ISO 3169:2023

Fine ceramics (advanced ceramics, advanced technical ceramics) — Methods for chemical analysis of impurities in aluminium oxide powders using inductively coupled plasma-optical emission spectrometry

This document specifies methods for the chemical analysis of impurities present in aluminium oxide powders used as a raw material for fine ceramics. Aluminium oxide powders are decomposed by acid pressure decomposition, acid decomposition or alkali fusion. The calcium, chromium, copper, iron, magnesium, manganese, potassium, silicon, sodium, titanium, zinc and zirconium contents in the test solution are determined by an inductively coupled plasma-optical emission spectrometer (ICP-OES).

Céramiques techniques (céramiques avancées, céramiques techniques avancées) — Méthodes d'analyse chimique des impuretés contenues dans les poudres d'oxyde d'aluminium à l'aide de la spectrométrie d'émission optique par plasma à couplage inductif

General Information

• Status: Published
• Publication Date: 15-Jan-2023
• ICS: 81.060.30 - Advanced ceramics
• Technical Committee: ISO/TC 206 - Fine ceramics
• Drafting Committee: ISO/TC 206/WG 3 - Chemical analysis
• Current Stage: 6060 - International Standard published
• Start Date: 16-Jan-2023
• Due Date: 20-Jan-2023
• Completion Date: 16-Jan-2023

Standards Content (Sample)

INTERNATIONAL ISO
STANDARD 3169
First edition
2023-01
Fine ceramics (advanced ceramics,
advanced technical ceramics) —
Methods for chemical analysis of
impurities in aluminium oxide
powders using inductively coupled
plasma-optical emission spectrometry
Céramiques techniques (céramiques avancées, céramiques techniques
avancées) — Méthodes d'analyse chimique des impuretés contenues
dans les poudres d'oxyde d'aluminium à l'aide de la spectrométrie
d'émission optique par plasma à couplage inductif
Reference number
ISO 3169:2023(E)
© ISO 2023

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ISO 3169:2023(E)
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© ISO 2023
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
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ISO 3169:2023(E)
Contents Page
Foreword .iv
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Analytical range .1
5 Preparation of test sample . 1
5.1 General . 1
5.2 Sampling . 2
5.3 Drying . 2
5.4 Weighing . 2
6 Reporting analytical values . 2
6.1 Number of analyses . 2
6.2 Blank test . 2
6.3 Evaluation of analytical results . 2
6.4 Expression of analytical results . 2
7 Decomposition of test sample .2
7.1 Classification of decomposition methods . 2
7.2 Acid pressure decomposition . 3
7.2.1 Reagents . 3
7.2.2 Apparatus and instruments . 3
7.2.3 Sample decomposition procedure . 4
7.2.4 Blank test . 5
7.3 Acid decomposition . 5
7.3.1 Reagents . 5
7.3.2 Apparatus and instruments . 5
7.3.3 Sample decomposition procedure . 5
7.3.4 Blank test . 5
7.4 Alkali fusion . 6
7.4.1 Reagents . 6
7.4.2 Apparatus and instruments . 6
7.4.3 Sample decomposition . 6
7.4.4 Blank test . 6
8 Determination of impurity elements .7
8.1 Principle . 7
8.2 Reagents . 7
8.2.1 Aluminium standard solution (Al 10 mg/ml). 7
8.2.2 Elemental standard solutions. 7
8.2.3 Mixed standard solution (each element 50 mg/l). . 7
8.3 Apparatus and instruments. 8
8.3.1 ICP-OES. . 8
8.4 Preparation of calibration standard solutions . 8
8.5 Measurement . 8
8.5.1 Set-up of the instruments . 8
8.5.2 Measurement of sample test solution and calibration standard solutions . 9
8.5.3 Measurement of blank test solution . 9
8.6 Drawing of calibration curve . 9
8.7 Calculation . 10
9 Test report .10
Annex A (informative) Interlaboratory chemical analysis of impurity in alumina powder .12
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ISO 3169:2023(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.
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
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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 206, Fine ceramics.
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.
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INTERNATIONAL STANDARD ISO 3169:2023(E)
Fine ceramics (advanced ceramics, advanced technical
ceramics) — Methods for chemical analysis of impurities
in aluminium oxide powders using inductively coupled
plasma-optical emission spectrometry
1 Scope
This document specifies methods for the chemical analysis of impurities present in aluminium oxide
powders used as a raw material for fine ceramics.
Aluminium oxide powders are decomposed by acid pressure decomposition, acid decomposition or
alkali fusion. The calcium, chromium, copper, iron, magnesium, manganese, potassium, silicon, sodium,
titanium, zinc and zirconium contents in the test solution are determined by an inductively coupled
plasma-optical emission spectrometer (ICP-OES).
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 3696, Water for analytical laboratory use — Specification and test methods
ISO 6353-2, Reagents for chemical analysis — Part 2: Specifications — First series
ISO 8656-1, Refractory products — Sampling of raw materials and unshaped products — Part 1: Sampling
scheme
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminology databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https:// www .iso .org/ obp
— IEC Electropedia: available at https:// www .electropedia .org/
4 Analytical range
Each element, range of 0,000 5 % to 0,5 % (mass fraction).
5 Preparation of test sample
5.1 General
Prepare the sample in accordance with ISO 8656-1, unless otherwise mutually agreed upon by the
analyser and the customer.
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ISO 3169:2023(E)
5.2 Sampling
Collect the sample in accordance with ISO 8656-1.
5.3 Drying
Place 10 g of the sample into a flat-type weighing bottle and spread it uniformly at the bottom of
the bottle. Heat the bottle for 2 h at 110 °C ± 5 °C, then cover the mouth of the bottle and cool it in a
desiccator for 1 h.
5.4 Weighing
Weigh the sample to the nearest 0,01 mg of the required quantity using a balance.
6 Reporting analytical values
6.1 Number of analyses
Prepare each sample twice and analyse them at intervals of time.
6.2 Blank test
Upon analysis, perform a blank test to correct the measured values. Double repetition is highly
recommended for the blank value determination.
6.3 Evaluation of analytical results
When the absolute difference between the two analytical results does not exceed the tolerance
(Table 1), the average value shall be reported. When the absolute difference between the two analytical
results exceeds the tolerance, perform two additional analyses. When the absolute difference of these
further two analyses does not exceed the tolerance, the average value thereof shall be reported. If the
difference also exceeds the tolerance, the median of four analytical results shall be reported.
Table 1 — Tolerances for two analytical results
Average value of two analytical results Tolerance
%
Less than 0,01 % 0,001
Not less than 0,01 %, and less than 0,1 % 0,005
Not less than 0,1 % 0,01
6.4 Expression of analytical results
Express the analytical results to four decimal places in % dryness (mass fraction).
7 Decomposition of test sample
7.1 Classification of decomposition methods
Aluminium oxide powders are decomposed by acid pressure decomposition, acid decomposition or
alkali fusion.
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ISO 3169:2023(E)
7.2 Acid pressure decomposition
7.2.1 Reagents
It shall be ascertained that the reagents are of sufficiently high purity to permit their use without
compromising the accuracy of the determination.
7.2.1.1 Water, grade 1 or superior as specified in ISO 3696.
7.2.1.2 Nitric acid (HNO ), 65 % minimum, as specified in ISO 6353-2.
3
7.2.1.3 Sulfuric acid (H SO ), 95 % minimum, as specified in ISO 6353-2.
2 4
7.2.1.4 Sulfuric acid solution (1 + 3). One volume of sulfuric acid (7.2.1.3) is mixed with three
volumes of water.
7.2.1.5 Nitric acid solution (1 + 50). One volume of nitric acid (7.2.1.2) is mixed with 50 volumes of
water.
7.2.1.6 Lanthanum standard solution (La 1 mg/ml). The SI traceable commercial standard solution
is available. Other internal standard solutions (e.g. Sc, Y) can be used after validation.
7.2.1.7 Internal standard solution (La 0,025 mg/ml). Transfer 5,0
...