oSIST prEN ISO 21068-1:2023
(Main)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/DIS 21068-1:2023)
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/DIS 21068-1:2023)
This part of ISO 21068 gives definitions and specifies techniques for the preparation of samples for the chemical analysis of silicon-carbide-containing raw materials and refractory products including:
a) SiC raw materials;
b) graphite brick containing silicon carbide;
c) silicon carbide brick (includes the bricks containing silicon nitride, silicon oxynitride, sialon);
d) refractories containing carbon and/or silicon carbide mixed with clay;
e) refractories containing carbon and/or silicon carbide mixed with silica (and fused silica);
f) refractories containing carbon and/or silicon carbide mixed with high alumina material;
g) refractories containing carbon and/or silicon carbide mixed with magnesia (and dolomite);
h) refractories containing carbon and/or silicon carbide mixed with chrome mineral or magnesia-chrome materials;
i) refractories containing carbon and/or silicon carbide except those described in a) to g) above.
The items of chemical analysis described in ISO 21068, Parts 1 to 4 are as follows:
1) loss on drying (LOD);
2) loss on ignition (LOI);
3) total carbon, Ctotal;
4) free carbon, Cfree;
5) silicon carbide, SiC;
6) free silicon (Sifree);
7) free aluminium (Alfree);
8) free magnesium (Mgfree);
9) free iron (Fefree);
10) silicon(IV) dioxide (SiO2);
11) aluminium oxide (Al2O3);
12) iron(III) oxide (total iron oxide calculated as Fe2O3);
13) titanium(IV) oxide (TiO2);
14) calcium oxide (CaO);
15) magnesium oxide (MgO);
16) sodium oxide (Na2O);
17) potassium oxide (K2O);
18) chromium(III) oxide (Cr2O3);
19) zirconium oxide (ZrO2);
20) boron oxide (total boron calculated as B2O3);
21) nitrogen;
22) oxygen;
23) nitrides (undifferentiated: Si3N4, AlN, BN, sialon, oxy-nitrides, etc.);
24) XRD-methods.
Chemische Analyse von Rohstoffen und feuerfesten Erzeugnissen, die Siliziumcarbid, Siliziumnitrid, Siliziumoxynitrid und Sialon enthalten - Teil1: Allgemeine Angaben und Probenvorbereitung (ISO/DIS 21068-1:2023)
Analyse chimique des matières premières et des produits réfractaires contenant du carbure de silicium, nitrure de silicium, oxynitrure de silicium et sialon - Partie 1: Informations générales et préparation des échantillons (ISO/DIS 21068-1:2023)
Kemijska analiza surovin in ognjevzdržnih izdelkov, ki vsebujejo silicijev karbid, silicijev nitrid, silicijev oksinitrid in sialon - 1. del: Splošne informacije in priprava vzorcev (ISO/DIS 21068-1:2023)
General Information
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Standards Content (Sample)
SLOVENSKI STANDARD
oSIST prEN ISO 21068-1:2023
01-julij-2023
Kemijska analiza surovin in ognjevzdržnih izdelkov, ki vsebujejo silicijev karbid,
silicijev nitrid, silicijev oksinitrid in sialon - 1. del: Splošne informacije in priprava
vzorcev (ISO/DIS 21068-1:2023)
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/DIS 21068-1:2023)
Chemische Analyse von Rohstoffen und feuerfesten Erzeugnissen, die Siliziumcarbid,
Siliziumnitrid, Siliziumoxynitrid und Sialon enthalten - Teil1: Allgemeine Angaben und
Probenvorbereitung (ISO/DIS 21068-1:2023)
Analyse chimique des matières premières et des produits réfractaires contenant du
carbure de silicium, nitrure de silicium, oxynitrure de silicium et sialon - Partie 1:
Informations générales et préparation des échantillons (ISO/DIS 21068-1:2023)
Ta slovenski standard je istoveten z: prEN ISO 21068-1
ICS:
71.040.40 Kemijska analiza Chemical analysis
81.080 Ognjevzdržni materiali Refractories
oSIST prEN ISO 21068-1:2023 en,fr,de
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.
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oSIST prEN ISO 21068-1:2023
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oSIST prEN ISO 21068-1:2023
DRAFT INTERNATIONAL STANDARD
ISO/DIS 21068-1
ISO/TC 33 Secretariat: BSI
Voting begins on: Voting terminates on:
2023-06-01 2023-08-24
Chemical analysis of raw materials and refractory products
containing silicon-carbide, silicon-nitride, silicon-
oxynitride and sialon —
Part 1:
General information and sample preparation
ICS: 81.080
This document is circulated as received from the committee secretariat.
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oSIST prEN ISO 21068-1:2023
DRAFT INTERNATIONAL STANDARD
ISO/DIS 21068-1
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 1:
General information and sample preparation
ICS: 81.080
This document is circulated as received from the committee secretariat.
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ii
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oSIST prEN ISO 21068-1:2023
ISO/DIS 21068-1:2023(E)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 2
3 Terms and definitions . 2
4 Sampling and preparation of the test sample . 3
4.1 General . 3
4.2 Sample pre-treatment . 4
4.2.1 General . 4
4.2.2 Crushing . 4
4.2.3 Thermal pre-treatment – Drying . 4
5 Preliminary analyses .4
6 Expression of results . 5
7 Test report . 5
Bibliography . 6
iii
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oSIST prEN ISO 21068-1:2023
ISO/DIS 21068-1:2023(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 21068-1 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 21068-1:2023
ISO/DIS 21068-1:2023(E)
Introduction
[8]
ISO 21068, Parts 1 to 4, have been developed from the combination of EN 12698:2007, Parts 1 and
[9] [10 to 12]
2 , and ISO 21068:2008, Parts 1 to 3 . The latter has been originally developed from the
[2]
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.
[9]
The new ISO 21068, 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.
ISO 21068, Parts 1 to 4, are applicable to the analysis of all refractory products as classified in
[3 to 6]
ISO 10081, Parts 1 to 4 , (shaped) and ISO 1927-1 (unshaped) and raw materials containing
carbon and/or silicon carbide. Therefore, ISO 21068, Parts 1 to 4, covers the full range of analysis from
pure silicon carbide to oxide refractory composition with low-content silicon carbide and/or nitrides.
Primarily, ISO 21068, Parts 1 to 4, provides methods to distinguish between different carbon bound
types like total carbon (C ) and free carbon (C ) and derives from these two the silicon carbide
total free
content. The new Part 4 includes details of sample preparation and general principles for qualitative
and quantitative analysis of mineralogical phase composition. Quantitative determination of α-Si N ,
3 4
β-Si N , Si ON , AlN, and SiAlON are described.
3 4 2 2
If free carbon is present, the standard includes different temperature treatment to determine the mass
changes gravimetrically. Frequently, the resulting residue is used for other determinations.
The determination of other groups of analytes described in ISO 21068, Parts 1 to 4, are free metals,
free silicon (Si ), free aluminium (Al ), free magnesium (Mg ), free iron (Fe ) and the group of
free free free free
oxides from main to trace components.
ISO 21068, Parts 1 to 4, also describe the determination of silicon dioxide, total silicon, oxygen and
nitrogen and other oxide bound metals that typically occur in the materials.
It represents a listing of analytical methods which is generally structured according to material
composition. However, it is still the user who should prove the applicability of the method depending on
the material and analytical requirements.
The most broadly used analytical techniques such as X-ray fluorescence spectroscopy (XRF) and
inductively coupled plasma-optical emission spectrometry (ICP-OES) suffer from the disadvantage that
the analytical results are chemical species independent. For carbon-containing ceramic raw materials
and compositions ISO 21068, Parts 1 to 4, provide analytical methods for the determination of free
carbon, and SiC in the presence of oxide compounds in particular SiO .
2
Due to the diversity of laboratory equipment, the four parts of ISO 21068 summarize broadly used
analytical techniques which lead to equivalent results. For example, the determination of carbon is
based in all described methods on the reaction of carbon with oxygen at elevated temperatures to CO .
2
Thus, carbon is analysed as CO .
2
As well as carbon and carbide compounds, metallic silicon, aluminium and magnesium are considered.
While metallic silicon is mainly a precursor material which remains after the production process of
SiC in the raw material, metallic aluminium is added as an antioxidant in carbon-containing refractory
formulations.
Mostly oxide bound components, such as Al O , CaO, MgO, TiO , Cr O , ZrO and alkalis, can be
2 3 2 2 3 2
[16]
determined by XRF, ICP-OES or wet chemical methods (see ISO 12677, ISO 26845 , ISO 21587
[13 to 15]
Parts 1-3 ). These results can be corrected by formulas provided by ISO 21068, Parts 1 to 4, in
consideration of the values obtained by the determination of carbon, SiC, and metallic components.
ISO 21068, Parts 1 to 4, also provide methods for qualitative and quantitative determinations of the
nitrogen content and the determination of oxygen. Thereby only the total content of nitrogen and
oxygen is given; a precise determination of non-carbide components (oxides and nitrides) is not possible
in this way.
v
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oSIST prEN ISO 21068-1:2023
ISO/DIS 21068-1:2023(E)
ISO 21068, Parts 1 to 4, also provide methods to distinguish quantitatively between different varieties
of nitrides like silicon nitride, silicon oxy-nitride and sialon.
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oSIST prEN ISO 21068-1:2023
DRAFT INTERNATIONAL STANDARD ISO/DI
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