Recycling of rare earth elements -- Methods for the measurement of rare earth elements in industrial waste and end-of-life products

Recyclage des éléments des terres rares -- Méthodes pour le mesurage des éléments des terres rares dans les déchets industriels et les produits en fin de vie

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ISO/PRF TS 22451 - Recycling of rare earth elements -- Methods for the measurement of rare earth elements in industrial waste and end-of-life products
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TECHNICAL ISO/TS
SPECIFICATION 22451
First edition
Recycling of rare earth elements —
Methods for the measurement of rare
earth elements in industrial waste and
end-of-life products
PROOF/ÉPREUVE
Reference number
ISO/TS 22451:2021(E)
ISO 2021
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ISO/TS 22451:2021(E)
COPYRIGHT PROTECTED DOCUMENT
© ISO 2021

All rights reserved. Unless otherwise specified, or required in the context of its implementation, no part of this publication may

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Published in Switzerland
ii PROOF/ÉPREUVE © ISO 2021 – All rights reserved
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ISO/TS 22451:2021(E)
Contents Page

Foreword ........................................................................................................................................................................................................................................iv

Introduction ..................................................................................................................................................................................................................................v

1 Scope ................................................................................................................................................................................................................................. 1

2 Normative references ...................................................................................................................................................................................... 1

3 Terms, definitions and abbreviated terms ................................................................................................................................ 1

3.1 Terms and definitions ....................................................................................................................................................................... 1

3.2 Abbreviated terms ............................................................................................................................................................................... 1

4 Sampling ........................................................................................................................................................................................................................ 2

4.1 Industrial waste ..................................................................................................................................................................................... 2

4.1.1 Processing waste.............................................................................................................................................................. 2

4.1.2 Scrap ........................................................................................................................................................................................... 2

4.2 End-of-life products ............................................................................................................................................................................ 2

4.2.1 Magnets .................................................................................................................................................................................... 2

4.2.2 NiMH batteries ...................................................................... ............................................................................................. 2

4.2.3 Phosphors .............................................................................................................................................................................. 2

5 Selection of measurement methods ................................................................................................................................................. 3

6 Measurement methods .................................................................................................................................................................................. 3

6.1 X-ray fluorescence spectrometry (XRF) ............................................................................................................................ 3

6.1.1 General...................................................................................................................................................................................... 3

6.1.2 Sample preparation ....................................................................................................................................................... 3

6.1.3 Calibration ............................................................................................................................................................................. 4

6.1.4 Analysis and calculation ............................................................................................................................................ 4

6.2 ICP-OES .......................................................................................................................................................................................................... 5

6.2.1 General...................................................................................................................................................................................... 5

6.2.2 Sample preparation ....................................................................................................................................................... 5

6.2.3 Calibration ............................................................................................................................................................................. 5

6.2.4 Analysis and calculation ............................................................................................................................................ 5

6.3 ICP-MS ............................................................................................................................................................................................................ 6

6.3.1 General...................................................................................................................................................................................... 6

6.3.2 Sample preparation ....................................................................................................................................................... 6

6.3.3 Calibration ............................................................................................................................................................................. 6

6.3.4 Analysis and calculation ............................................................................................................................................ 6

Annex A (informative) Example measurement report ...................................................................................................................... 8

Bibliography ................................................................................................................................................................................................................................ 9

© ISO 2021 – All rights reserved PROOF/ÉPREUVE iii
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ISO/TS 22451:2021(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 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.

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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ISO/TS 22451:2021(E)
Introduction

With technical advancement, rare earth elements (REEs) are increasingly important due to their

importance in a number of applications, including green technologies. However, there are high supply

risks arising from the dependence on a single source of extraction. Recycling and systemic management

of rare earth elements are key issues for solving the waste and supply risks of REEs.

In order to efficiently recycle and systemically manage rare earth elements, a standard measurement

method of REEs in industrial wastes and end-of-life cycled products is needed. Industrial wastes and

end-of-life products can be found in solid, solid-liquid mixture and liquid forms. For example, machining

waste contains chips and flakes with coolant oils, greases and numerous other forms of aqueous and

non-aqueous contaminants. Similarly, waste liquid slurries contain REEs, as in LEDs, and batteries

contain numerous acids, bases etc. Furthermore, in order to verify the information provided by the

producer about REEs in the waste, standardized measurement procedure is necessary.

There are several scientific methods for quantitatively measure REEs in matters, such as X-ray

fluorescence (XRF), inductively coupled plasma mass spectroscopy (ICP-MS), inductively coupled

plasma optical emission spectroscopy (ICP-OES) and glow discharge mass spectrometry (GD-MS).

However, these different characterization techniques often offer dissimilar measurement results

depending on the composition and physical state of the sample under observation. This is another

reason to establish standard measurement methods.

This document provides a brief overview and several measurement methods for REEs in industrial

wastes and end-of-life products. Sample preparation methods are also provided. The accurate

measurement of rare earth content (e.g. in ppm range) is still under active research and is not covered

by this document. However, this document does provide measurement methods for identifying the

presence and approximate content of rare earth elements.
This document is designed to be used with ISO 22450.
© ISO 2021 – All rights reserved PROOF/ÉPREUVE v
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TECHNICAL SPECIFICATION ISO/TS 22451:2021(E)
Recycling of rare earth elements — Methods for the
measurement of rare earth elements in industrial waste
and end-of-life products
1 Scope

This document provides measurement methods for quantifying rare earth elements (REEs) in industrial

wastes and end-of-life products in solid, solid-liquid mixture or liquid forms. It provides an overview of

sample preparation and measurement of REEs in industrial waste and end-of-life products.

WARNING — The use of this document can involve hazardous materials, operations and

equipment. This document does not 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.

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 22444-2, Rare earth — Vocabulary — Part 2: Metals and their alloys

ISO 22450, Recycling of rare earth elements — Requirements for providing information on industrial waste

and end-of-life products
3 Terms, definitions and abbreviated terms
3.1 Terms and definitions

For the purposes of this document, the terms and definitions given in ISO 22444-2 and ISO 22450 apply.

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/
3.2 Abbreviated terms
REE rare earth element
TREE total rare earth element content
ppm parts per million
XRF X-ray fluorescence spectrometry
EDXRF energy dispersive X-ray fluorescence spectrometry
© ISO 2021 – All rights reserved PROOF/ÉPREUVE 1
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ISO/TS 22451:2021(E)
WDXRF wavelength dispersive X-ray fluorescence spectrometry
ICP-MS inductively coupled plasma mass spectrometry
ICP-OES inductively coupled plasma optical emission spectrometry

[also referred to as inductively coupled plasma atomic emission spectroscopy (ICP-AES)]

4 Sampling
4.1 Industrial waste
4.1.1 Processing waste

Processing waste can be of solid or liquid type. In the case of solid waste, sampling can be done directly

without any special pre-treatment. In the case of liquid waste, it should be ensured that the sample is

safe to handle and does not contain any hazardous components. For that purpose, the pH of the waste

should be checked and neutralized. After the safety of the liquid waste is established, it should be

prepared for analysis. Because processing waste can be of numerous types, a single sampling procedure

is not recommended in this document. However, reg
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