Coal and coke -- Determination of total sulfur -- Eschka method

This document specifies a reference method for determining the total sulfur content of hard coal, brown coals and lignites, and coke by the Eschka method.

Charbon et coke -- Dosage du soufre total -- Méthode Eschka

Trdna fosilna goriva - Določevanje celotnega žvepla - Eschkajeva metoda

General Information

Status
Published
Publication Date
04-Aug-2020
Current Stage
5060 - Close of voting Proof returned by Secretariat
Start Date
08-Jul-2020
Completion Date
07-Jul-2020

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INTERNATIONAL ISO
STANDARD 334
Fourth edition
2020-08
Coal and coke — Determination of
total sulfur — Eschka method
Charbon et coke — Dosage du soufre total — Méthode Eschka
Reference number
ISO 334:2020(E)
ISO 2020
---------------------- Page: 1 ----------------------
ISO 334:2020(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: 2 ----------------------
ISO 334:2020(E)
Contents Page

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

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

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

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

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

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

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

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

7 Preparation of test sample ......................................................................................................................................................................... 2

8 Procedure..................................................................................................................................................................................................................... 3

8.1 Test portion ................................................................................................................................................................................................ 3

8.1.1 For coal ..................................................................................................................................................................................... 3

8.1.2 For coke .................. .................................................... .............................................................................................................. 3

8.2 Charging the crucible ......... ................................................................................................................................................................ 3

8.3 Ignition ........................................................................................................................................................................................................... 4

8.3.1 For coal ..................................................................................................................................................................................... 4

8.3.2 For coke .................. .................................................... .............................................................................................................. 4

8.4 Recovering the residue .................................................................................................................................................................... 4

8.5 Extraction .................................................................................................................................................................................................... 4

8.6 Precipitation of barium sulfate ................................................................................................................................................. 4

8.7 Blank testing ............................................................................................................................................................................................. 5

9 Expression of results ........................................................................................................................................................................................ 5

10 Precision ....................................................................................................................................................................................................................... 6

10.1 Repeatability limit ................................................................................................................................................................................ 6

10.2 Reproducibility limit .......................................................................................................................................................................... 6

11 Test report ................................................................................................................................................................................................................... 6

Annex A (informative) Derivation of factors used in the calculation in Clause 9 ...................................................7

© ISO 2020 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO 334:2020(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 of 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 www .iso .org/

iso/ foreword .html.

This document was prepared by Technical Committee ISO/TC 27, Coal and coke, Subcommittee SC 5,

Methods of analysis.

This fourth edition cancels and replaces the third edition (ISO 334:2013), of which it constitutes a

minor revision. The changes compared to the previous edition are as follows:
— updating of referenced documents;
— amending of Introduction;
— adding of the provision of terms and definitions.

Any feedback or questions on this document should be directed to the user’s national standards body. A

complete listing of these bodies can be found at www .iso .org/ members .html.
iv © ISO 2020 – All rights reserved
---------------------- Page: 4 ----------------------
ISO 334:2020(E)
Introduction

The objective of this document is to provide a reference method for determining the total sulfur content

in coal and coke with Eschka method.

Instrumental methods for a more rapid determination of total sulfur are now available. If such a method

is to be used, it is important to demonstrate that the method is free from bias, when compared to this

reference method, and will give levels of repeatability and reproducibility which are the same as, or

better than, those quoted for the reference method (see Clause 10).
© ISO 2020 – All rights reserved v
---------------------- Page: 5 ----------------------
INTERNATIONAL STANDARD ISO 334:2020(E)
Coal and coke — Determination of total sulfur — Eschka
method
1 Scope

This document specifies a reference method for determining the total sulfur content of hard coal, brown

coals and lignites, and coke by the Eschka method.
2 Normative references

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements of this document. For dated references, only the edition cited applies. For

undated references, the latest edition of the referenced document (including any amendments) applies.

ISO 687, Solid mineral fuels — Coke — Determination of moisture in the general analysis test sample

ISO 1170, Coal and coke — Calculation of analyses to different bases

ISO 5068-2, Brown coals and lignites — Determination of moisture content — Part 2: Indirect gravimetric

method for moisture in the analysis sample

ISO 11722, Solid mineral fuels — Hard coal — Determination of moisture in the general analysis test

sample by drying in nitrogen

ISO 13909-4, Hard coal and coke — Mechanical sampling — Part 4: Coal — Preparation of test samples

ISO 18283, Hard coal and coke — Manual sampling
3 Terms and definitions
No terms and definitions are listed in this document.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at http:// www .electropedia .org/
4 Principle

A test portion is ignited in intimate contact with the Eschka mixture in an oxidizing atmosphere at

800 °C to remove combustible matter and to convert the sulfur to sulfate. This is then extracted with

hydrochloric acid solution and determined gravimetrically by precipitation with barium chloride.

5 Reagents

WARNING — Care should be exercised when handling the reagents, many of which are toxic and

corrosive.

During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only

distilled water or water of equivalent purity.
© ISO 2020 – All rights reserved 1
---------------------- Page: 6 ----------------------
ISO 334:2020(E)
5.1 Eschka mixture.

Mix two parts by mass of light calcined magnesium oxide with one part by mass of anhydrous sodium (or

potassium) carbonate. The mixture shall entirely pass a test sieve of 212 μm nominal size of openings.

5.2 Hydrochloric acid.
Concentrated ρ approximately 1,18 g/ml, mass fraction approximately 36 %.
5.3 Potassium sulfate solution.

Weigh, to the nearest 0,1 mg, about 2 g of potassium sulfate, previously dried at a temperature of

...

FINAL
INTERNATIONAL ISO/FDIS
DRAFT
STANDARD 334
ISO/TC 27/SC 5
Coal and coke — Determination of
Secretariat: SA
total sulfur — Eschka method
Voting begins on:
2020­05­12
Charbon et coke — Dosage du soufre total — Méthode Eschka
Voting terminates on:
2020­07­07
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 SUPPOR TING
DOCUMENTATION.
IN ADDITION TO THEIR EVALUATION AS
Reference number
BEING ACCEPTABLE FOR INDUSTRIAL, TECHNO­
ISO/FDIS 334:2020(E)
LOGICAL, COMMERCIAL AND USER PURPOSES,
DRAFT INTERNATIONAL STANDARDS MAY ON
OCCASION HAVE TO BE CONSIDERED IN THE
LIGHT OF THEIR POTENTIAL TO BECOME STAN­
DARDS TO WHICH REFERENCE MAY BE MADE IN
NATIONAL REGULATIONS. ISO 2020
---------------------- Page: 1 ----------------------
ISO/FDIS 334:2020(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
CH­1214 Vernier, Geneva
Phone: +41 22 749 01 11
Fax: +41 22 749 09 47
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2020 – All rights reserved
---------------------- Page: 2 ----------------------
ISO/FDIS 334:2020(E)
Contents Page

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

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

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

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

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

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

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

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

7 Preparation of test sample ......................................................................................................................................................................... 2

8 Procedure..................................................................................................................................................................................................................... 3

8.1 Test portion ................................................................................................................................................................................................ 3

8.1.1 For coal ..................................................................................................................................................................................... 3

8.1.2 For coke .................. .................................................... .............................................................................................................. 3

8.2 Charging the crucible ......... ................................................................................................................................................................ 3

8.3 Ignition ........................................................................................................................................................................................................... 4

8.3.1 For coal ..................................................................................................................................................................................... 4

8.3.2 For coke .................. .................................................... .............................................................................................................. 4

8.4 Recovering the residue .................................................................................................................................................................... 4

8.5 Extraction .................................................................................................................................................................................................... 4

8.6 Precipitation of barium sulfate ................................................................................................................................................. 4

8.7 Blank testing ............................................................................................................................................................................................. 5

9 Expression of results ........................................................................................................................................................................................ 5

10 Precision ....................................................................................................................................................................................................................... 6

10.1 Repeatability limit ................................................................................................................................................................................ 6

10.2 Reproducibility limit .......................................................................................................................................................................... 6

11 Test report ................................................................................................................................................................................................................... 6

Annex A (informative) Derivation of factors used in the calculation in Clause 9 ...................................................7

© ISO 2020 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO/FDIS 334:2020(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 non­governmental, 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 of 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 www .iso .org/

iso/ foreword .html.

This document was prepared by Technical Committee ISO/TC 27, Coal and Coke, Subcommittee SC 5,

Methods of analysis.

This fourth edition cancels and replaces the third edition (ISO 334:2013), of which it constitutes a

minor revision. The changes compared to the previous edition are as follows:
— updating of referenced documents;
— amending of Introduction;
— adding of the provision of terms and definitions.

Any feedback or questions on this document should be directed to the user’s national standards body. A

complete listing of these bodies can be found at www .iso .org/ members .html.
iv © ISO 2020 – All rights reserved
---------------------- Page: 4 ----------------------
ISO/FDIS 334:2020(E)
Introduction

The objective of this document is to provide a reference method for determining the total sulfur content

in coal and coke with Eschka method.

Instrumental methods for a more rapid determination of total sulfur are now available. If such a method

is to be used, it is important to demonstrate that the method is free from bias, when compared to this

reference method, and will give levels of repeatability and reproducibility which are the same as, or

better than, those quoted for the reference method (see Clause 10).
© ISO 2020 – All rights reserved v
---------------------- Page: 5 ----------------------
FINAL DRAFT INTERNATIONAL STANDARD ISO/FDIS 334:2020(E)
Coal and coke — Determination of total sulfur — Eschka
method
1 Scope

This document specifies a reference method for determining the total sulfur content of hard coal, brown

coals and lignites, and coke by the Eschka method.
2 Normative references

The following documents are referred to in the text in such a way that some or all of their content

constitutes requirements of this document. For dated references, only the edition cited applies. For

undated references, the latest edition of the referenced document (including any amendments) applies.

ISO 687, Solid mineral fuels — Coke — Determination of moisture in the general analysis test sample

ISO 1170, Coal and coke — Calculation of analyses to different bases

ISO 5068­2, Brown coals and lignites — Determination of moisture content — Part 2: Indirect gravimetric

method for moisture in the analysis sample

ISO 11722, Solid mineral fuels — Hard coal — Determination of moisture in the general analysis test

sample by drying in nitrogen

ISO 13909­4, Hard coal and coke — Mechanical sampling — Part 4: Coal — Preparation of test samples

ISO 18283, Hard coal and coke — Manual sampling
3 Terms and definitions
No terms and definitions are listed in this document.

ISO and IEC maintain terminological databases for use in standardization at the following addresses:

— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at http:// www .electropedia .org/
4 Principle

A test portion is ignited in intimate contact with the Eschka mixture in an oxidizing atmosphere at

800 °C to remove combustible matter and to convert the sulfur to sulfate. This is then extracted with

hydrochloric acid solution and determined gravimetrically by precipitation with barium chloride.

5 Reagents

WARNING — Care should be exercised when handling the reagents, many of which are toxic and

corrosive.

During the analysis, unless otherwise stated, use only reagents of recognized analytical grade and only

distilled water or water of equivalent purity.
© ISO 2020 – All rights reserved 1
---------------------- Page: 6 ----------------------
ISO/FDIS 334:2020(E)
5.1 Eschka mixture.
Mix two parts by mass of light calcined magnes
...

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