Natural gas - Determination of water by the Karl Fischer method - Part 3: Coulometric procedure (ISO 10101-3:2022)

This document specifies a coulometric procedure for the determination of water content by the Karl Fischer method. The method is applicable to natural gas and other gases which do not react with Karl Fischer (KF) reagents.
It applies to water concentrations between 5 mg/m3 and 5 000 mg/m3. Volumes are expressed at temperature of 273,15 K (0 °C) and a pressure of 101,325 kPa (1 atm).

Erdgas - Bestimmung des Wassergehaltes nach Karl Fischer - Teil 3: Coulometrisches Verfahren (ISO 10101-3:2022)

Dieses Dokument legt ein coulometrisches Verfahren zur Bestimmung des Wassergehaltes nach Karl Fischer fest. Das Verfahren ist anwendbar für Erdgas und andere Gase, die nicht mit der Karl-Fischer-Lösung (KF Lösung) reagieren.
Dieses Dokument ist anzuwenden für Wasseranteile zwischen 5 mg/m3 und 5 000 mg/m3. Die Volumina beziehen sich auf eine Temperatur von 273,15 K (0 °C) und einen Druck von 101,325 kPa (1 atm).

Gaz naturel - Dosage de l'eau par la méthode de Karl Fischer - Partie 3: Méthode coulométrique (ISO 10101-3:2022)

Zemeljski plin - Določevanje vode po Karl-Fischerjevi metodi - 3. del: Kulometrijska metoda (ISO 10101-3:2022)

General Information

Status
Published
Public Enquiry End Date
01-Feb-2021
Publication Date
14-Nov-2022
Technical Committee
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
27-Oct-2022
Due Date
01-Jan-2023
Completion Date
15-Nov-2022

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SLOVENSKI STANDARD
SIST EN ISO 10101-3:2022
01-december-2022
Nadomešča:
SIST EN ISO 10101-3:2000
Zemeljski plin - Določevanje vode po Karl-Fischerjevi metodi - 3. del:
Kulometrijska metoda (ISO 10101-3:2022)

Natural gas - Determination of water by the Karl Fischer method - Part 3: Coulometric

procedure (ISO 10101-3:2022)

Erdgas - Bestimmung des Wassergehaltes nach Karl Fischer - Teil 3: Coulometrisches

Verfahren (ISO 10101-3:2022)
Gaz naturel - Dosage de l'eau par la méthode de Karl Fischer - Partie 3: Méthode
coulométrique (ISO 10101-3:2022)
Ta slovenski standard je istoveten z: EN ISO 10101-3:2022
ICS:
75.060 Zemeljski plin Natural gas
SIST EN ISO 10101-3:2022 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
SIST EN ISO 10101-3:2022
---------------------- Page: 2 ----------------------
SIST EN ISO 10101-3:2022
EN ISO 10101-3
EUROPEAN STANDARD
NORME EUROPÉENNE
October 2022
EUROPÄISCHE NORM
ICS 75.060 Supersedes EN ISO 10101-3:1998
English Version
Natural gas - Determination of water by the Karl Fischer
method - Part 3: Coulometric procedure (ISO 10101-
3:2022)

Gaz naturel - Dosage de l'eau par la méthode de Karl Erdgas - Bestimmung des Wassergehaltes nach Karl

Fischer - Partie 3: Méthode coulométrique (ISO 10101- Fischer - Teil 3: Coulometrisches Verfahren (ISO

3:2022) 10101-3:2022)
This European Standard was approved by CEN on 26 August 2022.

CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this

European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references

concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN

member.

This European Standard exists in three official versions (English, French, German). A version in any other language made by

translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management

Centre has the same status as the official versions.

CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,

Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,

Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and

United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels

© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 10101-3:2022 E

worldwide for CEN national Members.
---------------------- Page: 3 ----------------------
SIST EN ISO 10101-3:2022
EN ISO 10101-3:2022 (E)
Contents Page

European foreword ....................................................................................................................................................... 3

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SIST EN ISO 10101-3:2022
EN ISO 10101-3:2022 (E)
European foreword

This document (EN ISO 10101-3:2022) has been prepared by Technical Committee ISO/TC 193

"Natural gas" in collaboration with Technical Committee CEN/TC 238 “Test gases, test pressures,

appliance categories and gas appliance types” the secretariat of which is held by AFNOR.

This European Standard shall be given the status of a national standard, either by publication of an

identical text or by endorsement, at the latest by April 2023, and conflicting national standards shall be

withdrawn at the latest by April 2023.

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. CEN shall not be held responsible for identifying any or all such patent rights.

This document supersedes EN ISO 10101-3:1998.

Any feedback and questions on this document should be directed to the users’ national standards

body/national committee. A complete listing of these bodies can be found on the CEN website.

According to the CEN-CENELEC Internal Regulations, the national standards organizations of the

following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,

Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,

Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of

North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and the

United Kingdom.
Endorsement notice

The text of ISO 10101-3:2022 has been approved by CEN as EN ISO 10101-3:2022 without any

modification.
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SIST EN ISO 10101-3:2022
---------------------- Page: 6 ----------------------
SIST EN ISO 10101-3:2022
INTERNATIONAL ISO
STANDARD 10101-3
Second edition
2022-08
Natural gas — Determination of water
by the Karl Fischer method —
Part 3:
Coulometric procedure
Gaz naturel — Dosage de l'eau par la méthode de Karl Fischer —
Partie 3: Méthode coulométrique
Reference number
ISO 10101-3:2022(E)
© ISO 2022
---------------------- Page: 7 ----------------------
SIST EN ISO 10101-3:2022
ISO 10101-3:2022(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2022

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on

the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below

or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
© ISO 2022 – All rights reserved
---------------------- Page: 8 ----------------------
SIST EN ISO 10101-3:2022
ISO 10101-3:2022(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

Introduction .................................................................................................................................................................................................................................v

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ..................................................................................................................................................................................... 1

3 Terms and definitions .................................................................................................................................................................................... 1

4 Principle ........................................................................................................................................................................................................................ 1

5 Reagents ........................................................................................................................................................................................................................ 1

6 Apparatus .................................................................................................................................................................................................................... 2

7 Sampling ....................................................................................................................................................................................................................... 5

8 Procedure ....................................................................................................................................................................................................................6

8.1 Installation ................................................................................................................................................................................................. 6

8.2 Testing the response ......................................................................................................................................................................... 6

8.3 Measurement ........................................................................................................................................................................................... 6

8.4 Blank value determination .......................................................................................................................................................... 6

9 Expression of the results .............................................................................................................................................................................7

9.1 Method of calculation ....................................................................................................................................................................... 7

9.2 Measurement uncertainty ............................................................................................................................................................ 7

10 Test report .................................................................................................................................................................................................................. 8

Bibliography ................................................................................................................................................................................................................................ 9

iii
© ISO 2022 – All rights reserved
---------------------- Page: 9 ----------------------
SIST EN ISO 10101-3:2022
ISO 10101-3:2022(E)
Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards

bodies (ISO member bodies). The work of preparing International Standards is normally carried out

through ISO technical committees. Each member body interested in a subject for which a technical

committee has been established has the right to be represented on that committee. International

organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.

ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of

electrotechnical standardization.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

editorial rules of the ISO/IEC Directives, Part 2 (see www.iso.org/directives).

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of

any patent rights identified during the development of the document will be in the Introduction and/or

on the ISO list of patent declarations received (see www.iso.org/patents).

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation on the voluntary nature of standards, the meaning of ISO specific terms and

expressions related to conformity assessment, as well as information about ISO's adherence to the

World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following

URL: www.iso.org/iso/foreword.html.

This document was prepared by Technical Committee ISO/TC 193, Natural Gas, Subcommittee SC 1,

Analysis of natural gas, in collaboration with the European Committee for Standardization (CEN)

Technical Committee CEN/TC 238, Test gases, test pressures, appliance categories and gas appliance types,

in accordance with the Agreement on technical cooperation between ISO and CEN (Vienna Agreement).

This second edition cancels and replaces the first edition (ISO 10101-3:1993), which has been technically

revised.
The main changes are as follows:
— Clause 2 and Bibliography were revised;
— new fixed structure numbering inserted;
— Subclause 9.2 Measurement of uncertainty was added.
A list of all parts in the ISO 10101 series can be found on the ISO website.
© ISO 2022 – All rights reserved
---------------------- Page: 10 ----------------------
SIST EN ISO 10101-3:2022
ISO 10101-3:2022(E)
Introduction

Water vapour may be present in natural gas due to, for example, natural occurrence in the well

production stream, the storage of gas in underground reservoirs, transmission or distribution through

mains containing moisture or other reasons.

The Karl Fischer (KF) titration can be divided into two basic techniques – depending on the application

range – volumetric and coulometric KF titration. The two analysis techniques differ in the mode of

iodine addition or generation. Volumetric KF titration is preferably used for the determination of large

amounts of water in the range of 1 mg to 100 mg. Coulometry, however, is a micro-method which is

particularly well suited for determination of quantities of water from 10 μg to 10 mg.

Modern KF coulometers cover a range from 10 μg to 200 mg of water. Usually a resolution of 0,1 μg of

water is achieved.

In coulometric water determination, iodine is not added in the form of a titrating solution but rather

directly produced from an iodine-containing solution by an anodic oxidation reaction. The high analytic

precision at low absolute water quantities makes coulometric KF titration particularly well suited for

determination of the water content in aqueous gases.

Coulometric KF titration can be subdivided according to two distinct designs of the analysis cell:

Cells with and without diaphragm. In both variants, the measuring cells are made of a titration

vessel tightly sealed to prevent moisture ingress. The sample gas is passed directly through a glass

frit into the KF titration cell
...

SLOVENSKI STANDARD
oSIST prEN ISO 10101-3:2021
01-januar-2021

Zemeljski plin - Določevanje vode po Karl-Fischerjevi metodi - 3. del: Kulometrijski

postopek (ISO/DIS 10101-3:2020)

Natural gas - Determination of water by the Karl Fischer method - Part 3: Coulometric

procedure (ISO/DIS 10101-3:2020)

Erdgas - Bestimmung des Wassergehaltes nach Karl Fischer - Teil 3: Coulometrisches

Verfahren (ISO/DIS 10101-3:2020)
Gaz naturel - Dosage de l'eau par la méthode de Karl Fischer - Partie 3: Méthode
coulométrique (ISO/DIS 10101-3:2020)
Ta slovenski standard je istoveten z: prEN ISO 10101-3
ICS:
75.060 Zemeljski plin Natural gas
oSIST prEN ISO 10101-3:2021 en,fr,de

2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------
oSIST prEN ISO 10101-3:2021
---------------------- Page: 2 ----------------------
oSIST prEN ISO 10101-3:2021
DRAFT INTERNATIONAL STANDARD
ISO/DIS 10101-3
ISO/TC 193/SC 1 Secretariat: NEN
Voting begins on: Voting terminates on:
2020-11-13 2021-02-05
Natural gas — Determination of water by the Karl Fischer
method —
Part 3:
Coulometric procedure
Gaz naturel — Dosage de l'eau par la méthode de Karl Fischer —
Partie 3: Méthode coulométrique
ICS: 75.060
THIS DOCUMENT IS A DRAFT CIRCULATED
This document is circulated as received from the committee secretariat.
FOR COMMENT AND APPROVAL. IT IS
THEREFORE SUBJECT TO CHANGE AND MAY
NOT BE REFERRED TO AS AN INTERNATIONAL
STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS
ISO/CEN PARALLEL PROCESSING
BEING ACCEPTABLE FOR INDUSTRIAL,
TECHNOLOGICAL, COMMERCIAL AND
USER PURPOSES, DRAFT INTERNATIONAL
STANDARDS MAY ON OCCASION HAVE TO
BE CONSIDERED IN THE LIGHT OF THEIR
POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN
Reference number
NATIONAL REGULATIONS.
ISO/DIS 10101-3:2020(E)
RECIPIENTS OF THIS DRAFT ARE INVITED
TO SUBMIT, WITH THEIR COMMENTS,
NOTIFICATION OF ANY RELEVANT PATENT
RIGHTS OF WHICH THEY ARE AWARE AND TO
PROVIDE SUPPORTING DOCUMENTATION. ISO 2020
---------------------- Page: 3 ----------------------
oSIST prEN ISO 10101-3:2021
ISO/DIS 10101-3:2020(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2020

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting

on the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address

below or ISO’s member body in the country of the requester.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: +41 22 749 01 11
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2020 – All rights reserved
---------------------- Page: 4 ----------------------
oSIST prEN ISO 10101-3:2021
ISO/DIS 10101-3:2020(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

Introduction ..................................................................................................................................................................................................................................v

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 Terms and definitions ..................................................................................................................................................................................... 1

4 Principle ........................................................................................................................................................................................................................ 1

5 Reagents ........................................................................................................................................................................................................................ 2

5.1 Reagents specially formulated for coulometric determination. ................................................................... 2

5.2 Reference solution ............................................................................................................................................................................... 2

5.3 Commercially available dry cartridges............................................................................................................................... 2

6 Apparatus ..................................................................................................................................................................................................................... 2

7 Sampling ........................................................................................................................................................................................................................ 6

8 Procedure..................................................................................................................................................................................................................... 6

8.1 Installation .................................................................................................................................................................................................. 6

8.2 Testing the response .......................................................................................................................................................................... 6

8.3 Measurement ............................................................................................................................................................................................ 7

8.4 Blank value determination ........................................................................................................................................................... 7

9 Expression of the results .............................................................................................................................................................................. 7

9.1 Method of calculation ........................................................................................................................................................................ 7

9.2 Precision ....................................................................................................................................................................................................... 8

9.2.1 Repeatability, r ...................................................................................................................................................................8

9.2.2 Reproducibility, R ............................................................................................................................................................8

10 Test report ................................................................................................................................................................................................................... 8

Bibliography ................................................................................................................................................................................................................................ 9

© ISO 2020 – All rights reserved iii
---------------------- Page: 5 ----------------------
oSIST prEN ISO 10101-3:2021
ISO/DIS 10101-3:2020(E)
Foreword

ISO (the International Organization for Standardization) is a worldwide federation of national standards

bodies (ISO member bodies). The work of preparing International Standards is normally carried out

through ISO technical committees. Each member body interested in a subject for which a technical

committee has been established has the right to be represented on that committee. International

organizations, governmental and non-governmental, in liaison with ISO, also take part in the work.

ISO collaborates closely with the International Electrotechnical Commission (IEC) on all matters of

electrotechnical standardization.

The procedures used to develop this document and those intended for its further maintenance are

described in the ISO/IEC Directives, Part 1. In particular the different approval criteria needed for the

different types of ISO documents should be noted. This document was drafted in accordance with the

editorial rules of the ISO/IEC Directives, Part 2 (see www .iso .org/ directives).

Attention is drawn to the possibility that some of the elements of this document may be the subject of

patent rights. ISO shall not be held responsible for identifying any or all such patent rights. Details of

any patent rights identified during the development of the document will be in the Introduction and/or

on the ISO list of patent declarations received (see www .iso .org/ patents).

Any trade name used in this document is information given for the convenience of users and does not

constitute an endorsement.

For an explanation on the voluntary nature of standards, the meaning of ISO specific terms and

expressions related to conformity assessment, as well as information about ISO's adherence to the

World Trade Organization (WTO) principles in the Technical Barriers to Trade (TBT) see the following

URL: www .iso .org/ iso/ foreword .html.

This document was prepared by Technical Committee [or Project Committee] ISO/TC [or ISO/PC] 193,

Natural Gas, Subcommittee SC 1, Analysis of Natural Gas.

ISO 10101 consists of the following parts, under the general title Natural gas — Determination of water

by the Karl Fischer method:
— Part 1: Introduction
— Part 2: Volumetric procedure
— Part 3: Coulometric procedure
A list of all parts in the ISO 10101 series can be found on the ISO website.
iv © ISO 2020 – All rights reserved
---------------------- Page: 6 ----------------------
oSIST prEN ISO 10101-3:2021
ISO/DIS 10101-3:2020(E)
Introduction

Water vapour may be present in natural gas due to, for example, natural occurrence in the well

production stream, the storage of gas in underground reservoirs, transmission or distribution through

mains containing moisture or other reasons.

The Karl Fischer titration can be divided into two basic techniques – depending on the application

range – volumetric and coulometric KF titration. The two analysis techniques differ in the mode

of iodine addition or generation. Volumetric KF titration is preferably used for the determination of

large amounts of water in the range of 1 to 100 mg. Coulometry, however, is a micro‐method which is

particularly well suited for determination of quantities of water from 10 μg to 10 mg.

Modern KF coulometers cover a range from 10 μg to 200 mg of water. Usually a resolution of 0,1 μg of

water is achieved. (source?)

In coulometric water determination, iodine is not added in the form of a titrating solution but rather

directly produced from an iodine‐containing solution by an anodic oxidation reaction. The high analytic

precision at low absolute water quantities makes coulometric KF titration particularly well suited for

determination of the water content in aqueous gases.

Coulometric KF titration can be subdivided according to two distinct designs of the analysis cell:

Cells with and without diaphragm. In both variants, the measuring cells are made of a titration

vessel tightly sealed to prevent moisture ingress. The sample gas is passed directly through a glass

frit into the KF titration cell. Thus, absorption of moisture from the environment is prevented and the

gas finely dispersed. The fine distribution of the gas in the hygroscopic KF solution provides a large

surface for material exchange, so that the water contained in the gas can be fully absorbed by the

solution and then titrated. In the version with diaphragm, the cell is divided into a large anode and

a small cathode compartment, each filled with different reagents. Spatial separation is achieved by

means of the diaphragm. In both compartments platinum electrodes are installed, via which a working

current is passed through the titration cell. Due to the applied current, at the anode iodine is formed,

which immediately reacts with the absorbed water from the gas sam
...

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