Metrohm 875KF User Manual

875 KF Gas Analyzer

Manual

8.875.8001EN

Metrohm AG
CH-9100 Herisau
Switzerland
Phone [phone]
Fax [phone]
[e-mail]
www.metrohm.com

875 KF Gas Analyzer

8.875.8001EN

Manual

12.2012 fpe

Teachware
Metrohm AG
CH-9100 Herisau
[e-mail]

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://documents.metrohm.com.

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Table of contents

1 Introduction 1

1.1 Instrument description ......................................................... 1

1.2 System description ............................................................... 1

1.3 System specification ............................................................. 2

1.4 About the documentation ................................................... 3

1.4.1 Symbols and conventions ........................................................ 3

1.5 Safety instructions ................................................................ 4

1.5.1 General notes on safety ........................................................... 4

1.5.2 Electrical safety ........................................................................ 5

1.5.3 Flammable solvents and chemicals ........................................... 6

1.5.4 Recycling and disposal ............................................................. 6

2 Overview of the instrument 7

Table of contents

2.1 Instruments ........................................................................... 7

2.2 Piping diagram ...................................................................... 7

2.3 I/O controller ......................................................................... 8

3 Installation 10

3.1 Setting up the instrument .................................................. 10

3.1.1 Packaging .............................................................................. 10

3.1.2 Checks .................................................................................. 10

3.1.3 Location ................................................................................ 10

3.2 General ................................................................................ 11

3.3 Power connection ............................................................... 11

3.4 Connecting control lines .................................................... 12

3.5 Connecting the PC and the operating unit ....................... 13

3.6 Windows passwords .......................................................... 13

3.7 Gas connections .................................................................. 13

3.8 Drying cartridge for nitrogen ............................................ 14

3.9 851 Titrando ....................................................................... 14

3.10 Shutting down .................................................................... 14

4 Operation 15

4.1 Arrangement of the gas-carrying system ......................... 15

4.2 Methods .............................................................................. 17

4.2.1 Sequence of the "Sample measurement" method .................. 18

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Table of contents

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4.2.2 Working steps for carrying out a measurement ...................... 20

4.2.3 Explanations regarding the shape of the gas flow and titra-

tion curves ............................................................................. 22

4.2.4 Method "Reference measurement" ........................................ 23

4.2.5 Changing the gas type ........................................................... 23

4.2.6 Calibrating a new gas type .................................................... 24

4.2.7 Automatic addition of methanol, automatic reagent replace-

ment (optional accessories) .................................................... 31

4.2.8 Rinsing with solvent (optional accessories) ............................. 31

4.3 QUICKSTOP module ........................................................... 32

5 Operation and maintenance 33

5.1 General notes ...................................................................... 33

5.1.1 Care ...................................................................................... 33

5.1.2 Maintenance by Metrohm Service .......................................... 34

5.2 Quality Management and validation with Metrohm ....... 34

6 Troubleshooting 36

7 Technical specifications 38

7.1 Temperature ranges ........................................................... 38

7.2 Pressure ranges .................................................................. 38

7.3 Supply voltage .................................................................... 38

7.4 Safety specifications ........................................................... 38

7.5 Electromagnetic compatibility (EMC) ................................ 39

7.6 Dimensions .......................................................................... 39

7.7 Weight ................................................................................. 39

8 Conformity and warranty 40

8.1 Quality Management Principles ........................................ 40

8.2 Warranty (Guarantee) ........................................................ 41

9 Accessories 43

9.1 Scope of delivery ................................................................ 43

9.2 Spare parts for the basic unit ............................................ 44

9.3 Spare parts for the base plate ........................................... 44

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9.4 Spare parts for integrating the 851 Titrando .................. 45

9.5 Spare parts for the 851 Titrando ...................................... 45

9.6 Optional accessories ........................................................... 45

Index 47

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Table of figures

Figure 1 Operating unit and analysis module ................................................... 7

Figure 2 Schematic arrangement of the system ............................................... 7

Figure 3 I/O controller ................................................................................... 12

Figure 4 Schematic arrangement of the system ............................................. 16

Figure 5 Sample vessel connector ................................................................. 17

Figure 6 Schematic representation of the gas flows during an analysis .......... 20

Figure 7 Formula for calculating the extraction time ...................................... 22

Figure 8 Typical shape of the gas flow curve and drift curve .......................... 23

Figure 9 Systematic procedure for identifying the cause of drift rises ............. 37

Table of figures

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1 Introduction

1.1 Instrument description

The 875 KF Gas Analyzer is a robust, modularly designed analysis system
based on tiamo™ for routine analysis at a site.

The system described on the following pages has been devised for the
coulometric water content determination according to Karl Fischer in
gases and allows the analysis of both liquefied gases and permanent
gases. This method is also suitable for very low water contents.

The system comprises an operating unit and an analysis module. The ana­lysis module is equipped with a base plate to convey the gas and with a
water content determination cell as well as internally with an 851 Titrando
in order to carry out all required analysis steps fully automatically. For this
process, an amount of gas defined by the user is precisely measured with
the flow meter and fed to the connected coulometer cell. Sample residue
and water that might be present in the piping system are rinsed with dry
nitrogen. The water is absorbed by the coulometric reagent and deter­mined there by way of Karl Fischer titration. In coulometry, the iodine
required for titration is produced by anodic oxidation, and the water con­tent is subsequently determined. For the determination of liquefied gases,
the samples are first vaporized in a controlled manner and then conveyed
to sample determination.

1 Introduction

Please also refer to the manuals and the documentation regarding the
individual components (851 Titrando, mass flow controller, individual
components) in addition to this documentation of the KF Gas Analyzer.

1.2 System description

￭ Robust analysis system with high-quality components for routine analy-

sis tailored to the requirements of users.

￭ Gas-carrying system separate from the electronics and the power sup-

ply.

￭ The base plate with the system components is mounted behind a

hood.

￭ The base plate comprises all components of gas conveyance and prep-

aration as well as the coulometer cell.

￭ The base plate's gas system is pressure-tested.
￭ Nitrogen feed line with drying cartridge for predrying and check valve.
￭ Sample input filter preventing particles from entering the gas system.
￭ Deaeration bypass for pressure release during gas change.

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1.3 System specification

￭ Integrated, adjustable vaporizer for liquefied gases.
￭ Heated oil filter with stainless steel filter element for analyzing used

refrigerants with chiller oil contents.

￭ Rinsing connector for removing oil residue.
￭ Precise gas measurement with mass flow controller (MFC).
￭ Automated analysis process thanks to the use of solenoid valves.
￭ Predefined analysis method with a prerinsing, gas feed and postrinsing

phase.

￭ Coulometric procedure for direct water content determination.
￭ Industrial PC and TFT panel (available as an option).
￭ All components except for the TFT panel are contained in one housing.
￭ Flexible control, user-friendly method creation and management and

extensive data management using the tiamo™ software. The opera­tion of tiamo™ is described in the online help. Complete integration
and control of all system components via the software.

1.3 System specification

￭ The system must be operated in a fume cupboard.
￭ Maximum sample input pressure: 40 bar.
￭ Maximum vaporization temperature: 80 °C.
￭ Nitrogen is required as auxiliary gas. The molecular sieve is used for

predrying in the 875 KF Gas Analyzer. The input pressure must corre­spond to the vapor pressure of the samples.

￭ Gas connectors for nitrogen, rinsing medium, high-pressure waste gas:

6 mm Swagelok ferrule screw connector.

￭ Sample gas connector: 1/16'' or 6 mm Swagelok ferrule screw connec-

tor.

￭ Gas type: The system is suitable for the liquefied gases and permanent

gases listed below. The gas system must be rinsed with nitrogen after
each measurement. Additional gases may be approved on request and
after testing.

– Propane, propene, butane, butene, butadiene, LPG, natural gas
– Dimethyl ether, ethylene oxide
– Chlorinated hydrocarbons: methyl chloride, ethyl chloride, vinyl

chloride

– Refrigerants: various chlorofluorocarbon (CFC), hydrofluorocar-

bon (HFC) and chlorinated hydrocarbon (CHC) compounds.
Fresh and used refrigerants with chiller oil contents.

￭ Safety specification: degree of protection IP54.

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NOTE

The materials of the components used have been carefully selected in
accordance with the aforementioned gases. According to the current
state of technology and the material manufacturers' resistance lists,
these materials are resistant to the aforementioned gases.

However, a general guarantee is impossible to give, as we cannot pre­dict how the gas mixtures will behave in the system and we do not
know the concentration, degree of purity and aggregate state of the
various gases that flow through the system.

1.4 About the documentation

CAUTION

1 Introduction

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 opera­tion of the instrument.

1.4.1 Symbols and conventions

The following symbols and formatting may appear in this documentation:

Method Dialog text, parameter in the software

File ▶ New Menu or menu item

[Next] Button or key

Cross-reference to figure legend

The first number refers to the figure number, the sec­ond to the instrument part in the figure.

Instruction step

Carry out these steps in the sequence shown.

Warning

This symbol draws attention to a possible life hazard
or risk of injury.

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1.5 Safety instructions

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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.

1.5 Safety instructions

1.5.1 General notes on safety

WARNING

This instrument may only be operated in accordance with the specifica­tions in this documentation.

The present system is suitable for processing gases and liquefied gases. In
addition, hazardous substances are used in the wet end. Usage therefore
requires the user to have basic knowledge and experience in handling liq­uefied gases, gases and pressurized media. Knowledge with respect to the
application of the fire prevention measures prescribed for laboratories is
also mandatory. The system may be operated only by trained staff. The
operator must be trained both with regard to these operating instructions
and the customer's laboratory rules and regulations.

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.

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1 Introduction

NOTE

Check all connections of the system for leakage at regular intervals and
particularly after having made any modifications.

WARNING

The gas system is under pressure. It contains both pressurized gases
and liquefied gases.

Before the sample vessel can be changed, the pressure must be
released in the piping system and the latter may need to be rinsed with
nitrogen.

Observe the applicable regulations.

WARNING

The oven used for vaporizing the liquefied gases and the oil filter down­stream of the oven may exhibit a temperature of up to 70 °C. Avoid
direct skin contact. Wear heat-insulating gloves, if necessary.

Clean the oil filter and rinse the piping carrying gas through the oven
only with the instrument switched off and while it is cold.

1.5.2 Electrical safety

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

Only personnel qualified by Metrohm are authorized to carry out service
work on electronic components.

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.

WARNING

WARNING

There are no parts inside the housing which can be serviced or replaced
by the user.

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1.5 Safety instructions

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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.

1.5.3 Flammable solvents and chemicals

WARNING

All relevant safety measures are to be observed when working with
flammable solvents and chemicals.

￭ The instrument must be set up in a fume cupboard.
￭ Keep all sources of flame far from the workplace.
￭ Clean up spilled liquids and solids immediately.
￭ Follow the safety instructions of the chemical manufacturer.

1.5.4 Recycling and disposal

This product is covered by European Directive 2002/96/EC, WEEE – Waste
from Electrical and Electronic Equipment.

The correct disposal of your old equipment will help to prevent negative
effects on the environment and public health.

More details about the disposal of your old equipment can be obtained
from your local authorities, from waste disposal companies or from your
local dealer.

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2 Overview of the instrument

2.1 Instruments

Figure 1 Operating unit and analysis module

2 Overview of the instrument

2.2 Piping diagram

A

Nitrogen

Figure 2

Schematic arrangement of the system

Rinsing with solvent

B

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2.3 I/O controller

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Sample

C

To the coulometer cell

E

Drying cartridge (nitrogen)

1

Valve 1 (nitrogen)

3

Mass flow controller

5

Valve 2 (sample)

7

Sample input filter

9

Vaporizer

11

Oil filter, heated

13

2.3 I/O controller

Digital inputs

Table 1

Digital inputs

Waste gas

D

Stopcock 1 (deaeration)

2

Check valve

4

Stopcock 2 (rinsing with solvent)

6

Valve 4 (measurement)

8

Precision control valve (vaporizer regu-

10

lator)

Valve 3 (waste gas)

12

Terminal Function Port Port description

KL1104-1-1 E1 DigIn_1_1_1 QUICKSTOP

KL1104-1-2 +24 V

KL1104-1-3 GND

KL1104-1-4 E3 DigIn_1_1_3

KL1104-1-5 E2 DigIn_1_1_2

KL1104-1-6 +24 V

KL1104-1-7 GND

KL1104-1-8 E4 DigIn_1_1_4

Digital outputs and relay outputs

Table 2

Digital outputs and relay outputs

Terminal Function Port Port description

KL2424-2-1 A1 DigOut_1_2_1 Valve1 - N2

KL2424-2-2 GND

KL2424-2-3 GND

KL2424-2-4 A3 DigOut_1_2_3 Valve 3 - waste gas

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2 Overview of the instrument

Terminal Function Port Port description

KL2424-2-5 A2 DigOut_1_2_2 Valve 2 - sample

KL2424-2-6 GND

KL2424-2-7 GND

KL2424-2-8 A4 DigOut_1_2_4 Valve 4 - measure-

ment

Protective ground
conductor terminal, 4-

Earth Terminals 1 - 4 Earth for each of the

4 valves

pin

KL2424-3-1 A1 DigOut_1_3_1 -

KL2424-3-2 GND

KL2424-3-3 GND

KL2424-3-4 A3 DigOut_1_3_3 MFC

KL2424-3-5 A2 DigOut_1_3_2 Heater

KL2424-3-6 GND

KL2424-3-7 GND

KL2424-3-8 A4 DigOut_1_3_4 -

Analog inputs

Table 3

Analog inputs

Terminal Function Port Port description

KL3204-4-1 +I1 AnIn_1_4_1 Oven temperature

KL2424-4-2

KL2424-4-3 +I3 AnIn_1_4_3 -

KL2424-4-4 GND

KL2424-4-5 +I2 AnIn_1_4_2 -

KL2424-4-6 GND

KL2424-4-7 +I4 AnIn_1_4_4 -

KL2424-1-8 GND

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