ISO 24181-1

Rare earth — Determination of non-rare earth impurities in individual rare earth metals and their oxides — ICP-AES — Part 1: Analysis of Al, Ca, Mg, Fe and Si

Terres rares — Détermination des impuretés de terres non rares dans les métaux de terres rares individuels et leurs oxydes — ICP-AES — Partie 1: Analyse de Al, Ca, Mg, Fe et Si

General Information

• Status: Not Published
• ICS: 13.030.30 - Special wastes
• Technical Committee: ISO/TC 298 - Rare earth
• Drafting Committee: ISO/TC 298/WG 4 - Testing and Analysis
• Current Stage: 6000 - International Standard under publication
• Completion Date: 09-Jul-2024

Standards Content (Sample)

FINAL DRAFT
International
Standard
ISO/FDIS 24181-1
ISO/TC 298
Rare earth — Determination of non-
Secretariat: SAC
rare earth impurities in individual
Voting begins on:
rare earth metals and their oxides
2024-05-13
— ICP-AES —
Voting terminates on:
2024-07-08
Part 1:
Analysis of Al, Ca, Mg, Fe and Si
Terres rares — Détermination des impuretés de terres non rares
dans les métaux de terres rares individuels et leurs oxydes — ICP-
AES —
Partie 1: Analyse de Al, Ca, Mg, Fe et Si
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 SUPPOR TING DOCUMENTATION.
IN ADDITION TO THEIR EVALUATION AS
BEING ACCEPTABLE FOR INDUSTRIAL, TECHNO-
LOGICAL, COMMERCIAL AND USER PURPOSES, DRAFT
INTERNATIONAL STANDARDS MAY ON OCCASION HAVE
TO BE CONSIDERED IN THE LIGHT OF THEIR POTENTIAL
TO BECOME STAN DARDS TO WHICH REFERENCE MAY BE
MADE IN NATIONAL REGULATIONS.
Reference number
ISO/FDIS 24181-1:2024(en) © ISO 2024

FINAL DRAFT
ISO/FDIS 24181-1:2024(en)
International
Standard
ISO/FDIS 24181-1
ISO/TC 298
Rare earth — Determination of non-
Secretariat: SAC
rare earth impurities in individual
Voting begins on:
rare earth metals and their oxides
— ICP-AES —
Voting terminates on:
Part 1:
Analysis of Al, Ca, Mg, Fe and Si
Terres rares — Détermination des impuretés de terres non rares
dans les métaux de terres rares individuels et leurs oxydes —
ICP-AES —
Partie 1: Analyse de Al, Ca, Mg, Fe et Si
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 SUPPOR TING DOCUMENTATION.
© ISO 2024
IN ADDITION TO THEIR EVALUATION AS
All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may
BEING ACCEPTABLE FOR INDUSTRIAL, TECHNO-
LOGICAL, COMMERCIAL AND USER PURPOSES, DRAFT
be reproduced or utilized otherwise in any form or by any means, electronic or mechanical, including photocopying, or posting on
INTERNATIONAL STANDARDS MAY ON OCCASION HAVE
the internet or an intranet, without prior written permission. Permission can be requested from either ISO at the address below
TO BE CONSIDERED IN THE LIGHT OF THEIR POTENTIAL
or ISO’s member body in the country of the requester.
TO BECOME STAN DARDS TO WHICH REFERENCE MAY BE
MADE IN NATIONAL REGULATIONS.
ISO copyright office
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva
Phone: [phone]
Email: [e-mail]
Website: www.iso.org
Published in Switzerland Reference number
ISO/FDIS 24181-1:2024(en) © ISO 2024

ii
ISO/FDIS 24181-1:2024(en)
Contents Page
Foreword .iv
Introduction .v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 1
4 Principle . 3
5 Reagent . 4
6 Apparatus . 4
6.1 Volumetric glassware .4
6.2 Inductively coupled plasma atomic emission spectrometer .4
6.2.1 General .4
6.2.2 Line spectra selection .4
7 Procedure . 5
7.1 Weighing the test portion .5
7.2 Sample preparation .6
7.3 Preparation of calibration solutions .6
7.4 Measurements . .7
7.4.1 Instrument set-up .7
7.4.2 Measurement of the calibration solution and calibration curve construction .7
7.4.3 Measurement of the test solution .7
8 Calculation and expression of results . 7
8.1 Method of calculation .7
8.2 Precision . . .8
8.2.1 Interlaboratory test .8
8.2.2 Statistical analysis .8
9 Test report . 8
Annex A (informative) Interlaboratory test results . 9
Annex B (informative) Regression formulae of precision . 10
Bibliography .11

iii
ISO/FDIS 24181-1:2024(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 298, Rare earth.
A list of all parts in the ISO 24181 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/FDIS 24181-1:2024(en)
Introduction
Atomic spectroscopy has been recognised as the most common technique for trace elemental determinations.
Although atomic absorption spectroscopy is limited to determination of one element at a time, many elements
are analysed routinely at the same time by inductively coupled plasma atomic emission spectroscopy
(ICP-AES), which utilises the inductively coupled plasma (ICP) as an excitation source for atomic emission
spectrometry (AES). Several thousands of these instruments are in routine use throughout the world.
ICP-AES is the most common technique for trace elemental determinations, particularly for the analysis of
impurities. This method has been demonstrated to feature a linear response over a wide dynamic range,
a low chemical interference/matrix effect, good stability and good reproducibility. It demonstrates a low
detection limit and various sample introduction techniques are available for different sample analysis
demands.
In rare earth metals and oxides, during processing ores of rare earth elements, Aluminum(Al), calcium(Ca),
magnesium(Mg), iron(Fe) and silicon(Si) are contained as impurities. ICP-AES is well-suited for the
quantification of non-rare earth impurities in a matrix containing rare earth elements. Additionally, the ICP-
AES technique also offers high resolution for rare earth elements as rare earth elements exhibits line-rich
emission spectra.
This document provides a guide for chemical analysis of materials for producers, consumers, and traders in
the field of rare-earth metals and their oxides. This document is anticipated to reduce discrepancies caused
by inconsistencies in the analytical procedures used when working with rare earth metals and their oxides.

v
FINAL DRAFT International Standard ISO/FDIS 24181-1:2024(en)
Rare earth — Determination of non-rare earth impurities in
individual rare earth metals and their oxides — ICP-AES —
Part 1:
Analysis of Al, Ca, Mg, Fe and Si
WARNING — The use of this document can involve hazardous chemicals, materials, operations and
equipment. This document does not purport to address any safety problems associated with its use. It
is the responsibility of the user of this document to establish appropriate safety and health practices
and to determine the applicability of regulatory limitations before use according to ISO 15202-2 and
ISO 15202-3.
1 Scope
This document describes procedures for the determination of non-rare earth impurities in individual rare
earth metals and their oxides through the use of inductively coupled plasma atomic emission spectroscopy
(ICP-AES). Magnesium (Mg), aluminum (Al), silicon (Si), calcium (Ca) and iron (Fe) are included as non-
rare earth impurity elements, and the measurement ranges for each impurity element are specified. The
applicable measurement range (mass fraction %) of magnesium, aluminum, silicon and calcium is from
0,001 to 0,2, and that of iron is from 0,001 to 0,5. The verified measurement ranges in the interlaboratory
tests are described later in this document.
2 Normative references
The following documents are referred to in the text in such a way that some or all of their content dictates
requirements or specifications of this d
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Secretariat: SAC
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Rare Earth earth — Determination of non-rare earth impurities in
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Terres rares — Détermination des impuretés de terres non rares dans les métaux de terres rares individuels et
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ISO/FDIS 24181-1:20232024(en) Formatted: Font: 11 pt, Bold, English (United Kingdom)
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© ISO 2024
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All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication
may be reproduced or utilisedutilized otherwise in any form or by any means, electronic or mechanical, including Formatted: Left: 1.5 cm, Right: 1.5 cm, Header
distance from edge: 1.27 cm, Footer distance from
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.
Commented [eXtyles1]: The reference "ISO 2024" is to a
withdrawn standard
ISO copyright office
Formatted: Default Paragraph Font
CP 401 • Ch. de Blandonnet 8
CH-1214 Vernier, Geneva Formatted: Default Paragraph Font
Phone: + 41 22 749 01 11
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Formatted: French (France)
EmailE-mail: [e-mail]
Formatted: French (France)
Website: www.iso.orgwww.iso.org
Formatted: French (France)
Published in Switzerland
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numbers, Adjust space between Latin and Asian text,
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ii © ISO 2023 – All rights reserved

ISO/FDIS 24181-1:2024(en)
Formatted: Font: 11 pt, Bold, English (United Kingdom)
Formatted: Font: Bold
Formatted: HeaderCentered, Left, Space After: 0 pt,
Contents
Line spacing: single
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Foreword . v
Adjust space between Asian text and numbers
Introduction . vi
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 2
4 Principle . 4
5 Reagent . 5
6 Apparatus . 5
6.1 Volumetric glassware . 5
6.2 Inductively coupled plasma atomic emission spectrometer . 5
6.2.1 General. 5
6.2.2 Line spectra selection . 5
7 Procedure . 7
7.1 Weighing the test portion . 7
7.2 Sample preparation . 7
7.3 Preparation of calibration solutions . 7
7.4 Measurements . 8
7.4.1 Instrument set-up . 8
7.4.2 Measurement of the calibration solution and calibration curve construction . 8
7.4.3 Measurement of the test solution . 8
8 Calculation and expression of results . 8
8.1 Method of calculation . 8
8.2 Precision . 9
8.2.1 Interlaboratory test . 9
8.2.2 Statistical analysis . 9
9 Test report . 9
Annex A (informative) Interlaboratory test results . 10
Annex B (informative) Regression formulae of precision . 12
Bibliography . 13

Foreword . iv
Introduction . v
1 Scope . 1
2 Normative references . 1
3 Terms and definitions . 2
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4 Principle . 3
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5 Reagent . 3
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6 Apparatus . 4
6.1 Volumetric glassware . 4
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6.2 Inductively coupled plasma atomic emission spectrometer . 4
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© ISO 2024 – All rights reserved
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ISO/FDIS 24181-1:20232024(en) Formatted: Font: 11 pt, Bold, English (United Kingdom)
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7 Procedure . 5
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7.1 Weighing the test portion . 5
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7.2 Sample preparation . 5
7.3 Preparation of calibration solutions . 5
7.4 Measurements . 6
8 Calculation and expression of results . 7
8.1 Method of calculation . 7
8.2 Precision . 7
9 Test report . 7
Bibliography . 11

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single
iv © ISO 2023 – All rights reserved

ISO/FDIS 24181-1:2024(en)
Formatted: Font: 11 pt, Bold, English (United Kingdom)
Formatted: Font: Bold
Formatted: HeaderCentered, Left, Space After: 0 pt,
Foreword
Line spacing: single
Formatted: Adjust space between Latin and Asian text,
ISO (the International Organization for Standardization) is a worldwide federation of national standards
Adjust space between Asian text and numbers
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).
Formatted: English (United Kingdom)
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.www.iso.org/patents. ISO shall not be held responsible for identifying any or all such
patent rights.
Any trade name
...