IEC 62321-3-2:2020

Determination of certain substances in electrotechnical products - Part 3-2: Screening - Fluorine, bromine and chlorine in polymer and electronics by combustion-ion chromatography (C-IC)

IEC 62321-3-2:2020 is available as IEC 62321-3-2:2020 RLV which contains the International Standard and its Redline version, showing all changes of the technical content compared to the previous edition.
IEC 62321-3-2:2020 specifies the screening analysis of fluorine, chlorine and bromine in polymers and electronics using combustion-ion chromatography (C-IC). IEC 62321-3-2:2020 cancels and replaces the first edition published in 2013. This edition constitutes a technical revision. This edition includes the following significant technical changes with respect to the previous edition:
a) In the previous edition, a screening test method for bromine (Br) content only was provided. In this edition, a screening test method by C-IC for fluorine (F), chlorine (Cl) and bromine (Br) has been added to the normative part of the document.
b) A screening test method by C-IC for iodine (I) has been added in Annex D (informative).
It has the status of a horizontal standard in accordance with IEC Guide 108.

Détermination de certaines substances dans les produits électrotechniques - Partie 3-2: Détection - Fluor, chlore et brome dans les polymères et les produits électroniques par combustion - Chromatographie ionique (C-CI)

IEC 62321-3-2:2020 est disponible sous forme de IEC 62321-3-2:2020 RLV qui contient la Norme internationale et sa version Redline, illustrant les modifications du contenu technique depuis l'édition précédente.
L'IEC 62321-3-2:2020 spécifie une méthode d’analyse par détection du fluor, du chlore et du brome dans les polymères et les produits électroniques en appliquant la technique de combustion-chromatographie ionique (C-CI). L'IEC 62321-3-2:2020 annule et remplace la première édition publiée en 2013. Cette édition constitue une révision technique.
Cette édition inclut les modifications techniques majeures suivantes par rapport à l'édition précédente.
a) La précédente édition présentait une méthode d’essai de détection pour le brome (Br) seulement. La présente édition ajoute, dans sa partie normative, une méthode d’essai de détection par C-CI pour le fluor (F), le chlore (Cl) et le brome (Br).
b) Une méthode d’essai de détection par C-CI de l’iode a été ajoutée à l’Annexe D (informative).
Elle a le statut d'une norme horizontale conformément au Guide 108 de l'IEC.

General Information

• Status: Published
• Publication Date: 29-Jun-2020
• ICS: 01 - GENERALITIES. TERMINOLOGY. STANDARDIZATION. DOCUMENTATION
• ICS: 13.020.01 - Environment and environmental protection in general
• ICS: 43.040.10 - Electrical and electronic equipment
• Technical Committee: TC 111 - Environmental standardization for electrical and electronic products and systems
• Current Stage: PPUB - Publication issued
• Completion Date: 30-Jun-2020

Standards Content (Sample)

IEC 62321-3-2
Edition 2.0 2020-06
INTERNATIONAL
STANDARD
NORME
INTERNATIONALE
HORIZONTAL STANDARD
NORME HORIZONTALE
Determination of certain substances in electrotechnical products –
Part 3-2: Screening – Fluorine, chlorine and bromine in polymers and electronics
by combustion-ion chromatography (C-IC)
Détermination de certaines substances dans les produits électrotechniques –

Partie 3-2: Détection – Fluor, chlore et brome dans les polymères et les produits

électroniques par combustion-chromatographie ionique (C-CI)
IEC 62321-3-2:2020-06(en-fr)
---------------------- Page: 1 ----------------------
THIS PUBLICATION IS COPYRIGHT PROTECTED
Copyright © 2020 IEC, Geneva, Switzerland

All rights reserved. Unless otherwise specified, no part of this publication may be reproduced or utilized in any form

or by any means, electronic or mechanical, including photocopying and microfilm, without permission in writing from

either IEC or IEC's member National Committee in the country of the requester. If you have any questions about IEC

copyright or have an enquiry about obtaining additional rights to this publication, please contact the address below or

your local IEC member National Committee for further information.

Droits de reproduction réservés. Sauf indication contraire, aucune partie de cette publication ne peut être reproduite ni

utilisée sous quelque forme que ce soit et par aucun procédé, électronique ou mécanique, y compris la photocopie et

les microfilms, sans l'accord écrit de l'IEC ou du Comité national de l'IEC du pays du demandeur. Si vous avez des

questions sur le copyright de l'IEC ou si vous désirez obtenir des droits supplémentaires sur cette publication, utilisez

les coordonnées ci-après ou contactez le Comité national de l'IEC de votre pays de résidence.

IEC Central Office Tel.: [phone]
3, rue de Varembé [e-mail]
CH-1211 Geneva 20 www.iec.ch
Switzerland
About the IEC

The International Electrotechnical Commission (IEC) is the leading global organization that prepares and publishes

International Standards for all electrical, electronic and related technologies.
About IEC publications

The technical content of IEC publications is kept under constant review by the IEC. Please make sure that you have the

latest edition, a corrigendum or an amendment might have been published.

IEC publications search - webstore.iec.ch/advsearchform Electropedia - www.electropedia.org

The advanced search enables to find IEC publications by a The world's leading online dictionary on electrotechnology,

variety of criteria (reference number, text, technical containing more than 22 000 terminological entries in English

committee,…). It also gives information on projects, replaced and French, with equivalent terms in 16 additional languages.

and withdrawn publications. Also known as the International Electrotechnical Vocabulary

(IEV) online.
IEC Just Published - webstore.iec.ch/justpublished

Stay up to date on all new IEC publications. Just Published IEC Glossary - std.iec.ch/glossary

details all new publications released. Available online and once 67 000 electrotechnical terminology entries in English and

a month by email. French extracted from the Terms and definitions clause of IEC
publications issued between 2002 and 2015. Some entries

IEC Customer Service Centre - webstore.iec.ch/csc have been collected from earlier publications of IEC TC 37, 77,

If you wish to give us your feedback on this publication or need 86 and CISPR.
further assistance, please contact the Customer Service
Centre: [e-mail].
A propos de l'IEC

La Commission Electrotechnique Internationale (IEC) est la première organisation mondiale qui élabore et publie des

Normes internationales pour tout ce qui a trait à l'électricité, à l'électronique et aux technologies apparentées.

A propos des publications IEC

Le contenu technique des publications IEC est constamment revu. Veuillez vous assurer que vous possédez l’édition la

plus récente, un corrigendum ou amendement peut avoir été publié.

Recherche de publications IEC - Le premier dictionnaire d'électrotechnologie en ligne au monde,

webstore.iec.ch/advsearchform avec plus de 22 000 articles terminologiques en anglais et en

La recherche avancée permet de trouver des publications IEC français, ainsi que les termes équivalents dans 16 langues

en utilisant différents critères (numéro de référence, texte, additionnelles. Egalement appelé Vocabulaire

comité d’études,…). Elle donne aussi des informations sur les Electrotechnique International (IEV) en ligne.

projets et les publications remplacées ou retirées.
Glossaire IEC - std.iec.ch/glossary

IEC Just Published - webstore.iec.ch/justpublished 67 000 entrées terminologiques électrotechniques, en anglais

Restez informé sur les nouvelles publications IEC. Just et en français, extraites des articles Termes et définitions des

Published détaille les nouvelles publications parues. publications IEC parues entre 2002 et 2015. Plus certaines

Disponible en ligne et une fois par mois par email. entrées antérieures extraites des publications des CE 37, 77,

86 et CISPR de l'IEC.
Service Clients - webstore.iec.ch/csc
Si vous désirez nous donner des commentaires sur cette
publication ou si vous avez des questions contactez-nous:
[e-mail].
Electropedia - www.electropedia.org
---------------------- Page: 2 ----------------------
IEC 62321-3-2
Edition 2.0 2020-06
INTERNATIONAL
STANDARD
NORME
INTERNATIONALE
HORIZONTAL STANDARD
NORME HORIZONTALE
Determination of certain substances in electrotechnical products –
Part 3-2: Screening – Fluorine, chlorine and bromine in polymers and
electronics by combustion-ion chromatography (C-IC)
Détermination de certaines substances dans les produits électrotechniques –

Partie 3-2: Détection – Fluor, chlore et brome dans les polymères et les produits

électroniques par combustion-chromatographie ionique (C-CI)
INTERNATIONAL
ELECTROTECHNICAL
COMMISSION
COMMISSION
ELECTROTECHNIQUE
INTERNATIONALE
ICS 13.020.01; 43.040.10 ISBN 978-2-8322-8256-4

Warning! Make sure that you obtained this publication from an authorized distributor.

Attention! Veuillez vous assurer que vous avez obtenu cette publication via un distributeur agréé.

® Registered trademark of the International Electrotechnical Commission
Marque déposée de la Commission Electrotechnique Internationale
---------------------- Page: 3 ----------------------
– 2 – IEC 62321-3-2:2020 © IEC 2020
CONTENTS

FOREWORD ........................................................................................................................... 5

INTRODUCTION ..................................................................................................................... 7

1 Scope .............................................................................................................................. 8

2 Normative references ...................................................................................................... 9

3 Terms, definitions and abbreviated terms ........................................................................ 9

3.1 Terms and definitions .............................................................................................. 9

3.2 Abbreviated terms ................................................................................................. 10

4 Principle ........................................................................................................................ 11

5 Reagents and materials ................................................................................................. 11

6 Apparatus ...................................................................................................................... 12

7 Sampling ....................................................................................................................... 13

8 Procedure ...................................................................................................................... 14

8.1 Combustion........................................................................................................... 14

8.2 IC analysis ............................................................................................................ 14

8.3 Blank test .............................................................................................................. 14

8.4 Cleaning and recalibration .................................................................................... 14

8.5 Calibration ............................................................................................................ 15

8.6 Measurement of the sample .................................................................................. 15

8.7 Interference .......................................................................................................... 15

9 Calculation .................................................................................................................... 15

10 Precision ....................................................................................................................... 16

11 Quality assurance and control ....................................................................................... 17

11.1 General ................................................................................................................. 17

11.2 Limits of detection (LOD) and limits of quantification (LOQ) .................................. 17

12 Test report ..................................................................................................................... 18

Annex A (informative) Screening for fluorine, chlorine, bromine and iodine in polymers

and electronics by oxygen bomb combustion-ion chromatography ........................................ 19

A.1 General ................................................................................................................. 19

A.2 Principle ............................................................................................................... 19

A.3 Reagents and materials ........................................................................................ 19

A.4 Apparatus ............................................................................................................. 20

A.5 Sampling............................................................................................................... 20

A.6 Procedure ............................................................................................................. 21

A.6.1 General ......................................................................................................... 21

A.6.2 Choice of the absorption solution ................................................................... 21

A.6.3 Preparation of the bomb ................................................................................ 21

A.6.4 Combustion ................................................................................................... 22

A.6.5 Collection of halides ...................................................................................... 22

A.6.6 Cleaning procedure ....................................................................................... 23

A.7 Ion chromatographic analysis ................................................................................ 23

A.8 Calculation ............................................................................................................ 23

A.9 Quality assurance and control and test report ....................................................... 23

Annex B (informative) Screening for fluorine, chlorine, bromine and iodine in polymers

and electronics by oxygen flask combustion-ion chromatography .......................................... 25

B.1 General ................................................................................................................. 25

---------------------- Page: 4 ----------------------
IEC 62321-3-2:2020 © IEC 2020 – 3 –

B.2 Principle ............................................................................................................... 25

B.3 Reagents and materials ........................................................................................ 25

B.4 Apparatus ............................................................................................................. 25

B.5 Sampling............................................................................................................... 26

B.5.1 General ......................................................................................................... 26

B.5.2 Solid and paste-like samples ......................................................................... 26

B.5.3 Liquid samples .............................................................................................. 26

B.6 Procedure ............................................................................................................. 26

B.6.1 General ......................................................................................................... 26

B.6.2 Choice of the absorption solution ................................................................... 26

B.6.3 Combustion ................................................................................................... 27

B.7 Ion chromatographic analysis, calculation, quality assurance and control and

test report ............................................................................................................. 27

Annex C (informative) Example of a combustion device and IC system ................................ 28

Annex D (informative) Screening for iodine in polymers and electronics by

combustion-ion chromatography (C-IC) ................................................................................. 29

D.1 General ................................................................................................................. 29

D.2 Principle ............................................................................................................... 29

D.3 Reagents and materials ........................................................................................ 29

D.4 Apparatus ............................................................................................................. 30

D.5 Sampling............................................................................................................... 31

D.6 Procedure ............................................................................................................. 31

D.6.1 Combustion ................................................................................................... 31

D.6.2 IC analysis ..................................................................................................... 32

D.6.3 Blank test ...................................................................................................... 32

D.6.4 Cleaning and recalibration ............................................................................. 32

D.6.5 Calibration ..................................................................................................... 32

D.7 Measurement of the sample .................................................................................. 33

D.8 Interference .......................................................................................................... 33

D.9 Calculation ............................................................................................................ 33

Annex E (informative) Results of international interlaboratory study (IIS 4A and IIS 3-2) ...... 35

Annex F (informative) Additional results of TG 3-2 test ........................................................ 38

Annex G (informative) Additional validation data .................................................................. 40

Annex H (informative) Additional IC data ............................................................................. 42

Bibliography .......................................................................................................................... 44

Figure A.1 – Example of oxygen bomb combustion device .................................................... 24

Figure B.1 – Example of oxygen flask combustion device ..................................................... 27

Figure B.2 – Example of wrapping of sample ........................................................................ 27

Figure C.1 – Example of a combustion device connected to an ion chromatograph (IC) ........ 28

Figure C.2 – Example of ion chromatographic system ........................................................... 28

Figure H.1 – Example of a chromatogram of the standard solution (4 mg/l of each

standard) by IC ..................................................................................................................... 42

Table 1 – Tested concentration ranges for fluorine by C-IC in various materials ...................... 8

Table 2 – Tested concentration ranges for chlorine by C-IC in various materials ..................... 8

Table 3 – Tested concentration ranges for bromine by C-IC in various materials ..................... 8

---------------------- Page: 5 ----------------------
– 4 – IEC 62321-3-2:2020 © IEC 2020

Table 4 – Fluorine results of international inter-laboratory study (IIS 4A) .............................. 16

Table 5 – Chlorine results of international inter-laboratory study (IIS 4A) .............................. 16

Table 6 – Bromine results of international inter-laboratory study (IIS4A and IIS 3-2) ............. 16

Table 7 – Acceptance criteria of items for quality control ...................................................... 17

Table 8 – Student’s t values used for calculation of method detection limit (MDL = t ×

s ) .................................................................................................................................... 18

n–1

Table E.1 – Mean results and recovery rates for bromine obtained in the IIS4A study

using C-IC ............................................................................................................................ 35

Table E.2 – Statistical bromine data for IIS 4A results using C-IC ......................................... 35

Table E.3 – Mean results and recovery rates for fluorine obtained in the IIS 3-2 study

using C-IC ............................................................................................................................ 36

Table E.4 – Statistical fluorine data for IIS 3-2 results using C-IC ......................................... 36

Table E.5 – Mean results and recovery rates for chlorine obtained in the IIS 3-2 study

using C-IC ............................................................................................................................ 36

Table E.6 – Statistical for chlorine data for IIS 3-2 results using C-IC ................................... 37

Table F.1 – Mean results and recovery rates for bromine obtained in the TG 3-2

internal test study by using C-IC ........................................................................................... 38

Table F.2 – Mean results and recovery rates for bromine obtained in the TG 3-2

internal test study by using oxygen bomb-IC ......................................................................... 39

Table G.1 – General conditions for the combustion furnace and the absorption solution ....... 40

Table G.2 – Additional information – Difference in sample sizes and measured bromine

values in solder paste with burning aid (WO powder) .......................................................... 40

Table G.3 – Additional information – Difference in combustion temperatures and

measured bromine values in solder paste with burning aid (WO3 powder) ........................... 40

Table G.4 – Additional information – Difference in recovery rate of iodine according to

adsorbents (H O , hydrazine) .............................................................................................. 41

2 2

Table H.1 – Typical operating conditions for IC ..................................................................... 42

Table H.2 – Example of fluorine calibration solutions for IC .................................................. 43

Table H.3 – Example of chlorine calibration solutions for IC .................................................. 43

Table H.4 – Example of bromine calibration solutions for IC .................................................. 43

---------------------- Page: 6 ----------------------
IEC 62321-3-2:2020 © IEC 2020 – 5 –
INTERNATIONAL ELECTROTECHNICAL COMMISSION
____________
DETERMINATION OF CERTAIN SUBSTANCES
IN ELECTROTECHNICAL PRODUCTS –
Part 3-2: Screening – Fluorine, chlorine and bromine in polymers and
electronics by combustion-ion chromatography (C-IC)
FOREWORD

1) The International Electrotechnical Commission (IEC) is a worldwide organization for standardization comprising

all national electrotechnical committees (IEC National Committees). The object of IEC is to promote international

co-operation on all questions concerning standardization in the electrical and electronic fields. To this end and

in addition to other activities, IEC publishes International Standards, Technical Specifications, Technical Reports,

Publicly Available Specifications (PAS) and Guides (hereafter referred to as “IEC Publication(s)”). Their

preparation is entrusted to technical committees; any IEC National Committee interested in the subject dealt with

may participate in this preparatory work. International, governmental and non-governmental organizations liaising

with the IEC also participate in this preparation. IEC collaborates closely with the International Organization for

Standardization (ISO) in accordance with conditions determined by agreement between the two organizations.

2) The formal decisions or agreements of IEC on technical matters express, as nearly as possible, an international

consensus of opinion on the relevant subjects since each technical committee has representation from all

interested IEC National Committees.

3) IEC Publications have the form of recommendations for international use and are accepted by IEC National

Committees in that sense. While all reasonable efforts are made to ensure that the technical content of IEC

Publications is accurate, IEC cannot be held responsible for the way in which they are used or for any

misinterpretation by any end user.

4) In order to promote international uniformity, IEC National Committees undertake to apply IEC Publications

transparently to the maximum extent possible in their national and regional publications. Any divergence between

any IEC Publication and the corresponding national or regional publication shall be clearly indicated in the latter.

5) IEC itself does not provide any attestation of conformity. Independent certification bodies provide conformity

assessment services and, in some areas, access to IEC marks of conformity. IEC is not responsible for any

services carried out by independent certification bodies.

6) All users should ensure that they have the latest edition of this publication.

7) No liability shall attach to IEC or its directors, employees, servants or agents including individual experts and

members of its technical committees and IEC National Committees for any personal injury, property damage or

other damage of any nature whatsoever, whether direct or indirect, or for costs (including legal fees) and

expenses arising out of the publication, use of, or reliance upon, this IEC Publication or any other IEC Publications.

8) Attention is drawn to the Normative references cited in this publication. Use of the referenced publications is

indispensable for the correct application of this publication.

9) Attention is drawn to the possibility that some of the elements of this IEC Publication may be the subject of patent

rights. IEC shall not be held responsible for identifying any or all such patent rights.

International Standard IEC 62321-3-2 has been prepared by IEC technical committee 111:

Environmental standardization for electrical and electronic products and systems.

This second edition cancels and replaces the first edition published in 2013. This edition

constitutes a technical revision.

This edition includes the following significant technical changes with respect to the previous

edition:

a) In the previous edition, a screening test method for bromine (Br) content only was provided.

In this edition, a screening test method by C-IC for fluorine (F), chlorine (Cl) and bromine

(Br) has been added to the normative part of the document.

b) A screening test method by C-IC for iodine (I) has been added in Annex D (informative).

---------------------- Page: 7 ----------------------
– 6 – IEC 62321-3-2:2020 © IEC 2020
The text of this International Standard is based on the following documents:
FDIS Report on voting
111/573/FDIS 111/577/RVD

Full information on the voting for the approval of this International Standard can be found in the

report on voting indicated in the above table.

This document has been drafted in accordance with the ISO/IEC Directives, Part 2.

A list of all parts in the IEC 62321 series, published under the general title Determination of

certain substances in electrotechnical products can be found on the IEC website.

The committee has decided that the contents of this document will remain unchanged until the

stability date indicated on the IEC website under "http://webstore.iec.ch" in the data related to

the specific document. At this date, the document will be
• reconfirmed,
• withdrawn,
• replaced by a revised edition, or
• amended.
---------------------- Page: 8 ----------------------
IEC 62321-3-2:2020 © IEC 2020 – 7 –
INTRODUCTION

The widespread use of electrotechnical products has drawn increased attention to their impact

on the environment. In many countries all over the world this has resulted in the adaptation of

regulations affecting wastes, substances and energy use of electrotechnical products.

The use of certain substances (e.g. lead (Pb), cadmium (Cd), polybrominated diphenyl ethers

(PBDEs) and phthalates) in electrotechnical products is a source of concern in current and

proposed regional legislation.

The purpose of the IEC 62321 series is therefore to provide test methods that will allow the

electrotechnical industry to determine the levels of certain substances in electrotechnical

products on a consistent global basis.

The first edition of IEC 62321-3-2 (2013) was published to address screening for total bromine.

This document (revised edition of IEC 62321-3-2) describes the test methods to quantify

halogen (fluorine, chlorine and bromine) in polymers and electronics by C-IC in the normative

section and to quantify iodine (I) in an informative Annex D.

In addition, information on oxygen bomb combustion-ion chromatography and oxygen flask-ion

chromatography is provided in Annex A (informative) and Annex B (informative).

WARNING – Persons using this document should be familiar with normal laboratory practice.

This document does not purport to address all of the safety problems, if any, associated with

its use. It is the responsibility of the user to establish appropriate safety and health practices

and to ensure compliance with any national regulatory conditions.
---------------------- Page: 9 ----------------------
– 8 – IEC 62321-3-2:2020 © IEC 2020
DETERMINATION OF CERTAIN SUBSTANCES
IN ELECTROTECHNICAL PRODUCTS –
Part 3-2: Screening – Fluorine, chlorine and bromine in polymers and
electronics by combustion-ion chromatography (C-IC)
1 Scope

This part of IEC 62321 specifies the screening analysis of fluorine, chlorine and bromine in

polymers and electronics using combustion-ion chromatography (C-IC). A C-IC screening

analysis procedure for iodine can be found in Annex D.

This test method has been evaluated for ABS (acrylonitrile butadiene styrene), EMC (epoxy

moulding compound), PE (polyethylene) and PC (polycarbonate) within the concentration

ranges as specified in Table 1, Table 2 and Table 3. (Detailed results are shown in Table E.1

to Table E.6, and in Annex F (Table F.1 and Table F.2).

The use of this method for other types of materials or concentration ranges outside those

specified below has not been evaluated.
Table 1 – Tested concentration ranges for fluorine by C-IC in PC
Substance/element Fluorine
Polymer PC
Unit of
measure
Concentration or
mg/kg
575
concentration range tested
Table 2 – Tested concentration ranges for chlorine by C-IC in PE
Substance/element Chlorine
Polymer PE
Unit of
measure
Concentration or
mg/kg 102,2
concentration range tested
Table 3 – Tested concentration ranges for bromine by C-IC in various materials
Substance/element Bromine
Polymer ABS EMC PE
Unit of
measure
Concentration or
124 to 890 195 to 976 96
mg/kg
concentration range tested

This horizontal standard is primarily intended for use by technical committees in the preparation

of standards in accordance with the principles laid down in IEC Guide 108.

One of the responsibilities of a technical committee is, wherever applicable, to make use of

horizontal standards in the preparation of its publicatio
...