EN ISO 21814:2022

Fine ceramics (advanced ceramics, advanced technical ceramics) - Methods for chemical analysis of aluminium nitride powders (ISO 21814:2019)

This document specifies methods for the chemical analysis of fine aluminium nitride powders used as the raw material for fine ceramics.
This document stipulates the determination methods of the aluminium, total nitrogen, boron, calcium, copper, iron, magnesium, manganese, molybdenum, nickel, potassium, silicon, sodium, titanium, tungsten, vanadium, zinc, zirconium, carbon, chlorine, fluorine, and oxygen contents in aluminium nitride powders. The aluminium content is determined by using either an acid pressure decomposition-CyDTA-zinc back titration method or an acid digestion-inductively coupled plasma-optical emission spectrometry (ICP-OES) method. The total nitrogen content is determined by using an acid pressure decomposition-distillation separation-acidimetric titration method, a direct decomposition-distillation separation-acidimetric titration method, or an inert gas fusion-thermal conductivity method. The boron, calcium, copper, iron, magnesium, manganese, molybdenum, nickel, potassium, silicon, sodium, titanium, tungsten, vanadium and zinc contents are determined by using an acid digestion-ICP-OES method or an acid pressure decomposition-ICP-OES method. The sodium and potassium contents are determined via an acid pressure decomposition-flame emission method or an acid pressure decomposition-atomic absorption spectrometry method. The oxygen content is determined by using an inert gas fusion-IR absorption spectrometry method, while that of carbon is determined via a combustion-IR absorption spectrometry method or a combustion-conductometry method. The chlorine and fluorine contents are determined by using a pyrohydrolysation method followed by ion chromatography or spectrophotometry.

Hochleistungskeramik - Verfahren zur chemischen Analyse von Aluminiumnitridpulvern (ISO 21814:2019)

Dieses Dokument legt Verfahren für die chemische Analyse von feinen Aluminiumnitridpulvern fest, die als Rohstoffe für Hochleistungskeramik verwendet werden.
Dieses Dokument legt die Verfahren zur Bestimmung der Gehalte an Aluminium, Gesamtstickstoff, Bor, Calcium, Kupfer, Eisen, Magnesium, Mangan, Molybdän, Nickel, Kalium, Silicium, Natrium, Titan, Wolfram, Vanadium, Zink, Zirconium, Kohlenstoff, Chlor, Fluor und Sauerstoff in Aluminiumnitridpulvern fest. Der Aluminiumgehalt wird entweder mittels CyDTA-Zink-Rücktitration nach Säuredruckaufschluss oder mittels optischer Emissionsspektrometrie mit induktiv gekoppeltem Plasma (ICP-OES, en: inductively coupled plasma-optical emission spectrometry) nach Säureaufschluss bestimmt. Der Gesamtstickstoffgehalt wird mittels acidimetrischer Titration nach Säuredruckaufschluss und Destillationstrennung, acidimetrischer Titration nach direktem Aufschluss und Destillationstrennung oder mittels thermischer Konduktometrie nach Inertgas-Schmelzextraktion bestimmt. Die Gehalte an Bor, Calcium, Kupfer, Eisen, Magnesium, Mangan, Molybdän, Nickel, Kalium, Silicium, Natrium, Titan, Wolfram, Vanadium und Zink werden mittels ICP-OES nach Säureaufschluss oder Säuredruckaufschluss bestimmt. Die Gehalte an Natrium und Kalium werden mittels Flammenemission nach Säuredruckaufschluss oder mittels Atomabsorptions¬spektrometrie nach Säuredruckaufschluss bestimmt. Der Sauerstoffgehalt wird mittels IR-Absorptions¬spektrometrie nach Inertgas-Schmelzextraktion bestimmt, der Kohlenstoffgehalt mittels IR Absorptions¬spektrometrie nach Verbrennung oder mittels konduktometrischer Bestimmung nach Verbrennung. Die Gehalte an Chlor und Fluor werden mittels Pyrohydrolyse und anschließender Ionenchromatographie oder Spektrophotometrie bestimmt.

Céramiques techniques - Méthodes d'analyse chimique des poudres de nitrure d'aluminium (ISO 21814:2019)

Le présent document spécifie des méthodes d’analyse chimique des poudres de nitrure d’aluminium utilisées comme matière première pour les céramiques techniques.
Le présent document stipule les méthodes de détermination des teneurs en aluminium, azote total, bore, calcium, cuivre, fer, magnésium, manganèse, molybdène, nickel, potassium, silicium, sodium, titane, tungstène, vanadium, zinc, zirconium, carbone, chlore, fluor et oxygène des poudres de nitrure d’aluminium. La teneur en aluminium est déterminée à l’aide d’une méthode par décomposition sous pression en milieu acide / CyDTA / titrage en retour au zinc, ou d’une méthode par digestion acide / spectrométrie d’émission optique avec plasma à couplage inductif (ICP-OES). La teneur totale en azote est déterminée à l’aide d’une méthode par décomposition sous pression en milieu acide / séparation par distillation / titrage acidimétrique, d’une méthode par décomposition directe: séparation par distillation / titrage acidimétrique, ou d’une méthode par fusion sous gaz inerte / conductivité thermique. Les teneurs en bore, calcium, cuivre, fer, magnésium, manganèse, molybdène, nickel, potassium, silicium, sodium, titane, tungstène, vanadium et zinc sont déterminées à l’aide d’une méthode par digestion acide / ICP-OES ou d’une méthode par décomposition sous pression en milieu acide / ICP-OES. Les teneurs en sodium et potassium sont déterminées à l’aide d’une méthode par décomposition sous pression en milieu acide / émission de flamme, ou d’une méthode par décomposition sous pression en milieu acide / spectrométrie d’absorption atomique. La teneur en oxygène est déterminée à l’aide d’une méthode par fusion sous gaz inerte / spectrométrie d’absorption IR, tandis que la teneur en carbone est déterminée à l’aide d’une méthode par combustion / spectrométrie d’absorption IR ou d’une méthode par conduction / conductimétrie. Les teneurs en chlore et en fluor sont déterminées à l’aide d’une méthode par pyrohydrolyse suivie d’une chromatographie ionique ou d’une spectrophotométrie.

Fina keramika (sodobna keramika, sodobna tehnična keramika) - Preskusne metode za kemične analize praškov aluminijevega nitrida (ISO 21814:2019)

Ta dokument določa metode za kemično analizo finih praškov aluminijevega nitrida, ki se uporabljajo kot surovina za fino keramiko.
Ta dokument določa metode za določevanje vsebnosti aluminija, skupnega dušika, bora, kalcija, bakra, železa, magnezija, mangana, molibdena, niklja, kalija, silicija, natrija, titana, volframa, vanadija, cinka, cirkonija, ogljika, klora, fluora in kisika v praških aluminijevega nitrida. Vsebnost aluminija se določi z uporabo metode povratne titracije s CyDTA/cinkom v kombinaciji s kislinsko razgradnjo ali metode optične emisijske spektrometrije z induktivno sklopljeno plazmo (ICP-OES) v kombinaciji z razklopom v kislini. Vsebnost skupnega dušika se določi z uporabo metode acidimetrične titracije z destilacijskim ločevanjem v kombinaciji s kislinsko razgradnjo, metode acidimetrične titracije z destilacijskim ločevanjem v kombinaciji z neposredno razgradnjo ali metodo toplotne prevodnosti v kombinaciji s fuzijo inertnega plina. Vsebnost bora, kalcija, bakra, železa, magnezija, mangana, molibdena, niklja, kalija, silicija, natrija, titana, volframa, vanadija in cinka se določi z uporabo metode optične emisijske spektrometrije z induktivno sklopljeno plazmo v kombinaciji s kislinsko razgradnjo. Vsebnost natrija in kalija se določi z uporabo metode plamenske emisije ali metode atomske absorpcijske spektrometrije v kombinaciji s kislinsko razgradnjo. Vsebnost kisika se določi z uporabo metode IR-absorpcijske spektrometrije v kombinaciji s fuzijo inertnega plina, vsebnost ogljika pa z metodo IR-absorpcijske spektrometrije v kombinaciji z zgorevanjem ali metodo konduktometrije v kombinaciji z zgorevanjem. Vsebnost klora in fluora se določi z uporabo metode pirohidrolizacije, ki ji sledi ionska kromatografija ali spektrofotometrija.

General Information

• Status: Published
• Publication Date: 29-Nov-2022
• ICS: 81.060.30 - Advanced ceramics
• Technical Committee: CEN/TC 184 - Advanced technical ceramics
• Drafting Committee: CEN/TC 184 - Advanced technical ceramics
• Current Stage: 6060 - Definitive text made available (DAV) - Publishing
• Start Date: 30-Nov-2022
• Due Date: 11-Apr-2024
• Completion Date: 30-Nov-2022
• Ref Project: SIST EN ISO 21814:2023 - Fine ceramics (advanced ceramics, advanced technical ceramics) - Methods for chemical analysis of aluminium nitride powders (ISO 21814:2019)

Relations

• Replaces: EN 725-4:2006 - Advanced technical ceramics - Methods of test for ceramic powders - Part 4: Determination of oxygen content in aluminium nitride by XRF analysis
• Effective Date: 07-Dec-2022

Standards Content (Sample)

SLOVENSKI STANDARD
01-februar-2023
Nadomešča:
SIST EN 725-4:2007
Fina keramika (sodobna keramika, sodobna tehnična keramika) - Preskusne
metode za kemične analize praškov aluminijevega nitrida (ISO 21814:2019)
Fine ceramics (advanced ceramics, advanced technical ceramics) - Methods for
chemical analysis of aluminium nitride powders (ISO 21814:2019)
Hochleistungskeramik - Verfahren zur chemischen Analyse von Aluminiumnitridpulvern
(ISO 21814:2019)
Céramiques techniques - Méthodes d'analyse chimique des poudres de nitrure
d'aluminium (ISO 21814:2019)
Ta slovenski standard je istoveten z: EN ISO 21814:2022
ICS:
81.060.30 Sodobna keramika Advanced ceramics
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

EN ISO 21814
EUROPEAN STANDARD
NORME EUROPÉENNE
November 2022
EUROPÄISCHE NORM
ICS 81.060.30 Supersedes EN 725-4:2006
English Version
Fine ceramics (advanced ceramics, advanced technical
ceramics) - Methods for chemical analysis of aluminium
nitride powders (ISO 21814:2019)
Céramiques techniques - Méthodes d'analyse chimique Hochleistungskeramik - Verfahren zur chemischen
des poudres de nitrure d'aluminium (ISO 21814:2019) Analyse von Aluminiumnitridpulvern (ISO
21814:2019)
This European Standard was approved by CEN on 21 November 2022.

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
© 2022 CEN All rights of exploitation in any form and by any means reserved Ref. No. EN ISO 21814:2022 E
worldwide for CEN national Members.

Contents Page
European foreword . 3

European foreword
The text of ISO 21814:2019 has been prepared by Technical Committee ISO/TC 206 "Fine ceramics” of
the International Organization for Standardization (ISO) and has been taken over as EN ISO 21814:2022
by Technical Committee CEN/TC 184 “Advanced technical ceramics” the secretariat of which is held by
DIN.
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 May 2023, and conflicting national standards shall be
withdrawn at the latest by May 2023.
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.
This document supersedes EN 725-4:2006.
Any feedback and questions on this document should be directed to the users’ national standards body.
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 21814:2019 has been approved by CEN as EN ISO 21814:2022 without any modification.

INTERNATIONAL ISO
STANDARD 21814
First edition
2019-02
Fine ceramics (advanced ceramics,
advanced technical ceramics) —
Methods for chemical analysis of
aluminium nitride powders
Céramiques techniques — Méthodes d’analyse chimique des poudres
de nitrure d'aluminium
Reference number
ISO 21814:2019(E)
©
ISO 2019
ISO 21814:2019(E)
© ISO 2019
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: [phone]
Fax: [phone]
Email: [e-mail]
Website: www.iso.org
Published in Switzerland
ii © ISO 2019 – All rights reserved

ISO 21814:2019(E)
Contents Page
Foreword .vi
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 2
4 Analytes and ranges . 2
5 Preparation of the test sample . 2
5.1 General . 2
5.2 Sampling . 3
5.3 Drying . 3
5.4 Weighing . 3
6 Reporting the analytical values . 3
6.1 Number of analyses. 3
6.2 Blank test . 3
6.3 Evaluation of the analytical values. 3
6.4 Expression of the analytical values . 3
7 Determination of the aluminium content . 4
7.1 Classification of the determination methods . 4
7.2 Acid decomposition-ICP-OES method . 4
7.2.1 Principle . 4
7.2.2 Reagents . 4
7.2.3 Apparatus and instruments. 4
7.2.4 Procedure . 5
7.2.5 Blank test . 5
7.2.6 Drawing of the calibration curve . 5
7.2.7 Calculation . 5
7.3 Acid pressure decomposition-CyDTA-zinc back titration method . 5
7.3.1 Principle . 5
7.3.2 Reagents . 6
7.3.3 Apparatus and instruments. 6
7.3.4 Procedure . 8
7.3.5 Blank test . 8
7.3.6 Calculation . 8
8 Determination of the total nitrogen content . 8
8.1 Classification of the determination methods . 8
8.2 Acid pressure decomposition-distillation separation-acidimetric titration method . 9
8.2.1 Principle . 9
8.2.2 Reagents . 9
8.2.3 Apparatus .10
8.2.4 Procedure .12
8.2.5 Recovery measurement .12
8.2.6 Calculation .13
8.3 Direct decomposition-distillation separation-acidimetric titration method .13
8.3.1 Principle .13
8.3.2 Reagents .13
8.3.3 Apparatus .13
8.3.4 Procedure .13
8.3.5 Recovery measurement .13
8.3.6 Calculation .13
8.4 Inert gas fusion-thermal conductivity method .13
8.4.1 Principle .13
8.4.2 Reagents .14
8.4.3 Apparatus .14
ISO 21814:2019(E)
8.4.4 Instrument .14
8.4.5 Procedure .15
8.4.6 Blank test .16
8.4.7 Calculation of the calibration coefficient .16
8.4.8 Calculation .17
9 Determination of the sodium and potassium contents .17
9.1 Classification of the determination methods .17
9.2 Acid pressure decomposition-flame emission method .17
9.2.1 Principle .17
9.2.2 Reagents .17
9.2.3 Instruments .18
9.2.4 Procedure .18
9.2.5 Blank test .18
9.2.6 Drawing of the calibration curve .18
9.2.7 Calculation .18
9.3 Acid pressure decomposition-atomic absorption spectrometry method .19
9.3.1 Principle .19
9.3.2 Reagents .19
9.3.3 Instruments .19
9.3.4 Procedure .19
9.3.5 Blank test .19
9.3.6 Drawing of the calibration curve .19
9.3.7 Calculation .19
10 Determination of the trace element contents .19
10.1 Classification of the determination methods .19
10.2 Acid decomposition-ICP-OES method .20
10.2.1 Principle .20
10.2.2 Reagents .20
10.2.3 Apparatus and instruments.20
10.2.4 Procedure .21
10.2.5 Blank test .21
10.2.6 Drawing of the calibration curve .21
10.2.7 Calculation .21
10.3 Acid pressure decomposition-ICP-OES method .22
10.3.1 General.22
10.3.2 Reagents .22
10.3.3 Apparatus and instruments.22
10.3.4 Procedure .22
10.3.5 Blank test .22
10.3.6 Drawing of the calibration curve .22
10.3.7 Calculation .22
11 Determination of the oxygen content .22
11.1 Principle .22
11.2 Reagents.22
11.3 Apparatus .23
11.4 Instruments .23
11.5 Procedure .23
11.6 Blank test .23
11.7 Calculation of the calibration coefficient .23
11.8 Calculation .23
12 Determination of the carbon content .24
12.1 Classification of the determination methods .24
12.2 Combustion (resistance furnace)-IR absorption spectrometry .24
12.2.1 Principle .24
12.2.2 Reagents .24
12.2.3 Apparatus .24
iv © ISO 2019 – All rights reserved

ISO 21814:2019(E)
12.2.4 Instrument .24
12.2.5 Procedure .25
12.2.6 Blank test .26
12.2.7 Calculation of the calibration coefficient .26
12.2.8 Calculation .27
12.3 Combustion (radio frequency heating furnace)-thermal conductometry .27
12.3.1 Principle .27
12.3.2 Reagents .27
12.3.3 Apparatus .27
12.3.4 Instrument .27
12.3.5 Procedure .28
12.3.6 Blank test .29
12.3.7 Calculation of the calibration coefficient .29
12.3.8 Calculation .29
12.4 Combustion (radio frequency heating furnace)-IR absorption spectrometry .29
12.4.1 Principle .29
12.4.2 Reagents .29
12.4.3 Apparatus .29
12.4.4 Instrument .29
12.4.5 Procedure .30
12.4.6 Blank test .31
12.4.7 Calculation of the calibration coefficient .31
12.4.8 Calculation .31
13 Determination of the fluorine and chlorine contents .31
13.1 Principle .31
13.2 Reagents.31
13.3 Apparatus and instruments .32
13.4 Procedure .33
13.4.1 Extraction of fluorine and chlorine from the sample .33
13.4.2 Determination of the fluorine and chlorine contents .33
13.5 Blank test .33
13.6 Drawing of the calibration curve .34
13.7 Calculation .34
14 Test report .34
Annex A (informative) Analytical results obtained from the round robin test .35
Bibliography .36
ISO 21814:2019(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
constitute an endorsement.
For an explanation on 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 the following
URL: 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.
vi © ISO 2019 – All rights reserved

INTERNATIONAL STANDARD ISO 21814:2019(E)
Fine ceramics (advanced ceramics, advanced technical
ceramics) — Methods for chemical analysis of aluminium
nitride powders
1 Scope
This document specifies methods for the chemical analysis of fine aluminium nitride powders used as
the raw material for fine ceramics.
This document stipulates the determination methods of the aluminium, total nitrogen, boron, calcium,
copper, iron, magnesium, manganese, molybdenum, nickel, potassium, silicon, sodium, titanium,
tungsten, vanadium, zinc, zirconium, carbon, chlorine, fluorine, and oxygen contents in aluminium
nitride powders. The aluminium content is determined by using either an acid pressure decomposition-
CyDTA-zinc back titration method or an acid digestion-inductively coupled plasma-optical emission
spectrometry (ICP-OES) method. The total nitrogen content is determined by using an acid pressure
decomposition-distillation separation-acidimetric titration method, a direct decomposition-distillation
separation-acidimetric titration method, or an inert gas fusion-thermal conductivity method. The
boron, calcium, copper, iron, magnesium, manganese, molybdenum, nickel, potassium, silicon,
sodium, titanium, tungsten, vanadium and zinc contents are determined by using an acid digestion-
ICP-OES method or an acid pressure decomposition-ICP-OES method. The sodium and potassium
contents are determined via an acid pressure decomposition-flame emission method or an acid
pressure decomposition-atomic absorption spectrometry method. The oxygen content is determined
by using an inert gas fusion-IR absorption spectrometry method, while that of carbon is determined
via a combustion-IR absorption spectrometry method or a combustion-conductometry method. The
chlorine and fluorine contents are determined by using a pyrohydrolysation method followed by ion
chromatography or spectrophotometry.
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 2828, Aluminium oxide primarily used for the production of aluminium — Determination of fluorine
content — Alizarin complexone and lanthanum chloride spectrophotometric method
ISO 3696, Water for analytical laboratory use — Specification and test methods
ISO 8656-1, Refractory products — Sampling of raw materials and unshaped products — Part 1:
Sampling scheme
ISO 21068-3:2008, Chemical analysis of silicon-carbide-containing raw materials and refractory
products — Part 3: Determination of nitrogen, oxygen and metallic and oxidic constituents
ISO 21438-2, Workplace atmospheres — Determination of inorganic acids by ion chromatography —
Part 2: Volatile acids, except hydrofluoric acid (hydrochloric acid, hydrobromic acid and nitric acid)
ISO 21438-3, Workplace atmospheres — Determination of inorganic acids by ion chromatography —
Part 3: Hydrofluoric acid and particulate fluorides
ISO 26845:2008, Chemical analysis of refractories — General requirements for wet chemical analysis,
atomic absorption spectrometry (AAS) and inductively coupled plasma atomic emission spectrometry (ICP-
AES) methods
ISO 21814:2019(E)
3 Terms and definitions
No terms and definitions are listed in this document.
ISO and IEC maintain terminological databases for use in standardization at the following addresses:
— ISO Online browsing platform: available at https: //www .iso .org/obp
— IEC Electropedia: available at http: //www .electropedia .org/
4 Analytes and ranges
a) Aluminium (Al), range of 40 % to 70 % (mass fraction).
b) Total nitrogen (T.N), range of 20 % to 40 % (mass fraction).
c) Boron (B), range of 0,001 % to 0,03 % (mass fraction).
d) Calcium (Ca), range of 0,001 % to 0,03 % (mass fraction).
e) Copper (Cu), range of 0,001 % to 0,03 % (mass fraction).
f) Iron (Fe), range of 0,001 % to 0,03 % (mass fraction).
g) Magnesium (Mg), range of 0,001 % to 0,03 % (mass fraction).
h) Manganese (Mn), range of 0,001 % to 0,03 % (mass fraction).
i) Molybdenum (Mo), range of 0,001 % to 0,03 % (mass fraction).
j) Nickel (Ni), range of 0,001 % to 0,03 % (mass fraction).
k) Potassium (K), range of 0,001 % to 0,03 % (mass fraction).
l) Silicon (Si), range of 0,001 % to 0,03 % (mass fraction).
m) Sodium (Na), range of 0,001 % to 0,03 % (mass fraction).
n) Titanium (Ti), range of 0,001% to 0,03 % (mass fraction).
o) Tungsten (W), range of 0,001 % to 0,03 % (mass fraction).
p) Vanadium (V), range of 0,001 % to 0,03 % (mass fraction).
q) Zinc (Zn), range of 0,001 % to 0,03 % (mass fraction).
r) Carbon (C), range of 0,01 % to 6 % (mass fraction).
s) Chlorine (Cl), range of 0,001 % to 0,5 % (mass fraction).
t) Fluorine (F), range of 0,001 % to 0,2 % (mass fraction).
u) Oxygen (O), range of 0,05 % to 5 % (mass fraction).
5 Preparation of the test sample
5.1 General
The sample preparation method shall be in accordance with ISO 8656-1, unless otherwise mutually
agreed upon by the analyser and customer.
2 © ISO 2019 – All rights reserved

ISO 21814:2019(E)
5.2 Sampling
The sample shall be collected in accordance with ISO 8656-1.
5.3 Drying
Place 10 g sample into a flat-type weighing bottle (60 mm × 30 mm) and spread it uniformly over the
bottom of the bottle. Place the bottle in an air bath at 110 °C ± 5 °C for 2 h, uncovered, and cool in a
desiccator (desiccant: magnesium perchlorate), covered, for 1 h.
5.4 Weighing
Weigh the sample to the nearest 0,1 mg of the required quantity using a balance.
6 Reporting the analytical values
6.1 Number of analyses
Analyse the sample twice on different days.
6.2 Blank test
Upon analysis, perform a blank test to correct the measured values.
6.3 Evaluation of the analytical values
When the difference between the two analytical values does not exceed the tolerance value (Table 1),
the average value shall be reported. When the difference between the two analytical values exceeds the
tolerance value, perform two additional analyses. When the difference of these further two analyses
does not exceed the tolerance value, the average value thereof shall be reported. If the difference also
exceeds the tolerance value, the median of four analytical values shall be reported.
6.4 Expression of the analytical values
The analytical values shall be presented in % (mass fraction), in dryness.
a) Aluminium, total nitrogen, and oxygen: express the results in four figures to two decimal places.
b) Others: express the results to three decimal places.
Table 1 — Tolerances for the analytical values
Units: % (mass fraction)
Si, Ti, Fe, Ca, Mg, V, Mo, W, Cu,
Component Al Total N O C
Ni, Zn, Mn, B, Na, K, F, Cl
a c e
0,20 0,20 0,001
Tolerance 0,05 0,005
b d f
0,30 0,40 0,005
a
Acid pressure decomposition-CyDTA-zinc back titration method.
b
Acid decomposition-ICP-OES method.
c
Acid pressure decomposition (or direct decomposition)-distillation separation-acidimetric titration method.
d
Inert gas fusion-thermal conductivity method.
e
Applicable to content of less than 0,01 % (mass fraction).
f
Applicable to content of not less than 0,01 % (mass fraction).
ISO 21814:2019(E)
7 Determination of the aluminium content
7.1 Classification of the determination methods
Method A, acid decomposition-ICP-OES method.
Method B, acid pressure decomposition-CyDTA-zinc back titration method.
If analytical results with four significant figures are required, use method B; if two or three significant
figures are required, method A can be used.
7.2 Acid decomposition-ICP-OES method
7.2.1 Principle
A portion of the sample is decomposed in water, sulfuric acid, and hydrogen peroxide. After making up
to the required volume, the emission intensity of the aluminium present in the test solution is measured
by ICP-OES at one or more of the wavelengths: 396,15 nm, 309,28 nm and 394,40 nm.
7.2.2 Reagents
Reagents of analytical grade shall be used. Reagent solutions shall be preserved in plastic bottles.
7.2.2.1 Water, grade 1 or superior as specified in ISO 3696.
7.2.2.2 Sulfuric acid (1+9, 1+180).
7.2.2.3 Hydrochloric acid (1+1, 1+3).
7.2.2.4 Aluminium stock solution (Al 10 mg/ml).
Wash the surface of the aluminium (more than 99,999 % purity by mass fraction) with a hydrochloric
acid solution (1+3). Wash the oxidised layer with water, ethanol (99,5 %), and diethyl ether. Dry the
aluminium in a desiccator (desiccant: magnesium perchlorate). Weigh 5 g aluminium in a PTFE beaker
and cover with a PTFE watch glass. Add 50 ml hydrochloric acid solution (1+1) and heat to dissolve on
a steam bath. After cooling, transfer the solution to a 500 ml volumetric flask, dilute with water to the
mark and mix well.
NOTE The SI traceable commercial standard solution is also available.
7.2.2.5 Aluminium standard solution (Al 1 mg/ml).
Place 10 ml aluminium stock solution (7.2.2.4) in a 100 ml plastic volumet
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