coulometer ■■■■■■■■ 99


10.7 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

10.7.2 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

100 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 10 Appendix

10.8 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.

899 Coulometer ■■■■■■■■ 101


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

10.8.1 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. Exam-
ple:
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').

102 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 10 Appendix

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

10.9 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 min-
imal 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

899 Coulometer ■■■■■■■■ 103


10.9 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) calcula-
ted 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.

104 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 10 Appendix

Note

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


11.1 Measuring inputs ■■■■■■■■■■■■■■■■■■■■■■

11 Technical specifications

11.1 Measuring inputs


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

11.1.1 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 typical: 5, 10, 20 and 30 µA
current

11.1.2 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.)

11.2 Generator connector


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

11.2.1 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

106 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 11 Technical specifications

11.3 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

11.4 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.

11.5 Power supply


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

899 Coulometer ■■■■■■■■ 107


11.6 Safety specifications ■■■■■■■■■■■■■■■■■■■■■■

11.6 Safety specifications


This instrument fulfills the following electrical safety requirements:
CE designation in accordance with the EU directives:
■ 2006/95/EC (Low Voltage Directive, LVD)
■ 2004/108/EC (EMC Directive, EMC)

Design and testing According to EN/IEC/UL 61010-1, CSA-C22.2 No. 61010-1, protection
class III (external power supply unit).
Safety instructions This document contains safety instructions which have to be followed
by the user in order to ensure safe operation of the instrument.

11.7 Electromagnetic compatibility (EMC)


Emission
Standards fulfil- ■ EN/IEC 61326-1
led ■ EN/IEC 61000-6-3
■ EN 55011 / CISPR 11

Immunity
Standards fulfil- ■ EN/IEC 61326-1
led ■ EN/IEC 61000-6-2
■ EN/IEC 61000-4-2
■ EN/IEC 61000-4-3
■ EN/IEC 61000-4-4
■ EN/IEC 61000-4-5
■ EN/IEC 61000-4-6
■ EN/IEC 61000-4-11
■ EN/IEC 61000-4-14
■ EN/IEC 61000-4-28
■ NAMUR

108 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 11 Technical specifications

11.8 Ambient temperature


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

11.9 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

11.10 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

899 Coulometer ■■■■■■■■ 109


■■■■■■■■■■■■■■■■■■■■■■

12 Warranty (Guarantee)
Metrohm guarantees that the deliveries and services it provides are free of
errors in materials, design or manufacturing.
The general warranty period is 36 months (exclusions below) from the
date of delivery or 18 months in the event of continuous operation. The
warranty remains valid on the condition that the service is provided by an
authorized Metrohm Service Organization at defined intervals and with a
defined scope.
The warranty period for the suppressors "MSM II" and "MSM-HC" is 120
months from the date of delivery or 60 months in the event of continuous
operation.
The warranty period for IC separation columns is 12 months from the date
of delivery or 6 months in the event of continuous operation. The techni-
cal specifications contained in the manual are authoritative for warranty of
accuracy.
For third-party components that are recognizable as such, the manufac-
turer's warranty regulations apply.
Consumables and materials with limited storage life and glass breakage in
the case of electrodes or other glass parts are excluded from the warranty.
Warranty claims cannot be asserted if the customer has failed to meet his
payment obligations according to schedule.
During the warranty period, Metrohm undertakes either to replace free of
charge or to credit the purchaser for any instruments, assemblies or com-
ponents that can be shown to be faulty. Any transport or customs fees
that may apply are the ordering party’s responsibility.
The precondition for this is that the ordering party must use the Return
Material Authorization (RMA) to report the faulty part, along with specifi-
cation of the article number, the article designation, an adequate error
description, the delivery date and (if applicable) the serial number. In addi-
tion, the ordering party undertakes to store the faulty part for at least 2
years in accordance with current storage directives (in compliance with
ESD guidelines) and to hold it in readiness for onsite inspection or for
return shipment to Metrohm. Metrohm reserves the right to invoice the
ordering party for these articles, including retroactively, in the event of
noncompliance with these pre-conditions.
Deficiencies arising from circumstances that are not the responsibility of
Metrohm, such as improper storage or improper use, etc. are expressly
excluded from the warranty.

110 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 12 Warranty (Guarantee)

Metrohm also offers a 120-month spare parts warranty and a 5-year PC


software support warranty, calculated from the date on which the prod-
uct is withdrawn from the market. The content of this warranty is the abil-
ity of the customer to obtain functioning spare parts or appropriate soft-
ware support at market prices during the time of the warranty period.
If Metrohm AG is unable to meet this obligation due to circumstances
beyond the control of Metrohm AG, then the ordering party shall be
offered alternative solutions at preferential conditions.

899 Coulometer ■■■■■■■■ 111


13.1 Scope of delivery ■■■■■■■■■■■■■■■■■■■■■■

13 Accessories
Note

Subject to change without notice.

13.1 Scope of delivery


13.1.1 2.899.0010

Qty. Order no. Description


1.0 1.899.0010 899 Coulometer
1.0 6.0341.100 Double Pt wire electrode for coulometry
Double platinum wire electrode (0.8 x 4 mm), standard ground-joint,
Metrohm plug-in head G, for Karl Fischer titrations.
Shaft material: Glass
Measuring range: –2000…2000
Measuring unit: mV
Temp. continuous (°C): –20…70
Temp. short-term. (°C): –20…70
SGJ sleeve: Standard ground-joint 14/15
Shaft diameter top (mm): 12
Shaft diameter bottom (mm): 8.75
Minimum immersion depth 10
(mm):
Electrode plug-in head: Metrohm plug-in head G
Indicator electrode type: Pt
Indicator electrode shape: Wire

1.0 6.0344.100 Generator electrode with diaphragm


Generator electrode for Karl Fischer titrations, with diaphragm,
standard ground-joint 29/22.
Shaft material: Glass
Temp. continuous (°C): –20…70
Temp. short-term. (°C): –20…70
SGJ sleeve: Standard ground-joint 29/22
Shaft diameter top (mm): 24
Shaft diameter bottom (mm): 24
Minimum immersion depth 15
(mm):

112 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 13 Accessories

Qty. Order no. Description


Electrode plug-in head: Metrohm plug-in head G
Indicator electrode type: Cathode = Pt grid
Indicator electrode type (ref- Anode = Pt grid
erence):
1.0 6.1403.030 KF adsorber tube for coulometer cell
For KF coulometers.
Height (mm): 93
SGJ size: B-17/19

1.0 6.1437.000 Ground-joint stopper SGJ 14


Material: Glass
Height (mm): 34
SGJ size: B-14/15

2.0 6.1448.020 Septum / 16 mm / 5 pieces


Set of 5 pieces.
Material: Silicone rubber
Height (mm): 2
Outer diameter (mm): 16

899 Coulometer ■■■■■■■■ 113


13.1 Scope of delivery ■■■■■■■■■■■■■■■■■■■■■■

Qty. Order no. Description


1.0 6.1464.320 KF titration vessel / 80 - 250 mL / coulomet-
ric
Material: Clear glass
Height (mm): 114
Volume (mL): 80…250

1.0 6.1903.030 Stirring bar / 25 mm


Stirring bar with magnetic core, PTFE covering, length 25 mm.
Material: PTFE
Outer diameter (mm): 5
Length (mm): 25

1.0 6.2047.030 Titration vessel holder


1.0 6.2103.130 Adapter red plug 2 mm / 4 mm socket
For connecting plug B (4 mm) to socket 2 mm.

114 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 13 Accessories

Qty. Order no. Description


1.0 6.2103.140 Adapter black plug 2 mm / socket B 4 mm
For connecting plug B (4 mm) to socket 2 mm.

1.0 6.2104.020 Electrode cable / 1 m / F


For connecting electrodes with Metrohm plug-in head G to Metrohm
instruments (socket F).
Length (m): 1

1.0 6.2104.120 Electrode cable / 1 m / H


With plug H. For the connection generator electrode - KF coulome-
ter.
Length (m): 1

1.0 6.2151.100 Adapter USB Mini (OTG) - USB A


For connecting USB instruments.

1.0 6.2164.010 Power supply unit 100 - 240 V/24 V DC

899 Coulometer ■■■■■■■■ 115


13.1 Scope of delivery ■■■■■■■■■■■■■■■■■■■■■■

Qty. Order no. Description


1.0 6.2701.040 Screw cap
With a hole for the 6.1448.020 septum. For the 6.1464.32X and
6.1465.320 titration vessels.
Material: PBT
Height (mm): 20
Outer diameter (mm): 24
Inner diameter (mm): 18

3.0 6.2713.000 Sleeve


For the fat-free ground-joint connection with the standard ground-
joint SGJ 14.
Material: PTFE film

1.0 6.2713.010 Sleeve


Sleeve for the fat-free ground-joint connection with the standard
ground-joint SGJ 29.
Material: PTFE film

1.0 6.2713.020 Sleeve


For the fat-free ground-joint connection with the standard ground-
joint SGJ 19.
Material: PTFE film

1.0 6.2723.310 Protective cover


Protective cover for display and keypad for all instruments of the
Titrino plus family. Suitable for: 848 Titrino plus, 862 Compact Titro-
sampler, 863 Compact Autosampler, 865 Dosimat plus, 869 Com-
pact Sample Changer, 870 KF Titrino plus, 876 Dosimat plus, 877
Titrino plus, 899 Coulometer.
Material: PVC

116 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 13 Accessories

Qty. Order no. Description


1.0 6.2738.000 Funnel
For the KF coulometer.
Material: PP
Outer diameter (mm): 50
Inner diameter (mm): 6

1.0 6.2811.000 Molecular sieve


Molecular sieve. Bottle containing 250 g. Pore size: 0.3 nm. Without
moisture indicator. For Rancimats and Karl Fischer instruments.

2.0 6.2816.030 Needle with Luer connector


Outer diameter (mm): 0.8
Length (mm): 80

899 Coulometer ■■■■■■■■ 117


13.1 Scope of delivery ■■■■■■■■■■■■■■■■■■■■■■

Qty. Order no. Description


2.0 6.2816.090 Syringe 5 mL
Syringe 5 mL, PP, with Luer connector.
Material: PP

1.0 6.6063.900 tiBase 1.0 Demo CD


Demo CD for tiBase. Test version for 30 days.

1.0 6.2147.000 Numerical USB keypad


Numerical USB keypad for Titrino plus, Dosimat plus, 862 Compact
Titrosampler, 869 Compact Sample Changer, 863 Compact Auto-
sampler and 899 Coulometer. Including USB hub with two connec-
tors.

1 6.2122.0x0 Mains cable with C13 line socket


IEC-60320-C13
Cable plug according to customer requirements.
Switzerland: Type SEV 12
6.2122.020
Germany, …: Type CEE(7), VII
6.2122.040
USA, …: Type NEMA/ASA
6.2122.070

1 8.899.8002DE Manual – Short Instructions 899 Coulometer

118 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 13 Accessories

13.1.2 2.899.0110

Qty. Order no. Description


1.0 1.899.0010 899 Coulometer
1.0 6.0341.100 Double Pt wire electrode for coulometry
Double platinum wire electrode (0.8 x 4 mm), standard ground-joint,
Metrohm plug-in head G, for Karl Fischer titrations.
Shaft material: Glass
Measuring range: –2000…2000
Measuring unit: mV
Temp. continuous (°C): –20…70
Temp. short-term. (°C): –20…70
SGJ sleeve: Standard ground-joint 14/15
Shaft diameter top (mm): 12
Shaft diameter bottom (mm): 8.75
Minimum immersion depth 10
(mm):
Electrode plug-in head: Metrohm plug-in head G
Indicator electrode type: Pt
Indicator electrode shape: Wire

1.0 6.0345.100 Generator electrode without diaphragm


Generator electrode for Karl Fischer titrations, without diaphragm,
standard ground-joint 29/22.
Shaft material: Glass
Temp. continuous (°C): –20…70
Temp. short-term. (°C): –20…70
SGJ sleeve: Standard ground-joint 29/22
Shaft diameter top (mm): 24
Shaft diameter bottom (mm): 24
Minimum immersion depth 15
(mm):
Electrode plug-in head: Metrohm plug-in head G
Indicator electrode type: Cathode = Pt sheet
Indicator electrode type (ref- Anode = Pt grid
erence):

899 Coulometer ■■■■■■■■ 119


13.1 Scope of delivery ■■■■■■■■■■■■■■■■■■■■■■

Qty. Order no. Description


1.0 6.1403.030 KF adsorber tube for coulometer cell
For KF coulometers.
Height (mm): 93
SGJ size: B-17/19

1.0 6.1437.000 Ground-joint stopper SGJ 14


Material: Glass
Height (mm): 34
SGJ size: B-14/15

2.0 6.1448.020 Septum / 16 mm / 5 pieces


Set of 5 pieces.
Material: Silicone rubber
Height (mm): 2
Outer diameter (mm): 16

1.0 6.1464.320 KF titration vessel / 80 - 250 mL / coulomet-


ric
Material: Clear glass
Height (mm): 114
Volume (mL): 80…250

120 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 13 Accessories

Qty. Order no. Description


1.0 6.1903.030 Stirring bar / 25 mm
Stirring bar with magnetic core, PTFE covering, length 25 mm.
Material: PTFE
Outer diameter (mm): 5
Length (mm): 25

1.0 6.2047.030 Titration vessel holder


1.0 6.2103.130 Adapter red plug 2 mm / 4 mm socket
For connecting plug B (4 mm) to socket 2 mm.

1.0 6.2103.140 Adapter black plug 2 mm / socket B 4 mm


For connecting plug B (4 mm) to socket 2 mm.

899 Coulometer ■■■■■■■■ 121


13.1 Scope of delivery ■■■■■■■■■■■■■■■■■■■■■■

Qty. Order no. Description


1.0 6.2104.020 Electrode cable / 1 m / F
For connecting electrodes with Metrohm plug-in head G to Metrohm
instruments (socket F).
Length (m): 1

1.0 6.2104.120 Electrode cable / 1 m / H


With plug H. For the connection generator electrode - KF coulome-
ter.
Length (m): 1

1.0 6.2151.100 Adapter USB Mini (OTG) - USB A


For connecting USB instruments.

1.0 6.2164.010 Power supply unit 100 - 240 V/24 V DC


1.0 6.2701.040 Screw cap
With a hole for the 6.1448.020 septum. For the 6.1464.32X and
6.1465.320 titration vessels.
Material: PBT
Height (mm): 20
Outer diameter (mm): 24
Inner diameter (mm): 18

3.0 6.2713.000 Sleeve


For the fat-free ground-joint connection with the standard ground-
joint SGJ 14.
Material: PTFE film

122 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 13 Accessories

Qty. Order no. Description


1.0 6.2713.010 Sleeve
Sleeve for the fat-free ground-joint connection with the standard
ground-joint SGJ 29.
Material: PTFE film

1.0 6.2713.020 Sleeve


For the fat-free ground-joint connection with the standard ground-
joint SGJ 19.
Material: PTFE film

1.0 6.2723.310 Protective cover


Protective cover for display and keypad for all instruments of the
Titrino plus family. Suitable for: 848 Titrino plus, 862 Compact Titro-
sampler, 863 Compact Autosampler, 865 Dosimat plus, 869 Com-
pact Sample Changer, 870 KF Titrino plus, 876 Dosimat plus, 877
Titrino plus, 899 Coulometer.
Material: PVC

1.0 6.2738.000 Funnel


For the KF coulometer.
Material: PP
Outer diameter (mm): 50
Inner diameter (mm): 6

899 Coulometer ■■■■■■■■ 123


13.1 Scope of delivery ■■■■■■■■■■■■■■■■■■■■■■

Qty. Order no. Description


1.0 6.2811.000 Molecular sieve
Molecular sieve. Bottle containing 250 g. Pore size: 0.3 nm. Without
moisture indicator. For Rancimats and Karl Fischer instruments.

2.0 6.2816.030 Needle with Luer connector


Outer diameter (mm): 0.8
Length (mm): 80

2.0 6.2816.090 Syringe 5 mL


Syringe 5 mL, PP, with Luer connector.
Material: PP

1.0 6.6063.900 tiBase 1.0 Demo CD


Demo CD for tiBase. Test version for 30 days.

124 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 13 Accessories

Qty. Order no. Description


1.0 6.2147.000 Numerical USB keypad
Numerical USB keypad for Titrino plus, Dosimat plus, 862 Compact
Titrosampler, 869 Compact Sample Changer, 863 Compact Auto-
sampler and 899 Coulometer. Including USB hub with two connec-
tors.

1 6.2122.0x0 Mains cable with C13 line socket


IEC-60320-C13
Cable plug according to customer requirements.
Switzerland: Type SEV 12
6.2122.020
Germany, …: Type CEE(7), VII
6.2122.040
USA, …: Type NEMA/ASA
6.2122.070

1 8.899.8002DE Manual – Short Instructions 899 Coulometer

13.1.3 2.899.1010

Qty. Order no. Description


1.0 1.141.0100 USB thermal printer Neo's
1.0 1.899.0010 899 Coulometer
1.0 6.0341.100 Double Pt wire electrode for coulometry
Double platinum wire electrode (0.8 x 4 mm), standard ground-joint,
Metrohm plug-in head G, for Karl Fischer titrations.
Shaft material: Glass
Measuring range: –2000…2000
Measuring unit: mV
Temp. continuous (°C): –20…70
Temp. short-term. (°C): –20…70
SGJ sleeve: Standard ground-joint 14/15
Shaft diameter top (mm): 12
Shaft diameter bottom (mm): 8.75
Minimum immersion depth 10
(mm):
Electrode plug-in head: Metrohm plug-in head G

899 Coulometer ■■■■■■■■ 125


13.1 Scope of delivery ■■■■■■■■■■■■■■■■■■■■■■

Qty. Order no. Description


Indicator electrode type: Pt
Indicator electrode shape: Wire

1.0 6.0344.100 Generator electrode with diaphragm


Generator electrode for Karl Fischer titrations, with diaphragm,
standard ground-joint 29/22.
Shaft material: Glass
Temp. continuous (°C): –20…70
Temp. short-term. (°C): –20…70
SGJ sleeve: Standard ground-joint 29/22
Shaft diameter top (mm): 24
Shaft diameter bottom (mm): 24
Minimum immersion depth 15
(mm):
Electrode plug-in head: Metrohm plug-in head G
Indicator electrode type: Cathode = Pt grid
Indicator electrode type (ref- Anode = Pt grid
erence):
1.0 6.1403.030 KF adsorber tube for coulometer cell
For KF coulometers.
Height (mm): 93
SGJ size: B-17/19

1.0 6.1437.000 Ground-joint stopper SGJ 14


Material: Glass
Height (mm): 34
SGJ size: B-14/15

126 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 13 Accessories

Qty. Order no. Description


2.0 6.1448.020 Septum / 16 mm / 5 pieces
Set of 5 pieces.
Material: Silicone rubber
Height (mm): 2
Outer diameter (mm): 16

1.0 6.1464.320 KF titration vessel / 80 - 250 mL / coulomet-


ric
Material: Clear glass
Height (mm): 114
Volume (mL): 80…250

1.0 6.1903.030 Stirring bar / 25 mm


Stirring bar with magnetic core, PTFE covering, length 25 mm.
Material: PTFE
Outer diameter (mm): 5
Length (mm): 25

1.0 6.2047.030 Titration vessel holder

899 Coulometer ■■■■■■■■ 127


13.1 Scope of delivery ■■■■■■■■■■■■■■■■■■■■■■

Qty. Order no. Description


1.0 6.2103.130 Adapter red plug 2 mm / 4 mm socket
For connecting plug B (4 mm) to socket 2 mm.

1.0 6.2103.140 Adapter black plug 2 mm / socket B 4 mm


For connecting plug B (4 mm) to socket 2 mm.

1.0 6.2104.020 Electrode cable / 1 m / F


For connecting electrodes with Metrohm plug-in head G to Metrohm
instruments (socket F).
Length (m): 1

1.0 6.2104.120 Electrode cable / 1 m / H


With plug H. For the connection generator electrode - KF coulome-
ter.
Length (m): 1

128 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 13 Accessories

Qty. Order no. Description


1.0 6.2151.100 Adapter USB Mini (OTG) - USB A
For connecting USB instruments.

1.0 6.2151.120 Cable USB MINI (OTG) - USB B, 1.8 m


For connecting USB instruments.

1.0 6.2164.010 Power supply unit 100 - 240 V/24 V DC


1.0 6.2701.040 Screw cap
With a hole for the 6.1448.020 septum. For the 6.1464.32X and
6.1465.320 titration vessels.
Material: PBT
Height (mm): 20
Outer diameter (mm): 24
Inner diameter (mm): 18

3.0 6.2713.000 Sleeve


For the fat-free ground-joint connection with the standard ground-
joint SGJ 14.
Material: PTFE film

1.0 6.2713.010 Sleeve


Sleeve for the fat-free ground-joint connection with the standard
ground-joint SGJ 29.
Material: PTFE film

899 Coulometer ■■■■■■■■ 129


13.1 Scope of delivery ■■■■■■■■■■■■■■■■■■■■■■

Qty. Order no. Description


1.0 6.2713.020 Sleeve
For the fat-free ground-joint connection with the standard ground-
joint SGJ 19.
Material: PTFE film

1.0 6.2723.310 Protective cover


Protective cover for display and keypad for all instruments of the
Titrino plus family. Suitable for: 848 Titrino plus, 862 Compact Titro-
sampler, 863 Compact Autosampler, 865 Dosimat plus, 869 Com-
pact Sample Changer, 870 KF Titrino plus, 876 Dosimat plus, 877
Titrino plus, 899 Coulometer.
Material: PVC

1.0 6.2738.000 Funnel


For the KF coulometer.
Material: PP
Outer diameter (mm): 50
Inner diameter (mm): 6

1.0 6.2811.000 Molecular sieve


Molecular sieve. Bottle containing 250 g. Pore size: 0.3 nm. Without
moisture indicator. For Rancimats and Karl Fischer instruments.

130 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 13 Accessories

Qty. Order no. Description


2.0 6.2816.030 Needle with Luer connector
Outer diameter (mm): 0.8
Length (mm): 80

2.0 6.2816.090 Syringe 5 mL


Syringe 5 mL, PP, with Luer connector.
Material: PP

1.0 6.6063.900 tiBase 1.0 Demo CD


Demo CD for tiBase. Test version for 30 days.

4.0 6.9001.050 Thermal paper for USB thermal printer


Neo's
10-year guaranteed legibility with correct storage.
Width (mm): 60
Length (m): 25

899 Coulometer ■■■■■■■■ 131


13.1 Scope of delivery ■■■■■■■■■■■■■■■■■■■■■■

Qty. Order no. Description


1.0 6.2147.000 Numerical USB keypad
Numerical USB keypad for Titrino plus, Dosimat plus, 862 Compact
Titrosampler, 869 Compact Sample Changer, 863 Compact Auto-
sampler and 899 Coulometer. Including USB hub with two connec-
tors.

1 6.2122.0x0 Mains cable with C13 line socket


IEC-60320-C13
Cable plug according to customer requirements.
Switzerland: Type SEV 12
6.2122.020
Germany, …: Type CEE(7), VII
6.2122.040
USA, …: Type NEMA/ASA
6.2122.070

1 8.899.8002DE Manual – Short Instructions 899 Coulometer

13.1.4 2.899.1110

Qty. Order no. Description


1.0 1.141.0100 USB thermal printer Neo's
1.0 1.899.0010 899 Coulometer
1.0 6.0341.100 Double Pt wire electrode for coulometry
Double platinum wire electrode (0.8 x 4 mm), standard ground-joint,
Metrohm plug-in head G, for Karl Fischer titrations.
Shaft material: Glass
Measuring range: –2000…2000
Measuring unit: mV
Temp. continuous (°C): –20…70
Temp. short-term. (°C): –20…70
SGJ sleeve: Standard ground-joint 14/15
Shaft diameter top (mm): 12
Shaft diameter bottom (mm): 8.75
Minimum immersion depth 10
(mm):
Electrode plug-in head: Metrohm plug-in head G

132 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 13 Accessories

Qty. Order no. Description


Indicator electrode type: Pt
Indicator electrode shape: Wire

1.0 6.0345.100 Generator electrode without diaphragm


Generator electrode for Karl Fischer titrations, without diaphragm,
standard ground-joint 29/22.
Shaft material: Glass
Temp. continuous (°C): –20…70
Temp. short-term. (°C): –20…70
SGJ sleeve: Standard ground-joint 29/22
Shaft diameter top (mm): 24
Shaft diameter bottom (mm): 24
Minimum immersion depth 15
(mm):
Electrode plug-in head: Metrohm plug-in head G
Indicator electrode type: Cathode = Pt sheet
Indicator electrode type (ref- Anode = Pt grid
erence):
1.0 6.1403.030 KF adsorber tube for coulometer cell
For KF coulometers.
Height (mm): 93
SGJ size: B-17/19

1.0 6.1437.000 Ground-joint stopper SGJ 14


Material: Glass
Height (mm): 34
SGJ size: B-14/15

899 Coulometer ■■■■■■■■ 133


13.1 Scope of delivery ■■■■■■■■■■■■■■■■■■■■■■

Qty. Order no. Description


2.0 6.1448.020 Septum / 16 mm / 5 pieces
Set of 5 pieces.
Material: Silicone rubber
Height (mm): 2
Outer diameter (mm): 16

1.0 6.1464.320 KF titration vessel / 80 - 250 mL / coulomet-


ric
Material: Clear glass
Height (mm): 114
Volume (mL): 80…250

1.0 6.1903.030 Stirring bar / 25 mm


Stirring bar with magnetic core, PTFE covering, length 25 mm.
Material: PTFE
Outer diameter (mm): 5
Length (mm): 25

1.0 6.2047.030 Titration vessel holder

134 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 13 Accessories

Qty. Order no. Description


1.0 6.2103.130 Adapter red plug 2 mm / 4 mm socket
For connecting plug B (4 mm) to socket 2 mm.

1.0 6.2103.140 Adapter black plug 2 mm / socket B 4 mm


For connecting plug B (4 mm) to socket 2 mm.

1.0 6.2104.020 Electrode cable / 1 m / F


For connecting electrodes with Metrohm plug-in head G to Metrohm
instruments (socket F).
Length (m): 1

1.0 6.2104.120 Electrode cable / 1 m / H


With plug H. For the connection generator electrode - KF coulome-
ter.
Length (m): 1

899 Coulometer ■■■■■■■■ 135


13.1 Scope of delivery ■■■■■■■■■■■■■■■■■■■■■■

Qty. Order no. Description


1.0 6.2151.100 Adapter USB Mini (OTG) - USB A
For connecting USB instruments.

1.0 6.2151.120 Cable USB MINI (OTG) - USB B, 1.8 m


For connecting USB instruments.

1.0 6.2164.010 Power supply unit 100 - 240 V/24 V DC


1.0 6.2701.040 Screw cap
With a hole for the 6.1448.020 septum. For the 6.1464.32X and
6.1465.320 titration vessels.
Material: PBT
Height (mm): 20
Outer diameter (mm): 24
Inner diameter (mm): 18

3.0 6.2713.000 Sleeve


For the fat-free ground-joint connection with the standard ground-
joint SGJ 14.
Material: PTFE film

1.0 6.2713.010 Sleeve


Sleeve for the fat-free ground-joint connection with the standard
ground-joint SGJ 29.
Material: PTFE film

136 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 13 Accessories

Qty. Order no. Description


1.0 6.2713.020 Sleeve
For the fat-free ground-joint connection with the standard ground-
joint SGJ 19.
Material: PTFE film

1.0 6.2723.310 Protective cover


Protective cover for display and keypad for all instruments of the
Titrino plus family. Suitable for: 848 Titrino plus, 862 Compact Titro-
sampler, 863 Compact Autosampler, 865 Dosimat plus, 869 Com-
pact Sample Changer, 870 KF Titrino plus, 876 Dosimat plus, 877
Titrino plus, 899 Coulometer.
Material: PVC

1.0 6.2738.000 Funnel


For the KF coulometer.
Material: PP
Outer diameter (mm): 50
Inner diameter (mm): 6

1.0 6.2811.000 Molecular sieve


Molecular sieve. Bottle containing 250 g. Pore size: 0.3 nm. Without
moisture indicator. For Rancimats and Karl Fischer instruments.

899 Coulometer ■■■■■■■■ 137


13.1 Scope of delivery ■■■■■■■■■■■■■■■■■■■■■■

Qty. Order no. Description


2.0 6.2816.030 Needle with Luer connector
Outer diameter (mm): 0.8
Length (mm): 80

2.0 6.2816.090 Syringe 5 mL


Syringe 5 mL, PP, with Luer connector.
Material: PP

1.0 6.6063.900 tiBase 1.0 Demo CD


Demo CD for tiBase. Test version for 30 days.

4.0 6.9001.050 Thermal paper for USB thermal printer


Neo's
10-year guaranteed legibility with correct storage.
Width (mm): 60
Length (m): 25

138 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 13 Accessories

Qty. Order no. Description


1.0 6.2147.000 Numerical USB keypad
Numerical USB keypad for Titrino plus, Dosimat plus, 862 Compact
Titrosampler, 869 Compact Sample Changer, 863 Compact Auto-
sampler and 899 Coulometer. Including USB hub with two connec-
tors.

1 6.2122.0x0 Mains cable with C13 line socket


IEC-60320-C13
Cable plug according to customer requirements.
Switzerland: Type SEV 12
6.2122.020
Germany, …: Type CEE(7), VII
6.2122.040
USA, …: Type NEMA/ASA
6.2122.070

1 8.899.8002DE Manual – Short Instructions 899 Coulometer

13.1.5 2.899.2110

Qty. Order no. Description


1.0 1.860.0010 860 KF Thermoprep
1.0 1.899.0010 899 Coulometer
1.0 6.0341.100 Double Pt wire electrode for coulometry
Double platinum wire electrode (0.8 x 4 mm), standard ground-joint,
Metrohm plug-in head G, for Karl Fischer titrations.
Shaft material: Glass
Measuring range: –2000…2000
Measuring unit: mV
Temp. continuous (°C): –20…70
Temp. short-term. (°C): –20…70
SGJ sleeve: Standard ground-joint 14/15
Shaft diameter top (mm): 12
Shaft diameter bottom (mm): 8.75
Minimum immersion depth 10
(mm):
Electrode plug-in head: Metrohm plug-in head G

899 Coulometer ■■■■■■■■ 139


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Qty. Order no. Description


Indicator electrode type: Pt
Indicator electrode shape: Wire

1.0 6.0345.100 Generator electrode without diaphragm


Generator electrode for Karl Fischer titrations, without diaphragm,
standard ground-joint 29/22.
Shaft material: Glass
Temp. continuous (°C): –20…70
Temp. short-term. (°C): –20…70
SGJ sleeve: Standard ground-joint 29/22
Shaft diameter top (mm): 24
Shaft diameter bottom (mm): 24
Minimum immersion depth 15
(mm):
Electrode plug-in head: Metrohm plug-in head G
Indicator electrode type: Cathode = Pt sheet
Indicator electrode type (ref- Anode = Pt grid
erence):
1.0 6.1403.030 KF adsorber tube for coulometer cell
For KF coulometers.
Height (mm): 93
SGJ size: B-17/19

1.0 6.1437.000 Ground-joint stopper SGJ 14


Material: Glass
Height (mm): 34
SGJ size: B-14/15

140 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 13 Accessories

Qty. Order no. Description


1.0 6.1446.170 Heating tubing stopper
For coulometric KF vessels in connection with heatable tubing con-
nection.
Material: PP
Height (mm): 34
Outer diameter (mm): 13

2.0 6.1448.020 Septum / 16 mm / 5 pieces


Set of 5 pieces.
Material: Silicone rubber
Height (mm): 2
Outer diameter (mm): 16

1.0 6.1448.057 Aluminum septum seal / 100 pieces


Including Al seal.
Material: Aluminum
Material 2: Silicone
Height (mm): 7.4
Outer diameter (mm): 20.7

1.0 6.1464.320 KF titration vessel / 80 - 250 mL / coulomet-


ric
Material: Clear glass
Height (mm): 114
Volume (mL): 80…250

899 Coulometer ■■■■■■■■ 141


13.1 Scope of delivery ■■■■■■■■■■■■■■■■■■■■■■

Qty. Order no. Description


2.0 6.1602.145 Drying flask cover
Screw cap with thread GL 45 for the 6.1608.050 drying flask.

2.0 6.1608.050 Drying flask / 100 mL / GL 45


Material: Clear glass
Height (mm): 100
Outer diameter (mm): 56
Volume (mL): 100

1.0 6.1805.010 FEP tubing / M6 / 13 cm


With light protection and protection against kinks.
Material: FEP
Inner diameter (mm): 2
Length (mm): 130

142 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 13 Accessories

Qty. Order no. Description


2.0 6.1805.080 FEP tubing / M6 / 25 cm
With light protection and protection against kinks.
Material: FEP
Inner diameter (mm): 2
Length (mm): 250

1.0 6.1805.100 FEP tubing / M6 / 40 cm


With light protection and protection against kinks.
Material: FEP
Inner diameter (mm): 2
Length (mm): 400

1.0 6.1808.040 Tubing adapter M6 outer / M8 inner


Thread M6 outer, M8 inner.
Material: PTCFE

899 Coulometer ■■■■■■■■ 143


13.1 Scope of delivery ■■■■■■■■■■■■■■■■■■■■■■

Qty. Order no. Description


1.0 6.1808.050 Tubing adapter olive / M8 outer
1 outer thread M8 and 1 tubing olive.
Material: PVDF
Length (mm): 31.5

2.0 6.1821.040 Filter tube


Filter tube for the 6.1608.050 drying flask. For Rancimats and Karl
Fischer ovens.
Length (mm): 112

1.0 6.1830.030 Heatable outlet tubing


Heatable outlet tubing for 860 KF Thermoprep and 874 Oven Sam-
ple Processor.

144 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 13 Accessories

Qty. Order no. Description


1.0 6.1903.030 Stirring bar / 25 mm
Stirring bar with magnetic core, PTFE covering, length 25 mm.
Material: PTFE
Outer diameter (mm): 5
Length (mm): 25

1.0 6.2047.030 Titration vessel holder


1.0 6.2048.030 Guidance rod
Guidance rod for 860 KF Thermoprep.

1.0 6.2049.040 Needle holder with Luer lock


Length (mm): 58

1.0 6.2060.010 Cable holder


Utilization with 860 KF Thermoprep.

899 Coulometer ■■■■■■■■ 145


13.1 Scope of delivery ■■■■■■■■■■■■■■■■■■■■■■

Qty. Order no. Description


1.0 6.2063.010 Sample insert for 6 mL sample vials
(6.2419.007)

1.0 6.2103.130 Adapter red plug 2 mm / 4 mm socket


For connecting plug B (4 mm) to socket 2 mm.

1.0 6.2103.140 Adapter black plug 2 mm / socket B 4 mm


For connecting plug B (4 mm) to socket 2 mm.

1.0 6.2104.020 Electrode cable / 1 m / F


For connecting electrodes with Metrohm plug-in head G to Metrohm
instruments (socket F).
Length (m): 1

146 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 13 Accessories

Qty. Order no. Description


1.0 6.2104.120 Electrode cable / 1 m / H
With plug H. For the connection generator electrode - KF coulome-
ter.
Length (m): 1

1.0 6.2151.100 Adapter USB Mini (OTG) - USB A


For connecting USB instruments.

1.0 6.2164.010 Power supply unit 100 - 240 V/24 V DC


1.0 6.2419.007 Sample vial 6 mL / 100 pieces
Suitable for the 6.1448.05X septum. Utilization for KF determinations
with oven.
Volume (mL): 6

1.0 6.2621.110 Septum crimping tongs


Septum crimping tongs for sealing 6 mL sample vessels (6.2419.000,
6.2419.007).
Length (mm): 210

899 Coulometer ■■■■■■■■ 147


13.1 Scope of delivery ■■■■■■■■■■■■■■■■■■■■■■

Qty. Order no. Description


1.0 6.2621.120 Hexagon key 1.5 mm

1.0 6.2627.000 Oven insert


Utilization with 860 KF Thermoprep.

1.0 6.2701.040 Screw cap


With a hole for the 6.1448.020 septum. For the 6.1464.32X and
6.1465.320 titration vessels.
Material: PBT
Height (mm): 20
Outer diameter (mm): 24
Inner diameter (mm): 18

3.0 6.2713.000 Sleeve


For the fat-free ground-joint connection with the standard ground-
joint SGJ 14.
Material: PTFE film

148 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 13 Accessories

Qty. Order no. Description


1.0 6.2713.010 Sleeve
Sleeve for the fat-free ground-joint connection with the standard
ground-joint SGJ 29.
Material: PTFE film

1.0 6.2713.020 Sleeve


For the fat-free ground-joint connection with the standard ground-
joint SGJ 19.
Material: PTFE film

1.0 6.2723.310 Protective cover


Protective cover for display and keypad for all instruments of the
Titrino plus family. Suitable for: 848 Titrino plus, 862 Compact Titro-
sampler, 863 Compact Autosampler, 865 Dosimat plus, 869 Com-
pact Sample Changer, 870 KF Titrino plus, 876 Dosimat plus, 877
Titrino plus, 899 Coulometer.
Material: PVC

1.0 6.2724.010 Dust filter


Dust filter for Rancimats and Karl Fischer ovens.
Outer diameter (mm): 44
Length (mm): 53

1.0 6.2738.000 Funnel


For the KF coulometer.
Material: PP
Outer diameter (mm): 50
Inner diameter (mm): 6

899 Coulometer ■■■■■■■■ 149


13.1 Scope of delivery ■■■■■■■■■■■■■■■■■■■■■■

Qty. Order no. Description


1.0 6.2739.000 Wrench
For tightening connectors.
Length (mm): 68

1.0 6.2811.000 Molecular sieve


Molecular sieve. Bottle containing 250 g. Pore size: 0.3 nm. Without
moisture indicator. For Rancimats and Karl Fischer instruments.

2.0 6.2816.030 Needle with Luer connector


Outer diameter (mm): 0.8
Length (mm): 80

150 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 13 Accessories

Qty. Order no. Description


1.0 6.2816.070 Needle for the gas inlet
Used with Karl Fischer ovens.
Material: Stainless steel (AISI 304)

1.0 6.2816.080 Exhaust air needle


For 860 KF Thermoprep and sample changers with oven module.
Material: Stainless steel (AISI 304)

2.0 6.2816.090 Syringe 5 mL


Syringe 5 mL, PP, with Luer connector.
Material: PP

1.0 6.6063.900 tiBase 1.0 Demo CD


Demo CD for tiBase. Test version for 30 days.

899 Coulometer ■■■■■■■■ 151


13.1 Scope of delivery ■■■■■■■■■■■■■■■■■■■■■■

Qty. Order no. Description


1.0 6.2147.000 Numerical USB keypad
Numerical USB keypad for Titrino plus, Dosimat plus, 862 Compact
Titrosampler, 869 Compact Sample Changer, 863 Compact Auto-
sampler and 899 Coulometer. Including USB hub with two connec-
tors.

1 6.2122.0x0 Mains cable with C13 line socket


IEC-60320-C13
Cable plug according to customer requirements.
Switzerland: Type SEV 12
6.2122.020
Germany, …: Type CEE(7), VII
6.2122.040
USA, …: Type NEMA/ASA
6.2122.070

1 8.899.8002DE Manual – Short Instructions 899 Coulometer

13.1.6 2.899.3110

Qty. Order no. Description


1.0 1.141.0100 USB thermal printer Neo's
1.0 1.885.0010 885 Compact Oven SC
1.0 1.899.0010 899 Coulometer
1.0 6.0341.100 Double Pt wire electrode for coulometry
Double platinum wire electrode (0.8 x 4 mm), standard ground-joint,
Metrohm plug-in head G, for Karl Fischer titrations.
Shaft material: Glass
Measuring range: –2000…2000
Measuring unit: mV
Temp. continuous (°C): –20…70
Temp. short-term. (°C): –20…70
SGJ sleeve: Standard ground-joint 14/15
Shaft diameter top (mm): 12
Shaft diameter bottom (mm): 8.75
Minimum immersion depth 10
(mm):

152 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 13 Accessories

Qty. Order no. Description


Electrode plug-in head: Metrohm plug-in head G
Indicator electrode type: Pt
Indicator electrode shape: Wire

1.0 6.0345.100 Generator electrode without diaphragm


Generator electrode for Karl Fischer titrations, without diaphragm,
standard ground-joint 29/22.
Shaft material: Glass
Temp. continuous (°C): –20…70
Temp. short-term. (°C): –20…70
SGJ sleeve: Standard ground-joint 29/22
Shaft diameter top (mm): 24
Shaft diameter bottom (mm): 24
Minimum immersion depth 15
(mm):
Electrode plug-in head: Metrohm plug-in head G
Indicator electrode type: Cathode = Pt sheet
Indicator electrode type (ref- Anode = Pt grid
erence):
1.0 6.1403.030 KF adsorber tube for coulometer cell
For KF coulometers.
Height (mm): 93
SGJ size: B-17/19

1.0 6.1437.000 Ground-joint stopper SGJ 14


Material: Glass
Height (mm): 34
SGJ size: B-14/15

899 Coulometer ■■■■■■■■ 153


13.1 Scope of delivery ■■■■■■■■■■■■■■■■■■■■■■

Qty. Order no. Description


1.0 6.1446.170 Heating tubing stopper
For coulometric KF vessels in connection with heatable tubing con-
nection.
Material: PP
Height (mm): 34
Outer diameter (mm): 13

2.0 6.1448.020 Septum / 16 mm / 5 pieces


Set of 5 pieces.
Material: Silicone rubber
Height (mm): 2
Outer diameter (mm): 16

1.0 6.1448.067 Screw cap with septum

1.0 6.1464.320 KF titration vessel / 80 - 250 mL / coulomet-


ric
Material: Clear glass
Height (mm): 114
Volume (mL): 80…250

2.0 6.1602.145 Drying flask cover


Screw cap with thread GL 45 for the 6.1608.050 drying flask.

154 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 13 Accessories

Qty. Order no. Description


2.0 6.1608.050 Drying flask / 100 mL / GL 45
Material: Clear glass
Height (mm): 100
Outer diameter (mm): 56
Volume (mL): 100

1.0 6.1805.010 FEP tubing / M6 / 13 cm


With light protection and protection against kinks.
Material: FEP
Inner diameter (mm): 2
Length (mm): 130

1.0 6.1805.060 FEP tubing / M6 / 60 cm


With light protection and protection against kinks.
Material: FEP
Inner diameter (mm): 2
Length (mm): 600

899 Coulometer ■■■■■■■■ 155


13.1 Scope of delivery ■■■■■■■■■■■■■■■■■■■■■■

Qty. Order no. Description


2.0 6.1805.080 FEP tubing / M6 / 25 cm
With light protection and protection against kinks.
Material: FEP
Inner diameter (mm): 2
Length (mm): 250

1.0 6.1808.040 Tubing adapter M6 outer / M8 inner


Thread M6 outer, M8 inner.
Material: PTCFE

1.0 6.1808.050 Tubing adapter olive / M8 outer


1 outer thread M8 and 1 tubing olive.
Material: PVDF
Length (mm): 31.5

156 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 13 Accessories

Qty. Order no. Description


2.0 6.1821.040 Filter tube
Filter tube for 6.1608.050 drying flask. For Rancimats and Karl
Fischer ovens.
Length (mm): 112

1.0 6.1830.030 Heatable outlet tubing


Heatable outlet tubing for 860 KF Thermoprep and 874 Oven Sam-
ple Processor.

1.0 6.1903.030 Stirring bar / 25 mm


Stirring bar with magnetic core, PTFE covering, length 25 mm.
Material: PTFE
Outer diameter (mm): 5
Length (mm): 25

2.0 6.2043.005 Holding clip for bottles

899 Coulometer ■■■■■■■■ 157


13.1 Scope of delivery ■■■■■■■■■■■■■■■■■■■■■■

Qty. Order no. Description


1.0 6.2047.030 Titration vessel holder
1.0 6.2049.050 Needle holder with Luer lock.
Length (mm): 73

1.0 6.2103.130 Adapter red plug 2 mm / 4 mm socket


For connecting plug B (4 mm) to socket 2 mm.

1.0 6.2103.140 Adapter black plug 2 mm / socket B 4 mm


For connecting plug B (4 mm) to socket 2 mm.

158 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 13 Accessories

Qty. Order no. Description


1.0 6.2104.020 Electrode cable / 1 m / F
For connecting electrodes with Metrohm plug-in head G to Metrohm
instruments (socket F).
Length (m): 1

1.0 6.2104.120 Electrode cable / 1 m / H


With plug H. For the connection generator electrode - KF coulome-
ter.
Length (m): 1

1.0 6.2141.390 Cable Remote (9 pin) - 885

2.0 6.2151.100 Adapter USB Mini (OTG) - USB A


For connecting USB instruments.

1.0 6.2151.120 Cable USB MINI (OTG) - USB B, 1.8 m


For connecting USB instruments.

1.0 6.2164.010 Power supply unit 100 - 240 V/24 V DC


1.0 6.2420.007 Sample vial with thread

899 Coulometer ■■■■■■■■ 159


13.1 Scope of delivery ■■■■■■■■■■■■■■■■■■■■■■

Qty. Order no. Description


1.0 6.2621.140 Hexagon key 2.5 mm

1.0 6.2701.040 Screw cap


With a hole for the 6.1448.020 septum. For the 6.1464.32X and
6.1465.320 titration vessels.
Material: PBT
Height (mm): 20
Outer diameter (mm): 24
Inner diameter (mm): 18

3.0 6.2713.000 Sleeve


For the fat-free ground-joint connection with the standard ground-
joint SGJ 14.
Material: PTFE film

1.0 6.2713.010 Sleeve


Sleeve for the fat-free ground-joint connection with the standard
ground-joint SGJ 29.
Material: PTFE film

1.0 6.2713.020 Sleeve


For the fat-free ground-joint connection with the standard ground-
joint SGJ 19.
Material: PTFE film

160 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 13 Accessories

Qty. Order no. Description


1.0 6.2723.310 Protective cover
Protective cover for display and keypad for all instruments of the
Titrino plus family. Suitable for: 848 Titrino plus, 862 Compact Titro-
sampler, 863 Compact Autosampler, 865 Dosimat plus, 869 Com-
pact Sample Changer, 870 KF Titrino plus, 876 Dosimat plus, 877
Titrino plus, 899 Coulometer.
Material: PVC

1.0 6.2724.010 Dust filter


Dust filter for Rancimats and Karl Fischer ovens.
Outer diameter (mm): 44
Length (mm): 53

1.0 6.2738.000 Funnel


For the KF coulometer.
Material: PP
Outer diameter (mm): 50
Inner diameter (mm): 6

1.0 6.2739.000 Wrench


For tightening connectors.
Length (mm): 68

899 Coulometer ■■■■■■■■ 161


13.1 Scope of delivery ■■■■■■■■■■■■■■■■■■■■■■

Qty. Order no. Description


1.0 6.2811.000 Molecular sieve
Molecular sieve. Bottle containing 250 g. Pore size: 0.3 nm. Without
moisture indicator. For Rancimats and Karl Fischer instruments.

2.0 6.2816.030 Needle with Luer connector


Outer diameter (mm): 0.8
Length (mm): 80

1.0 6.2816.070 Needle for the gas inlet


Used with Karl Fischer ovens.
Material: Stainless steel (AISI 304)

162 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 13 Accessories

Qty. Order no. Description


1.0 6.2816.080 Exhaust air needle
For 860 KF Thermoprep and sample changers with oven module.
Material: Stainless steel (AISI 304)

2.0 6.2816.090 Syringe 5 mL


Syringe 5 mL, PP, with Luer connector.
Material: PP

1.0 6.6063.900 tiBase 1.0 Demo CD


Demo CD for tiBase. Test version for 30 days.

4.0 6.9001.050 Thermal paper for USB thermal printer


Neo's
10-year guaranteed legibility with correct storage.
Width (mm): 60
Length (m): 25

1.0 6.2147.000 Numerical USB keypad

899 Coulometer ■■■■■■■■ 163


13.2 Optional accessories ■■■■■■■■■■■■■■■■■■■■■■

Qty. Order no. Description


Numerical USB keypad for Titrino plus, Dosimat plus, 862 Compact
Titrosampler, 869 Compact Sample Changer, 863 Compact Auto-
sampler and 899 Coulometer. Including USB hub with two connec-
tors.

1 6.2122.0x0 Mains cable with C13 line socket


IEC-60320-C13
Cable plug according to customer requirements.
Switzerland: Type SEV 12
6.2122.020
Germany, …: Type CEE(7), VII
6.2122.040
USA, …: Type NEMA/ASA
6.2122.070

1 8.899.8002DE Manual – Short Instructions 899 Coulometer

13.2 Optional accessories

Order no. Description


2.141.0100 USB thermal printer Neo's
Compact printer with USB interface for the Titrino plus, Dosimat plus and 899
Coulometer. Paper width 60 mm (40 characters). Including the 6.2151.120 USB
cable.

2.801.0010 801 Magnetic Stirrer


Magnetic stirrer without stand for extending the Titrino plus, Titrando, Sample
Processor, 805 Dosimat, 780/781 pH/Ion Meter and 899 Coulometer. With per-
manently attached cable for MSB (Metrohm Serial Bus).

164 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ 13 Accessories

Order no. Description


2.803.0010 803 Ti Stand with stirrer and pump
Compact titration stand with magnetic stirrer and built-in pump for adding sol-
vent and aspirating the titration vessel content. Suitable for Karl Fischer titrations
with Titrando and 899 Coulometer. MSB connector. Including extensive acces-
sories, solvent bottle and waste bottle.
Dimensions in mm (W/H/D): 106/ 101/ 220
Dimensions remark: Height with support rod: 412 mm

2.860.0010 860 KF Thermoprep


The 860 KF Thermoprep is used for thermal sample preparation in Karl Fischer
titration. Many substances are not suitable for a direct Karl Fischer titration
because they are not soluble, react with the KF reagent or because they release
their water content only very slowly or only at high temperatures. With the aid
of tightly sealed sample vials the samples are brought to the oven and can after-
wards be determined by every volumetric or coulometric KF titrator.
Dimensions in mm (W/H/D): 440/500/230

2.885.0010 885 Compact Oven Sample Changer


The 885 Compact Oven Sample Changer is used for thermal sample preparation
in Karl Fischer titration. The samples are heated in the oven up to a temperature
of 250°C. This causes the water to vaporize and be transported with a dry car-
rier gas into a titration cell in which the analysis takes place.

6.2148.030 RS-232/USB Box


Extends the Titrino plus and the 899 coulometer by two RS-232 interfaces for
the connection of e.g. balances, PC, LIMS. Requires 6.2151.030 cable.

6.2164.500 Power Box


For the power supply to the 899 Coulometer in environments where power sup-
plies are either unstable or absent.

899 Coulometer ■■■■■■■■ 165


13.2 Optional accessories ■■■■■■■■■■■■■■■■■■■■■■

Order no. Description


6.5406.000 Coulometric KF equipment, including generator elec-
trode with diaphragm
Complete accessory set for KF coulometer.

6.5406.010 Coulometric KF equipment, including generator elec-


trode without diaphragm
Complete accessory set for KF coulometer.

166 ■■■■■■■■ 899 Coulometer


■■■■■■■■■■■■■■■■■■■■■■ Index

Index
A Water standard .................. 29 Instrument diagnosis ................ 71
Adapter Working conditions ............ 33
Connect ............................. 24 Curve ....................................... 56 K
Addition and aspiration tube Karl Fischer
Mounting ........................... 13 D Coulometry ........................ 28
Adsorber tube Determination Karl Fischer oven
Fill ........................................ 9 Cancel ................................ 52 Method examples ............... 97
Application Bulletin .................. 31 Carry out ............................ 49 Using .................................. 14
Result ................................. 56 Karl Fischer titration
B Diagnosis ................................. 72 Troubleshooting ................. 89
Backup ..................................... 66 Dialog language ....................... 62 Keyboard
Balance .............................. 49, 92 Load ................................... 71 Connect ............................. 24
Connect ............................. 22 Dialog type ............................... 63 Key assignment ............ 93, 94
Interface parameters ........... 69 Directory structure .................... 67 Keyboard layout ....................... 68
Balance type ............................. 69 KFC
E Parameters ......................... 73
C Electrical connection
Calculation Power Box .......................... 15 L
Method "Blank" .................. 84 Power supply unit ............... 14 Language ................................. 62
Method "KFC" .................... 82 Electrode Language file
Method "KFC-Blank" .......... 83 Connect ............................. 17 Load ................................... 71
Numerical format ............. 103 Electrode connector Live modifications ..................... 52
Rounding-off process ....... 103 Double Pt wire electrode ...... 7 Live parameters ........................ 55
Catholyte Generator electrode ............. 7
Replacing ........................... 34 Indicator electrode ............... 7 M
Common variable ..................... 65 Electrostatic charge .................... 4 Mains connection ....................... 7
Edit .................................... 65 End of Determination EOD ..... 100 Mains voltage ............................. 4
Common Variable Endpoint Manual control
Delete ................................ 65 Dependency ....................... 95 Stirring ............................... 60
Set to invalid ...................... 65 Expert dialog ............................ 63 Method
Conditioning Delete ................................ 66
Parameters ......................... 73 F Export ................................ 42
Contrast ................................... 64 Formula editor .......................... 39 Import ................................ 66
Control ..................................... 43 Front of the instrument .............. 6 Save ................................... 41
Autostart ............................ 43 Method examples
Sample table ...................... 43 G Karl Fischer oven ................ 97
Control parameters .................. 76 Generator electrode Method template
Control range Filling ................................. 12 Load ................................... 40
Dependency ....................... 95 GLP .......................................... 88 Molecular sieve
Coulometer Graphics width ......................... 68 Replacing ........................... 10
Set up .................................. 8 Guarantee .............................. 110 MSB
Coulometer cell Connector ............................ 7
Equipping ........................... 11 I Multiple determination
Filling ................................. 12 Indicator electrode Statistics calculation ............ 85
Inserting ............................... 9 Warm-up time .................... 34
Coulometry Initialization .............................. 98 N
Drift ................................... 33 Instrument Navigate ................................... 37
Practical tips ....................... 29 Set up .................................. 8 Numerical input ........................ 37
Principle ............................. 28 Switch off ........................... 35
Sample size ........................ 31 Switch on ........................... 35

899 Coulometer ■■■■■■■■ 167


Index ■■■■■■■■■■■■■■■■■■■■■■

O Report Stirrer
Operation Print manually .................... 59 Connect ............................. 21
General .............................. 36 Select ................................. 86 Stirring rate .............................. 92
Oven module ........................... 14 Result ....................................... 56 Stop conditions
Recalculate ......................... 57 Parameters ......................... 81
P Rounding-off process ....... 103 Switch off ................................. 35
Parameters Save as a common variable . 65 Switch on ................................. 35
Calculation ......................... 81 Result report System initialization .................. 98
Conditioning ...................... 73 Define ................................ 86
Dependency ....................... 95 Routine dialog .......................... 64 T
KFC .................................... 73 RS-232 Temperature sensor
Modify live ......................... 55 Interface parameters ........... 70 Connect ............................. 17
Start conditions .................. 75 RS-232 connection ................. 101 Text input ................................. 37
Stop conditions .................. 81 Titration cell
Titration ............................. 79 S Equipping ........................... 11
PC/LIMS report ......................... 68 Safety instructions ...................... 3 Filling ................................. 12
Pin assignment ......................... 99 Sample Inserting ............................... 9
Polarization current Liquid ................................. 32 Titration parameters ................. 79
Dependency ....................... 95 Solid ................................... 32 Troubleshooting ....................... 89
Preparation time Sample changer
Generator electrode with dia- Connect ............................. 27 U
phragm .............................. 33 With oven module .............. 14 Update
Generator electrode without Sample data Dialog language ................. 71
diaphragm .......................... 33 Enter .................................. 44 Program version ................. 71
Print ......................................... 59 Modify live ......................... 52 USB .......................................... 93
Printer ................................ 68, 95 Sample size Numerical keypad ............... 93
Connect ............................. 24 Send from a balance ..... 49, 92 PC keyboard ....................... 94
Program crash .......................... 98 Size .................................... 31 PC mouse ........................... 95
Program version Sample table ............................ 45 Printer ................................ 95
Update ............................... 71 Insert line ........................... 48 USB (OTG)
Load ................................... 47 Connector ............................ 7
Q Modify live ......................... 53 USB device
Quality Management ................ 88 Save ................................... 47 Adapter .............................. 24
Sensor Connect ............................. 24
R Connect ............................. 17 USB flash drive
Reagent replacement ................ 34 Sensor connector Directory structure .............. 67
Rear of the instrument ................ 7 Pt1000 ................................. 7 User name ................................ 62
Recalculate ............................... 56 Temperature sensor .............. 7
Remote Service ....................................... 3 V
Connector ............................ 7 Service Agreement ................... 88 Validation ................................. 88
Interface ............................. 99 Start conditions
Pin assignment ................... 99 Parameters ......................... 75 W
Status diagram ................. 100 Statistics ................................... 57 Warranty ................................ 110
Remote connector Statistics calculation .................. 85 Water standard
Sample changer .................. 27 Certified ............................. 29
Remote control ...................... 101

168 ■■■■■■■■ 899 Coulometer

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