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 document 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 preparations and general principles for qualitative and quantitative analyses of mineralogical phase composition. Quantitative determination of α-Si3N4, β-Si3N4, Si2ON2, AlN, and β’- SiAlON are described.
For quantitative determination of α-Si3N4, β-Si3N4, Si2ON2, AlN and β’-SiAlON refinement procedures based on the total nitrogen content of the sample are described.
NOTE            ISO 21068-3 is used for the analysis of the total nitrogen content of the sample.

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

Status
Published
Publication Date
18-Jun-2024
Current Stage
6060 - Definitive text made available (DAV) - Publishing
Start Date
19-Jun-2024
Due Date
02-Jan-2026
Completion Date
19-Jun-2024

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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
...

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