SIST EN ISO 21068-4:2024
(Main)Chemical analysis of raw materials and refractory products containing silicon-carbide, silicon-nitride, silicon-oxynitride and sialon - Part 4: XRD methods (ISO 21068-4:2024)
Chemical analysis of raw materials and refractory products containing silicon-carbide, silicon-nitride, silicon-oxynitride and sialon - Part 4: XRD methods (ISO 21068-4:2024)
This standard describes methods for the determination of mineralogical phases typically apparent in nitride and oxy-nitride bonded silicon carbide refractory products 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 -Si3N4, -Si3N4, Si2ON2, AlN, and SiAlON are described.
NOTE For the refinement procedures the total nitrogen content, analysed in accordance with ISO 21068-3 is needed.
Chemische Analyse von Rohstoffen und feuerfesten Erzeugnissen, die Siliciumcarbid, Siliciumnitrid, Siliciumoxinitrid und Sialon enthalten - Teil 4: XRD-Verfahren (ISO 21068-4:2024)
Dieses Dokument beschreibt Verfahren zur Bestimmung von mineralogischen Phasen, die gewöhnlich in feuerfesten Erzeugnissen aus nitrid und oxinitridgebundenem Siliciumcarbid vorkommen, unter Verwendung eines Bragg Brentano Diffraktometers.
Es enthält Einzelheiten zu Probenvorbereitungen sowie allgemeine Grundlagen für qualitative und quantitative Analysen der mineralogischen Phasen Zusammensetzung. Die quantitative Bestimmung von α Si3N4, β Si3N4, Si2ON2, AlN und β’ SiAlON wird beschrieben.
Für die quantitative Bestimmung von α Si3N4, β Si3N4, Si2ON2, AlN und β’ SiAlON werden Optimie-rungsverfahren auf der Grundlage des Gesamtstickstoffgehalts der Probe beschrieben.
ANMERKUNG ISO 21068 3 wird für die Analyse des Gesamtstickstoffgehalts der Probe verwendet.
Analyse chimique des matières premières et des produits réfractaires contenant du carbure de silicium, du nitrure de silicium, de l’oxynitrure de silicium et du sialon - Partie 4: Méthodes de DRX (ISO 21068-4:2024)
Le présent document décrit des méthodes destinées à déterminer les phases minéralogiques généralement présentes dans les produits réfractaires contenant du carbure de silicium lié au nitrure et à l’oxynitrure, au moyen d’un diffractomètre à géométrie Bragg-Brentano.
Elle contient des détails relatifs à la préparation des échantillons ainsi que des principes généraux de l’analyse qualitative et quantitative de la composition des phases minéralogiques. La détermination quantitative de α-Si3N4, β-Si3N4, Si2ON2, AlN et β’-SiAlON est décrite.
Concernant la détermination quantitative de α-Si3N4, β-Si3N4, Si2ON2, AlN et β’-SiAlON, des modes opératoire d’affinement basés sur la teneur en azote total de l’échantillon sont décrites.
NOTE L'ISO 21068-3 est utilisée pour l'analyse de la teneur en azote total de l'échantillon.
Kemijska analiza surovin in ognjevzdržnih izdelkov, ki vsebujejo silicijev karbid, silicijev nitrid, silicijev oksinitrid in sialon - 4. del: Metode XRD (ISO 21068-4:2024)
General Information
Standards Content (Sample)
SLOVENSKI STANDARD
01-september-2024
Kemijska analiza surovin in ognjevzdržnih izdelkov, ki vsebujejo silicijev karbid,
silicijev nitrid, silicijev oksinitrid in sialon - 4. del: Metode XRD (ISO 21068-4:2024)
Chemical analysis of raw materials and refractory products containing silicon-carbide,
silicon-nitride, silicon-oxynitride and sialon - Part 4: XRD methods (ISO 21068-4:2024)
Chemische Analyse von Rohstoffen und feuerfesten Erzeugnissen, die Siliciumcarbid,
Siliciumnitrid, Siliciumoxinitrid und Sialon enthalten - Teil 4: XRD-Verfahren (ISO 21068-
4:2024)
Analyse chimique des matières premières et des produits réfractaires contenant du
carbure de silicium, du nitrure de silicium, de l’oxynitrure de silicium et du sialon - Partie
4: Méthodes de DRX (ISO 21068-4:2024)
Ta slovenski standard je istoveten z: EN ISO 21068-4:2024
ICS:
71.040.40 Kemijska analiza Chemical analysis
81.080 Ognjevzdržni materiali Refractories
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
EN ISO 21068-4
EUROPEAN STANDARD
NORME EUROPÉENNE
June 2024
EUROPÄISCHE NORM
ICS 81.080
English Version
Chemical analysis of raw materials and refractory
products containing silicon-carbide, silicon-nitride, silicon-
oxynitride and sialon - Part 4: XRD methods (ISO 21068-
4:2024)
Analyse chimique des matières premières et des Chemische Analyse von Rohstoffen und feuerfesten
produits réfractaires contenant du carbure de silicium, Erzeugnissen, die Siliciumcarbid, Siliciumnitrid,
du nitrure de silicium, de l'oxynitrure de silicium et du Siliciumoxinitrid und Sialon enthalten - Teil 4: XRD-
sialon - Partie 4: Méthodes de DRX (ISO 21068-4:2024) Verfahren (ISO 21068-4:2024)
This European Standard was approved by CEN on 24 May 2024.
CEN members are bound to comply with the CEN/CENELEC Internal Regulations which stipulate the conditions for giving this
European Standard the status of a national standard without any alteration. Up-to-date lists and bibliographical references
concerning such national standards may be obtained on application to the CEN-CENELEC Management Centre or to any CEN
member.
This European Standard exists in three official versions (English, French, German). A version in any other language made by
translation under the responsibility of a CEN member into its own language and notified to the CEN-CENELEC Management
Centre has the same status as the official versions.
CEN members are the national standards bodies of Austria, Belgium, Bulgaria, Croatia, Cyprus, Czech Republic, Denmark, Estonia,
Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway,
Poland, Portugal, Republic of North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and
United Kingdom.
EUROPEAN COMMITTEE FOR STANDARDIZATION
COMITÉ EUROPÉEN DE NORMALISATION
EUROPÄISCHES KOMITEE FÜR NORMUNG
CEN-CENELEC Management Centre: Rue de la Science 23, B-1040 Brussels
© 2024 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 21068-4:2024 E
worldwide for CEN national Members.
Contents Page
European foreword . 3
European foreword
This document (EN ISO 21068-4:2024) has been prepared by Technical Committee ISO/TC 33
"Refractories" in collaboration with Technical Committee CEN/TC 187 “Refractory products and
materials” the secretariat of which is held by BSI.
This European Standard shall be given the status of a national standard, either by publication of an
identical text or by endorsement, at the latest by December 2024, and conflicting national standards
shall be withdrawn at the latest by December 2024.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CEN shall not be held responsible for identifying any or all such patent rights.
Any feedback and questions on this document should be directed to the users’ national standards
body/national committee. A complete listing of these bodies can be found on the CEN website.
According to the CEN-CENELEC Internal Regulations, the national standards organizations of the
following countries are bound to implement this European Standard: Austria, Belgium, Bulgaria,
Croatia, Cyprus, Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland,
Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, Netherlands, Norway, Poland, Portugal, Republic of
North Macedonia, Romania, Serbia, Slovakia, Slovenia, Spain, Sweden, Switzerland, Türkiye and the
United Kingdom.
Endorsement notice
The text of ISO 21068-4:2024 has been approved by CEN as EN ISO 21068-4:2024 without any
modification.
International
Standard
ISO 21068-4
First edition
Chemical analysis of raw materials
2024-06
and refractory products containing
silicon-carbide, silicon-nitride,
silicon-oxynitride and sialon —
Part 4:
XRD methods
Analyse chimique des matières premières et des produits
réfractaires contenant du carbure de silicium, du nitrure de
silicium, de l’oxynitrure de silicium et du SiAlON —
Partie 4: Méthodes de DRX
Reference number
ISO 21068-4:2024(en) © ISO 2024
ISO 21068-4:2024(en)
© ISO 2024
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 21068-4:2024(en)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Apparatus . 2
5 Sampling . 2
6 Procedure . 2
6.1 Sample preparation .2
6.2 Measuring parameters .2
6.3 Qualitative analysis .3
6.4 Quantitative analysis .3
6.4.1 General .3
6.4.2 Calculation .4
7 Precision . 7
7.1 Repeatability .7
7.2 Reproducibility . .7
8 Test report . 7
Annex A (informative) X-ray diffraction data for the determination of β’-SiAlON content . 8
Bibliography .11
iii
ISO 21068-4:2024(en)
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 document 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).
ISO draws attention to the possibility that the implementation of this document may involve the use of (a)
patent(s). ISO takes no position concerning the evidence, validity or applicability of any claimed patent
rights in respect thereof. As of the date of publication of this document, ISO had not received notice of (a)
patent(s) which may be required to implement this document. However, implementers are cautioned that
this may not represent the latest information, which may be obtained from the patent database available at
www.iso.org/patents. ISO shall not be held responsible for identifying any or all such patent rights.
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, in collaboration with the
European Committee for Standardization (CEN) Technical Committee CEN/TC 187, Refractory products
and materials, in accordance with the Agreement on technical cooperation between ISO and CEN (Vienna
Agreement).
A list of all parts in the ISO 21068 series can be found on the ISO website.
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 21068-4:2024(en)
Introduction
[1]
The ISO 21068 series has been developed from the combination of EN 12698-1:2007 and EN 12698-
[2] [3] [4] [5]
2:2007 and ISO 21068-1:2008, ISO 21068-2:2008 and ISO 21068-3:2008. The last three standards
[6]
have been originally developed from the combination of Japanese standard JIS R 2011:2007 and work items
developed within CEN. Because there is a wide variety of laboratory equipment in use, the most commonly
used methods are described.
[2]
This document is derived from EN 12698-2:2007 describing XRD methods for the determination of
mineralogical phases typically apparent in nitr
...
SLOVENSKI STANDARD
oSIST prEN ISO 21068-4:2023
01-julij-2023
Kemijska analiza surovin in ognjevzdržnih izdelkov, ki vsebujejo silicijev karbid,
silicijev nitrid, silicijev oksinitrid in sialon - 4. del: Metode XRD (ISO/DIS 21068-
4:2023)
Chemical analysis of raw materials and refractory products containing silicon-carbide,
silicon-nitride, silicon-oxynitride and sialon - Part 4: XRD methods (ISO/DIS 21068-
4:2023)
Chemische Analyse von Rohstoffen und feuerfesten Erzeugnissen, die Siliciumcarbid,
Siliciumnitrid, Siliciumoxinitrid und Sialon enthalten - Teil 4: XRD-Verfahren (ISO/DIS
21068-4:2023)
Analyse chimique des matières premières et des produits réfractaires contenant du
carbure de silicium, du nitrure de silicium, de l’oxynitrure de silicium et du sialon - Partie
4: Méthodes de DRX (ISO/DIS 21068-4:2023)
Ta slovenski standard je istoveten z: prEN ISO 21068-4
ICS:
71.040.40 Kemijska analiza Chemical analysis
81.080 Ognjevzdržni materiali Refractories
oSIST prEN ISO 21068-4:2023 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
oSIST prEN ISO 21068-4:2023
oSIST prEN ISO 21068-4:2023
DRAFT INTERNATIONAL STANDARD
ISO/DIS 21068-4
ISO/TC 33 Secretariat: BSI
Voting begins on: Voting terminates on:
2023-06-02 2023-08-25
Chemical analysis of raw materials and refractory products
containing silicon-carbide, silicon-nitride, silicon-
oxynitride and sialon —
Part 4:
XRD methods
ICS: 81.080
This document is circulated as received from the committee secretariat.
THIS DOCUMENT IS A DRAFT CIRCULATED
FOR COMMENT AND APPROVAL. IT IS
ISO/CEN PARALLEL PROCESSING
THEREFORE SUBJECT TO CHANGE AND MAY
NOT BE REFERRED TO AS AN INTERNATIONAL
STANDARD UNTIL PUBLISHED AS SUCH.
IN ADDITION TO THEIR EVALUATION AS
BEING ACCEPTABLE FOR INDUSTRIAL,
TECHNOLOGICAL, COMMERCIAL AND
USER PURPOSES, DRAFT INTERNATIONAL
STANDARDS MAY ON OCCASION HAVE TO
BE CONSIDERED IN THE LIGHT OF THEIR
POTENTIAL TO BECOME STANDARDS TO
WHICH REFERENCE MAY BE MADE IN
Reference number
NATIONAL REGULATIONS.
ISO/DIS 21068-4:2023(E)
RECIPIENTS OF THIS DRAFT ARE INVITED
TO SUBMIT, WITH THEIR COMMENTS,
NOTIFICATION OF ANY RELEVANT PATENT
RIGHTS OF WHICH THEY ARE AWARE AND TO
PROVIDE SUPPORTING DOCUMENTATION. © ISO 2023
oSIST prEN ISO 21068-4:2023
DRAFT INTERNATIONAL STANDARD
ISO/DIS 21068-4
ISO/TC 33 Secretariat: BSI
Voting begins on: Voting terminates on:
Chemical analysis of raw materials and refractory products
containing silicon-carbide, silicon-nitride, silicon-
oxynitride and sialon —
Part 4:
XRD methods
ICS: 81.080
This document is circulated as received from the committee secretariat.
THIS DOCUMENT IS A DRAFT CIRCULATED
FOR COMMENT AND APPROVAL. IT IS
© ISO 2023
ISO/CEN PARALLEL PROCESSING
THEREFORE SUBJECT TO CHANGE AND MAY
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
NOT BE REFERRED TO AS AN INTERNATIONAL
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on STANDARD UNTIL PUBLISHED AS SUCH.
the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below
IN ADDITION TO THEIR EVALUATION AS
or ISO’s member body in the country of the requester. BEING ACCEPTABLE FOR INDUSTRIAL,
TECHNOLOGICAL, COMMERCIAL AND
ISO copyright office
USER PURPOSES, DRAFT INTERNATIONAL
CP 401 • Ch. de Blandonnet 8
STANDARDS MAY ON OCCASION HAVE TO
BE CONSIDERED IN THE LIGHT OF THEIR
CH-1214 Vernier, Geneva
POTENTIAL TO BECOME STANDARDS TO
Phone: +41 22 749 01 11
WHICH REFERENCE MAY BE MADE IN
Reference number
Email: copyright@iso.org
NATIONAL REGULATIONS.
Website: www.iso.org ISO/DIS 21068-4:2023(E)
RECIPIENTS OF THIS DRAFT ARE INVITED
Published in Switzerland
TO SUBMIT, WITH THEIR COMMENTS,
NOTIFICATION OF ANY RELEVANT PATENT
RIGHTS OF WHICH THEY ARE AWARE AND TO
ii
PROVIDE SUPPORTING DOCUMENTATION. © ISO 2023
oSIST prEN ISO 21068-4:2023
ISO/DIS 21068-4:2023(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Apparatus . 2
5 Sampling . 2
6 Procedure .2
6.1 Sample preparation . 2
6.2 Measuring parameters . 2
6.3 Qualitative analysis . 3
6.4 Quantitative analysis . 3
6.4.1 General . 3
6.4.2 Calculation . 4
7 Precision . 7
7.1 Repeatability . 7
7.2 Reproducibility . . 7
8 Test report . 7
Annex A (normative) X-ray diffraction data for the determination of β’-SiAlON content .8
Bibliography .11
iii
oSIST prEN ISO 21068-4:2023
ISO/DIS 21068-4:2023(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.
International Standards are drafted in accordance with the rules given in the ISO/IEC Directives, Part 2.
The main task of technical committees is to prepare International Standards. Draft International
Standards adopted by the technical committees are circulated to the member bodies for voting.
Publication as an International Standard requires approval by at least 75 % of the member bodies
casting a vote.
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.
ISO 21068-4 was prepared by Technical Committee ISO/TC 33, Refractories
ISO 21068 consists of the following parts, under the general title Chemical analysis of raw materials and
refractory products containing silicon-carbide, silicon-nitride, silicon-oxynitride and sialon:
— Part 1: General information and sample preparation
— Part 2: Determination of volatile components, total carbon, free carbon, silicon carbide, total and free
silicon, free and surface silica
— Part 3: Determination of nitrogen, oxygen and metallic and oxide constituents
— Part 4: XRD methods
iv
oSIST prEN ISO 21068-4:2023
ISO/DIS 21068-4:2023(E)
Introduction
[4]
ISO 21068, Parts 1 to 4, have been developed from the combination of EN 12698:2007, Parts 1
[5] [6 to 8]
and 2 , and ISO 21068:2008, Parts 1 to 3 . The latter has been originally developed from the
[1]
combination of Japanese standard JIS R 2011 and work items developed within CEN.
[5]
The new Part 4 is derived from the European standard EN 12698-2:2007 describing XRD methods
for the determination of mineralogical phases typically apparent in nitride and oxy-nitride bonded
silicon carbide refractory products using a Bragg-Brentano diffractometer.
v
oSIST prEN ISO 21068-4:2023
oSIST prEN ISO 21068-4:2023
DRAFT INTERNATIONAL STANDARD ISO/DIS 21068-4:2023(E)
Chemical analysis of raw materials and refractory products
containing silicon-carbide, silicon-nitride, silicon-
oxynitride and sialon —
Part 4:
XRD methods
1 Scope
This standard describes methods for the determination of mineralogical phases typically apparent
in nitride and oxy-nitride bonded silicon carbide refractory products 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 , Si ON , AlN, and
3 4 3 4 2 2
SiAlON are described.
NOTE For the refinement procedures the total nitrogen content, analysed in accordance with ISO 21068-3 is
needed.
2 Normative references
The following referenced documents are indispensable for the application 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 21068-1, Chemical analysis of raw materials and refractory products containing silicon-carbide, silicon-
nitride, silicon-oxynitride and sialon — Part 1: General information and sample preparation
ISO 21068-2, Chemical analysis of raw materials and refractory products containing silicon-carbide,
silicon-nitride, silicon-oxynitride and sialon — Part 2: Determination of volatile components, total carbon,
free carbon, silicon carbide, total and free silicon, free and surface silica
ISO 21068-3, Chemical analysis of raw materials and refractory products containing silicon-carbide, silicon-
nitride, silicon-oxynitride and sialon — Part 3: Determination of nitrogen, oxygen and metallic and oxidic
constituents
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 10081-4, Classification of dense shaped refractory products — Part 4: Special products
3 Terms and definitions
For the purposes of this document the terms and definitions given in ISO 21068-1 and ISO 10081-4
apply.
oSIST prEN ISO 21068-4:2023
ISO/DIS 21068-4:2023(E)
4 Apparatus
The aim is to have a high resolution diffractogram with well defined peaks on a low background with
minimal artefacts due to fluorescence and Kβ peaks. A Bragg-Brentano diffractometer with a copper
X-ray tube operating at 40 kV and 20 mA to 45 mA. Primary beam monochromation is achieved using
a suitable filter or primary beam monochromator or equivalent, secondary beam monochromation
is achieved using a graphite monochromator, energy discriminator or equivalent and the following
experimental setting for data collection are used:
— goniometer with a measurement uncertainty of ≤ 0,5° at a confidence level of 95 %;
— Suitable primary and secondary slit arrangements include variable slots or fixed slits with a primary
soller slit with a divergence ≤ 2,5°;
— divergence slit 1°;
— receiving slit ≤ 0,2 mm;
— scatter slit ≤ 1°;
5 Sampling
Sample shaped and unshaped products using the procedures given in ISO 5022 and ISO 8656-1.
When sampling large fragments, take care to collect samples from different points of individual pieces.
Follow the sampling and grinding procedure as described in IS
...
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