oSIST prEN ISO 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)

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/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)

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)

General Information

• Status: Not Published
• Public Enquiry End Date: 23-Aug-2023
• ICS: 71.040.40 - Chemical analysis
• ICS: 81.080 - Refractories
• Technical Committee: IKER - Ceramics
• Current Stage: 4020 - Public enquire (PE) (Adopted Project)
• Start Date: 09-Jun-2023
• Due Date: 27-Oct-2023
• Completion Date: 18-Aug-2023
• Ref Project: prEN ISO 21068-4 - 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)

Standards Content (Sample)

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.

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oSIST prEN ISO 21068-4:2023

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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

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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.
COPYRIGHT PROTECTED DOCUMENT
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
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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: [phone]
WHICH REFERENCE MAY BE MADE IN
Reference number
Email: [e-mail]
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
  © ISO 2023 – All rights reserved
PROVIDE SUPPORTING DOCUMENTATION. © ISO 2023

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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
© ISO 2023 – All rights reserved

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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
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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
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oSIST prEN ISO 21068-4:2023

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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.
1
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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.
Fo
...