Coal and coke -- Determination of chlorine using Eschka mixture

This document specifies a method of determining the chlorine content of hard coal, brown coals and lignites, and coke using Eschka mixture.

Charbon et coke -- Dosage du chlore à l'aide du mélange Eschka

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Status
Published
Publication Date
04-Aug-2020
Current Stage
5060 - Close of voting Proof returned by Secretariat
Start Date
10-Jul-2020
Completion Date
09-Jul-2020
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INTERNATIONAL ISO
STANDARD 587
Third edition
2020-08
Coal and coke — Determination of
chlorine using Eschka mixture
Charbon et coke — Dosage du chlore à l'aide du mélange Eschka
Reference number
ISO 587:2020(E)
ISO 2020
---------------------- Page: 1 ----------------------
ISO 587:2020(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 587:2020(E)
Contents Page

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

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

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

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

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

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

5.1 For all methods ....................................................................................................................................................................................... 2

5.2 For the Volhard and ISE methods ........................................................................................................................................... 2

5.3 For the Volhard method only ...................................................................................................................................................... 2

5.4 For the Mohr method only ............................................................................................................................................................ 2

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

7 Preparation of the test sample ............................................................................................................................................................... 3

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

8.1 Combustion ................................................................................................................................................................................................ 3

8.2 Completion ................................................................................................................................................................................................. 3

8.2.1 Volhard method ................................................................................................................................................................ 3

8.2.2 Mohr method ...................................................................................................................................................................... 4

8.2.3 ISE method ............................................................................................................................................................................ 4

8.3 Blank test ..................................................................................................................................................................................................... 4

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

9.1 Volhard method ...................................................................................................................................................................................... 5

9.2 Mohr titration .......................................................................................................................................................................................... 5

9.3 ISE method ................................................................................................................................................................................................. 5

9.4 All methods ................................................................................................................................................................................................ 6

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 calculations in this International Standard ......7

© ISO 2020 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO 587:2020(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 587:1997), of which it constitutes a minor

revision. The changes compared to the previous edition are as follows:
— updating of referenced documents;
— 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 ----------------------
INTERNATIONAL STANDARD ISO 587:2020(E)
Coal and coke — Determination of chlorine using Eschka
mixture
1 Scope

This document specifies a method of determining the chlorine content of hard coal, brown coals and

lignites, and coke using Eschka mixture.
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 known mass of sample is ignited in intimate contact with Eschka mixture in an oxidizing atmosphere

to remove combustible matter and to convert the chlorine to alkaline chlorides. These are extracted

with nitric acid or water and determined by either the Volhard or the Mohr method, or by potentiometric

titration using an Ion Selective Electrode (ISE).
5 Reagents

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

corrosive.

During 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: 5 ----------------------
ISO 587:2020(E)
5.1 For all methods
5.1.1 Eschka mixture.

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

potassium carbonate. The mixture shall entirely pass a test sieve of 0,212 mm nominal aperture.

5.1.2 Nitric acid, concentrated, chlorine-free, mass fraction approximately 70 %.

5.2 For the Volhard and ISE methods
5.2.1 Silver nitrate, standard volumetric solution, c(AgNO ) = 0,025 mol/l.

Heat crushed, crystalline silver nitrate at 125 °C for two to three hours. Dissolve 4,247 g in water and

dilute to 1 l. Store in an amber glass bottle.
5.3 For the Volhard method only
5.3.1 3,5,5-Trimethylhexan-1-ol.
5.3.2 n-Hexan-1-ol.

5.3.3 Potassium thiocyanate, standard volumetric solution, c(KSCN) ≈ 0,025 mol/l.

Dissolve 2,4 g of potassium thiocyanate in water and dilute to 1 l. Titrate against the silver nitrate

solution (5.2.1) and calculate the exact equivalence.

5.3.4 Iron (III) alum (ammonium iron (III) sulfate) indicator, saturated solution.

Saturate 100 ml of water with approximately 125 g of iron (III) alum [(NH ) SO ⋅Fe (SO ) ⋅24H O] and

4 2 4 2 4 3 2
add sufficient nitric acid (5.1.2) to remove the brown colour.
5.4 For the Mohr method only
5.4.1 Silver nitrate, standard volumetric solution, c(AgNO ) = 0,050 mol/l.

Weigh 8,494 g of silver nitrate, dried as in (5.2.1), dissolve in water and dilute to 1 l. Store in an amber

glass bottle.
5.4.2 Potassium chromate, indicator solution.
Dissolve 5 g of potassiu
...

FINAL
INTERNATIONAL ISO/FDIS
DRAFT
STANDARD 587
ISO/TC 27/SC 5
Coal and coke — Determination of
Secretariat: SA
chlorine using Eschka mixture
Voting begins on:
2020­05­14
Charbon et coke — Dosage du chlore à l'aide du mélange Eschka
Voting terminates on:
2020­07­09
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 587:2020(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 587:2020(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 587:2020(E)
Contents Page

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

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

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

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

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

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

5.1 For all methods ....................................................................................................................................................................................... 2

5.2 For the Volhard and ISE methods ........................................................................................................................................... 2

5.3 For the Volhard method only ...................................................................................................................................................... 2

5.4 For the Mohr method only ............................................................................................................................................................ 2

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

7 Preparation of the test sample ............................................................................................................................................................... 3

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

8.1 Combustion ................................................................................................................................................................................................ 3

8.2 Completion ................................................................................................................................................................................................. 3

8.2.1 Volhard method ................................................................................................................................................................ 3

8.2.2 Mohr method ...................................................................................................................................................................... 4

8.2.3 ISE method ............................................................................................................................................................................ 4

8.3 Blank test ..................................................................................................................................................................................................... 4

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

9.1 Volhard method ...................................................................................................................................................................................... 5

9.2 Mohr titration .......................................................................................................................................................................................... 5

9.3 ISE method ................................................................................................................................................................................................. 5

9.4 All methods ................................................................................................................................................................................................ 6

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 calculations in this International Standard ......7

© ISO 2020 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO/FDIS 587:2020(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 587:1997), of which it constitutes a minor

revision. The changes compared to the previous edition are as follows:
— updating of referenced documents;
— 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 ----------------------
FINAL DRAFT INTERNATIONAL STANDARD ISO/FDIS 587:2020(E)
Coal and coke — Determination of chlorine using Eschka
mixture
1 Scope

This document specifies a method of determining the chlorine content of hard coal, brown coals and

lignites, and coke using Eschka mixture.
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 known mass of sample is ignited in intimate contact with Eschka mixture in an oxidizing atmosphere

to remove combustible matter and to convert the chlorine to alkaline chlorides. These are extracted

with nitric acid or water and determined by either the Volhard or the Mohr method, or by potentiometric

titration using an Ion Selective Electrode (ISE).
5 Reagents

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

corrosive.

During 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: 5 ----------------------
ISO/FDIS 587:2020(E)
5.1 For all methods
5.1.1 Eschka mixture.

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

potassium carbonate. The mixture shall entirely pass a test sieve of 0,212 mm nominal aperture.

5.1.2 Nitric acid, concentrated, chlorine-free, mass fraction approximately 70 %.

5.2 For the Volhard and ISE methods
5.2.1 Silver nitrate, standard volumetric solution, c(AgNO ) = 0,025 mol/l.

Heat crushed, crystalline silver nitrate at 125 °C for two to three hours. Dissolve 4,247 g in water and

dilute to 1 l. Store in an amber glass bottle.
5.3 For the Volhard method only
5.3.1 3,5,5-Trimethylhexan-1-ol.
5.3.2 n-Hexan-1-ol.

5.3.3 Potassium thiocyanate, standard volumetric solution, c(KSCN) ≈ 0,025 mol/l.

Dissolve 2,4 g of potassium thiocyanate in water and dilute to 1 l. Titrate against the silver nitrate

solution (5.2.1) and calculate the exact equivale
...

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