Brown coals and lignites -- Determination of the volatile matter in the analysis sample: one furnace method

This document specifies a method of determining the volatile matter of brown coals and lignites by the one furnace method.

Charbons bruns et lignites -- Détermination des matières volatiles dans l'échantillon pour analyse : méthode avec utilisation d'un four

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Status
Published
Publication Date
29-Jun-2020
Current Stage
5060 - Close of voting Proof returned by Secretariat
Start Date
04-Jun-2020
Completion Date
03-Jun-2020
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INTERNATIONAL ISO
STANDARD 20360
First edition
2020-06
Brown coals and lignites —
Determination of the volatile matter
in the analysis sample: one furnace
method
Charbons bruns et lignites — Détermination des matières volatiles
dans l'échantillon pour analyse : méthode avec utilisation d'un four
Reference number
ISO 20360:2020(E)
ISO 2020
---------------------- Page: 1 ----------------------
ISO 20360:2020(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 20360:2020(E)
Contents Page

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

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

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

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

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

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

5 Reagent and materials .................................................................................................................................................................................... 2

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

7 Preparation of test sample ......................................................................................................................................................................... 8

7.1 Preparation of the general analysis test sample ........................................................................................................ 8

7.2 Preparation of the sample pellets ........................................................................................................................................... 8

8 Procedure..................................................................................................................................................................................................................... 8

8.1 Furnace temperature check ......................................................................................................................................................... 8

8.2 Crucible and lid process .................................................................................................................................................................. 9

8.3 Volatile matter determination ................................................................................................................................................... 9

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

10 Precision ....................................................................................................................................................................................................................10

10.1 Repeatability limit .............................................................................................................................................................................10

10.2 Reproducibility limit .......................................................................................................................................................................10

11 Test report ................................................................................................................................................................................................................10

Bibliography .............................................................................................................................................................................................................................12

© ISO 2020 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO 20360:2020(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.

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 20360:2020(E)
Introduction

The volatile matter is determined as the loss in mass, corrected for moisture, when an analysis sample

of brown coals or lignites is heated out of contact with air under specified conditions. Due to the nature

of brown coals and lignites, the sample being pressed and cut into small pellets is necessary to minimize

the possibility of ejection of sample from the test crucible when the sample is heated at 900 °C, which

has been demonstrated for its good precision and accuracy, and applied in GB/T 212 for many years.

Results obtained by this method agree with measurements of volatile matter content by ISO 5071-1.

The test of volatile matter is empirical and, in order to obtain reproducible results, it is essential that the

rate of heating, the final temperature and the overall duration of the test are carefully controlled. It is

also essential to exclude air from the coal during heating to prevent oxidation. The fit of the crucible lid

is, therefore, critical. The moisture content of the sample is determined at the same time as the volatile

matter so that the appropriate correction can be made.

To arrive at a valid comparison of volatile matter results conducted in different laboratories, it is

essential that the moisture condition of the test samples in the two laboratories is within the expected

variance of the moisture test. If a sample is re-equilibrated with the laboratory atmosphere or partially

dried in one laboratory and not the other then oxidation can and will most definitely occur for brown

coals and lignites. Oxidation will alter the, as-determined, volatile matter of a test sample.

The dry basis precision for volatile matter includes a variance contribution from the moisture

determination and potentially a covariance component, both of which can influence the precision

statistics for volatile matter on a dry basis.

Mineral matter associated with the sample may also lose mass under the conditions of the test, the

magnitude of the loss being dependent on both the nature and the quantity of the minerals present.

© ISO 2020 – All rights reserved v
---------------------- Page: 5 ----------------------
INTERNATIONAL STANDARD ISO 20360:2020(E)
Brown coals and lignites — Determination of the volatile
matter in the analysis sample: one furnace method
1 Scope

This document specifies a method of determining the volatile matter of brown coals and lignites by the

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

ISO 1213-2, Solid mineral fuels — Vocabulary — Part 2: Terms relating to sampling, testing and analysis

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

method for moisture in the analysis sample

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

For the purposes of this document, the terms and definitions given in ISO 1213-2 and the following apply.

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/
3.1
total volatile matter
V,T

fractional loss in mass, without correction for moisture, when a solid mineral fuel is heated out of

contact with air under specified conditions
3.2
volatile matter

loss in mass, corrected for moisture, when a solid mineral fuel is heated out of contact with air under

specified conditions
[SOURCE: ISO 1213-2:2016, 3.239]
4 Principle

A portion of the general analysis sample which is pressed and cut into pellets with the side length

of about 3 mm is heated out of contact with air at 900 °C for 7 min. The percentage mass fraction of

volatile matter is calculated from the loss in mass of the test portion after deducting the loss in mass

due to moisture.
© ISO 2020 – All rights reserved 1
---------------------- Page: 6 ----------------------
ISO 20360:2020(E)
5 Reagent and materials

5.1 Desiccant, fresh or freshly regenerated and preferably self-indicating. Suitable desiccants are

magnesium perchlorate and silica gel.

WARNING — Magnesium perchlorate is a strong oxidizing agent. Do not attempt to regenerate

the absorbent. Do not permit contact with organic materials or a reducing agent.
6 Apparatus

6.1 Furnace, heated by electricity, in which a zone of uniform temperature of 900 °C ± 5 °C can be

maintained (see Figure 1, which is the same as the one given in ISO 562:2010, Figure 1).

It may be of the stop-ended type or fitted at the back with a flue approximately 25 mm in diameter and

150 mm in length.

It is important for furnaces with flues that the furnace door seals well. The flue should not reach far out

of the oven and should be fitted with a butterfly valve to restrict airflow through the fu

...

FINAL
INTERNATIONAL ISO/FDIS
DRAFT
STANDARD 20360
ISO/TC 27/SC 5
Brown coals and lignites —
Secretariat: SA
Determination of the volatile matter
Voting begins on:
2020­04­08 in the analysis sample: one furnace
method
Voting terminates on:
2020­06­03
Charbons bruns et lignites — Détermination des matières volatiles
dans l'échantillon pour analyse: méthode avec utilisation d'un four
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 20360:2020(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 20360:2020(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 20360:2020(E)
Contents Page

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

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

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

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

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

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

5 Reagent and materials .................................................................................................................................................................................... 2

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

7 Preparation of test sample ......................................................................................................................................................................... 8

7.1 Preparation of the general analysis test sample ........................................................................................................ 8

7.2 Preparation of the sample pellets ........................................................................................................................................... 8

8 Procedure..................................................................................................................................................................................................................... 8

8.1 Furnace temperature check ......................................................................................................................................................... 8

8.2 Crucible and lid process .................................................................................................................................................................. 9

8.3 Volatile matter determination ................................................................................................................................................... 9

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

10 Precision ....................................................................................................................................................................................................................10

10.1 Repeatability limit .............................................................................................................................................................................10

10.2 Reproducibility limit .......................................................................................................................................................................10

11 Test report ................................................................................................................................................................................................................10

Bibliography .............................................................................................................................................................................................................................11

© ISO 2020 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO/FDIS 20360:2020(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, Solid mineral fuels, Subcommittee

SC 5, Methods of analysis.

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 20360:2020(E)
Introduction

The volatile matter is determined as the loss in mass, corrected for moisture, when an analysis sample

of brown coals or lignites is heated out of contact with air under specified conditions. Due to the nature

of brown coals and lignites, the sample being pressed and cut into small pellets is necessary to minimize

the possibility of ejection of sample from the test crucible when the sample is heated at 900 °C, which

has been demonstrated for its good precision and accuracy, and applied in GB/T 212 for many years.

Results obtained by this method agree with measurements of volatile matter content by ISO 5071-1.

The test of volatile matter is empirical and, in order to obtain reproducible results, it is essential that the

rate of heating, the final temperature and the overall duration of the test are carefully controlled. It is

also essential to exclude air from the coal during heating to prevent oxidation. The fit of the crucible lid

is, therefore, critical. The moisture content of the sample is determined at the same time as the volatile

matter so that the appropriate correction can be made.

To arrive at a valid comparison of volatile matter results conducted in different laboratories, it is

essential that the moisture condition of the test samples in the two laboratories is within the expected

variance of the moisture test. If a sample is re-equilibrated with the laboratory atmosphere or partially

dried in one laboratory and not the other then oxidation can and will most definitely occur for brown

coals and lignites. Oxidation will alter the, as-determined, volatile matter of a test sample.

The dry basis precision for volatile matter includes a variance contribution from the moisture

determination and potentially a covariance component, both of which can influence the precision

statistics for volatile matter on a dry basis.

Mineral matter associated with the sample may also lose mass under the conditions of the test, the

magnitude of the loss being dependent on both the nature and the quantity of the minerals present.

© ISO 2020 – All rights reserved v
---------------------- Page: 5 ----------------------
FINAL DRAFT INTERNATIONAL STANDARD ISO/FDIS 20360:2020(E)
Brown coals and lignites — Determination of the volatile
matter in the analysis sample: one furnace method
1 Scope

This document specifies a method of determining the volatile matter of brown coals and lignites by the

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

ISO 1213­2, Solid mineral fuels — Vocabulary — Part 2: Terms relating to sampling, testing and analysis

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

method for moisture in the analysis sample

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

For the purposes of this document, the terms and definitions given in ISO 1213­2 and the following apply.

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/
3.1
total volatile matter
V,T

fractional loss in mass, without correction for moisture, when a solid mineral fuel is heated out of

contact with air under specified conditions
3.2
volatile matter

loss in mass, corrected for moisture, when a solid mineral fuel is heated out of contact with air under

specified conditions
[SOURCE: ISO 1213­2:2016, 3.239]
4 Principle

A portion of the general analysis sample which is pressed and cut into pellets with the side length

of about 3 mm is heated out of contact with air at 900 °C for 7 min. The percentage mass fraction of

volatile matter is calculated from the loss in mass of the test portion after deducting the loss in mass

due to moisture.
© ISO 2020 – All rights reserved 1
---------------------- Page: 6 ----------------------
ISO/FDIS 20360:2020(E)
5 Reagent and materials

5.1 Desiccant, fresh or freshly regenerated and preferably self-indicating. Suitable desiccants are

magnesium perchlorate and silica gel.

WARNING — Magnesium perchlorate is a strong oxidizing agent. Do not attempt to regenerate

the absorbent. Do not permit contact with organic materia
...

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