Refractory products — Determination of reduced species in carbon containing refractories by XRD

This document describes methods for the determination of mineralogical phases often present as additives or reaction products in carbon containing or graphitic refractory products by X-ray Diffraction (XRD) using a Bragg-Brentano diffractometer. It includes details of sample preparation and general principles for qualitative and quantitative analysis of mineralogical phase composition. Quantitative determination of α-Si3N4, β-Si3N4, AlN, aluminium metal, Al4C3, silicon metal, boron carbide and BN are described. The problems encountered with some determinations are highlighted. Additional reduced species present in some refractories could include Al2O3⋅AlN solid solutions (so called Alons), Si3N4⋅SiO2 solid solutions and Si3N4⋅Al2O3 solid solutions (Sialons). The presence of some of these solid solution components will cause problems with both identification and quantification as they are not well-defined structures. NOTE For rationalisation of nitrogen containing phases, the total nitrogen content, analysed in accordance with EN 12698-1 is used.

Produits réfractaires - Détermination par DRX des espèces réduites dans les réfractaires contenant du carbone

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Published
Publication Date
07-Apr-2021
Current Stage
6060 - International Standard published
Start Date
08-Apr-2021
Completion Date
08-Apr-2021
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INTERNATIONAL ISO
STANDARD 23071
First edition
2021-04
Refractory products — Determination
of reduced species in carbon
containing refractories by XRD
Produits réfractaires - Détermination par DRX des espèces réduites
dans les réfractaires contenant du carbone
Reference number
ISO 23071:2021(E)
ISO 2021
---------------------- Page: 1 ----------------------
ISO 23071:2021(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2021

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 2021 – All rights reserved
---------------------- Page: 2 ----------------------
ISO 23071:2021(E)
Contents Page

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

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

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

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

4 Apparatus ..................................................................................................................................................................................................................... 2

5 Instrument performance ............................................................................................................................................................................. 2

6 Sampling ........................................................................................................................................................................................................................ 2

7 Procedure..................................................................................................................................................................................................................... 3

7.1 Sample preparation ............................................................................................................................................................................ 3

7.2 Measuring parameters ..................................................................................................................................................................... 3

7.3 Qualitative analysis ............................................................................................................................................................................. 3

7.4 Quantitative analysis .......................................................................................................................................................................... 4

7.4.1 General...................................................................................................................................................................................... 4

7.4.2 Quantitative phase determination using Rietveld Refinement................................................ 4

7.5 Rationalisation of results ............................................................................................................................................................... 5

7.5.1 Calculation refinement for α-Si N , β-Si N , Si ON , BN and AlN ......................................... 5

3 4 3 4 2 2

8 Limitations of method..................................................................................................................................................................................... 6

9 Test report ................................................................................................................................................................................................................... 6

Bibliography ................................................................................................................................................................................................................................ 7

© ISO 2021 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO 23071:2021(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 33 Refractories.

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 2021 – All rights reserved
---------------------- Page: 4 ----------------------
INTERNATIONAL STANDARD ISO 23071:2021(E)
Refractory products — Determination of reduced species
in carbon containing refractories by XRD
1 Scope

This document describes methods for the determination of mineralogical phases often present as

additives or reaction products in carbon containing or graphitic refractory products by X-ray Diffraction

(XRD) using a Bragg-Brentano diffractometer. It includes details of sample preparation and general

principles for qualitative and quantitative analysis of mineralogical phase composition. Quantitative

determination of α-Si N , β-Si N , AlN, aluminium metal, Al C , silicon metal, boron carbide and BN are

3 4 3 4 4 3
described. The problems encountered with some determinations are highlighted.

Additional reduced species present in some refractories could include Al O ⋅AlN solid solutions (so

2 3

called Alons), Si N ⋅SiO solid solutions and Si N ⋅Al O solid solutions (Sialons). The presence of some

3 4 2 3 4 2 3

of these solid solution components will cause problems with both identification and quantification as

they are not well-defined structures.

NOTE For rationalisation of nitrogen containing phases, the total nitrogen content, analysed in accordance

with EN 12698-1 is used.
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 836, Terminology for refractories
ISO 5022, Shaped refractory products — Sampling and acceptance testing

ISO 8656-1, Refractory products — Sampling of raw materials and unshaped products — Part 1:

Sampling scheme

ISO 10081-1, Classification of dense shaped refractory products — Part 1: Alumina-silica

ISO 10081-2, Classification of dense shaped refractory products — Part 2: Basic products containing less

than 7 % residual carbon

ISO 10081-3, Classification of dense shaped refractory products — Part 3: Basic products containing from

7 % to 50 % residual carbon

ISO 10081-4, Classification of dense shaped refractory products — Part 4: Special products

EN 13925-1, Non-destructive testing. X-ray diffraction from polycrystalline and amorphous materials.

General principles
3 Terms and definitions

For the purposes of this document the terms and definitions given in ISO 836, ISO 10081-1, ISO 10081-2,

ISO 10081-3, ISO 10081-4, EN 13925-1 and the following apply.
© ISO 2021 – All rights reserved 1
---------------------- Page: 5 ----------------------
ISO 23071:2021(E)
3.1
carbon containing refractories

refractory products containing greater than 20% carbon where carbon is dominantly added in the

manufacturing process in the form of graphite, pitch, tar, resin or similar

Note 1 to entry: For refractories in which silicon carbide is the dominant form of carbon isare beyond the scope of

this document, refer to EN 12698-2.
4 Apparatus
4.1 X-ray diffractometer
Generally comprising of but not limited to:

Bragg-Brentano X-ray diffractometer. The diffractometer will comprise of goniometer, X-ray source

(normally copper X-ray tube), incidence beam optics, diffracted beam optics, specimen stage, detector

and data collection system. More detail on suitable systems can be found in EN 13925-3.

The equipment should be aligned and calibrated as detailed in EN 13925-3.

The equipment should be capable of attaining the performance criteria given in Clause 5.

[1]

For samples containing a considerable amount of an iron (as Fe), a Cobalt X-ray tube shall be used

[1]

instead of a Copper X-ray tube due to fluorescence of the iron by the copper X-rays . In the case of

Cobalt X-ray tube, the diffractometer angles stated in this standard will need to be re calculated.

4.2 Software

Capable of peak matching, whole pattern fitting and Rietveld refinement for phase quantification.

5 Instrument performance

The instrument should be capable of the following performance parameters as defined in Annex C of

EN 13925-3):

The peak position of major peaks for a certified reference material shall not deviate by more than

0.05° 2θ.

NOTE A suitable certified reference material to check instrument performance is NIST SRM 640f-

alumina powder.
6 Sampling

Sample shaped and unshaped products using the procedures given in ISO 5022 and ISO 8656-1. When

sampling large fr
...

FINAL
INTERNATIONAL ISO/FDIS
DRAFT
STANDARD 23071
ISO/TC 33
Refractory products — Determination
Secretariat: BSI
of reduced species in carbon
Voting begins on:
2020­12­23 containing refractories by XRD
Voting terminates on:
2021­02­17
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 23071:2020(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 23071:2020(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
Email: copyright@iso.org
Website: www.iso.org
Published in Switzerland
ii © ISO 2020 – All rights reserved
---------------------- Page: 2 ----------------------
ISO/FDIS 23071:2020(E)
Contents Page

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

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

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

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

4 Apparatus ..................................................................................................................................................................................................................... 2

5 Instrument performance ............................................................................................................................................................................. 2

6 Sampling ........................................................................................................................................................................................................................ 2

7 Procedure..................................................................................................................................................................................................................... 3

7.1 Sample preparation ............................................................................................................................................................................ 3

7.2 Measuring parameters ..................................................................................................................................................................... 3

7.3 Qualitative analysis ............................................................................................................................................................................. 3

7.4 Quantitative analysis .......................................................................................................................................................................... 4

7.4.1 General...................................................................................................................................................................................... 4

7.4.2 Quantitative phase determination using Rietveld Refinement................................................ 4

7.5 Rationalisation of results ............................................................................................................................................................... 5

7.5.1 Calculation refinement for α-Si N , β-Si N , Si ON , BN and AlN ......................................... 5

3 4 3 4 2 2

8 Limitations of method..................................................................................................................................................................................... 6

9 Test report ................................................................................................................................................................................................................... 6

Bibliography ................................................................................................................................................................................................................................ 7

© ISO 2020 – All rights reserved iii
---------------------- Page: 3 ----------------------
ISO/FDIS 23071:2020(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 33 Refractories.

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 23071:2020(E)
Refractory products — Determination of reduced species
in carbon containing refractories by XRD
1 Scope

This document describes methods for the determination of mineralogical phases often present as

additives or reaction products in carbon containing or graphitic refractory products by X-ray Diffraction

(XRD) using a Bragg-Brentano diffractometer. It includes details of sample preparation and general

principles for qualitative and quantitative analysis of mineralogical phase composition. Quantitative

determination of α-Si N , β-Si N , AlN, aluminium metal, Al C , silicon metal, boron carbide and BN are

3 4 3 4 4 3
described. The problems encountered with some determinations are highlighted.

Additional reduced species present in some refractories could include Al O ⋅AlN solid solutions (so

2 3

called Alons), Si N ⋅SiO solid solutions and Si N ⋅Al O solid solutions (Sialons). The presence of some

3 4 2 3 4 2 3

of these solid solution components will cause problems with both identification and quantification as

they are not well-defined structures.

NOTE For rationalisation of nitrogen containing phases, the total nitrogen content, analysed in accordance

with EN 12698­1 is used.
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 836, Terminology for refractories
ISO 5022, Shaped refractory products — Sampling and acceptance testing

ISO 8656­1, Refractory products — Sampling of raw materials and unshaped products — Part 1:

Sampling scheme

ISO 10081­1, Classification of dense shaped refractory products — Part 1: Alumina-silica

ISO 10081­2, Classification of dense shaped refractory products — Part 2: Basic products containing less

than 7 % residual carbon

ISO 10081­3, Classification of dense shaped refractory products — Part 3: Basic products containing from

7 % to 50 % residual carbon

ISO 10081­4, Classification of dense shaped refractory products — Part 4: Special products

EN 13925­1, Non-destructive testing. X-ray diffraction from polycrystalline and amorphous materials.

General principles
3 Terms and definitions

For the purposes of this document the terms and definitions given in ISO 836, ISO 10081-1, ISO 10081-2,

ISO 10082-3, ISO 10081-4, EN 13925-1 and the following apply.
© ISO 2020 – All rights reserved 1
---------------------- Page: 5 ----------------------
ISO/FDIS 23071:2020(E)
3.1
carbon containing refractories

refractory products containing greater than 20% carbon where carbon is dominantly added in the

manufacturing process in the form of graphite, pitch, tar, resin or similar

Note 1 to entry: For refractories in which silicon carbide is the dominant form of carbon isare beyond the scope of

this document , refer to EN 12698­2.
4 Apparatus
4.1 X-ray diffractometer
Generally comprising of but not limited to:

Bragg-Brentano X-ray diffractometer. The diffractometer will comprise of goniometer, X-ray source

(normally copper X-ray tube), incidence beam optics, diffracted beam optics, specimen stage, detector

and data collection system. More detail on suitable systems can be found in EN 13925-3.

The equipment should be aligned and calibrated as detailed in EN 13925-3.

The equipment should be capable of attaining the performance criteria given in Clause 5.

[1]

For samples containing a considerable amount of an iron (as Fe), a Cobalt X-ray tube shall be used

[1]

instead of a Copper X-ray tube due to fluorescence of the iron by the copper X-rays . In the case of

Cobalt X-ray tube, the diffractometer angles stated in this standard will need to be re calculated.

4.2 Software

Capable of peak matching, whole pattern fitting and Rietveld refinement for phase quantification.

5 Instrument performance

The instrument should be capable of the following performance parameters as defined in Annex C of

EN 13925­3):
The peak position of major peaks for a certified reference material s
...

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