Determination of certain substances in electrotechnical products - Part 3-1: Screening test methods - Screening of electrotechnical products for lead, mercury, cadmium, total chromium and total bromine using X-ray fluorescence spectrometry

EN-IEC 62321-3-1 describes the screening analysis of five substances, specifically lead (Pb), mercury (Hg), cadmium (Cd), total chromium (Cr) and total bromine (Br) in uniform materials found in electrotechnical products, using the analytical technique of X-ray fluorescence (XRF) spectrometry. It is applicable to polymers, metals and ceramic materials. The test method may be applied to raw materials, individual materials taken from products and “homogenized” mixtures of more than one material. Screening of a sample is performed using any type of XRF spectrometer, provided it has the performance characteristics specified in this test method. Not all types of XRF spectrometers are suitable for all sizes and shapes of sample. Care should be taken to select the appropriate spectrometer design for the task concerned.

Verfahren zur Bestimmung von bestimmten Substanzen in Produkten der Elektrotechnik - Teil 3-1: Ermittlung von Blei (Pb), Quecksilber (Hg), Cadmium (Cd), Gesamtchrom (Cr) und Brom (Br) durch Röntgenfluoreszenz-Spektrometrie in elektrotechnischen Produkten

Détermination de certaines substances dans les produits électrotechniques -- Partie 3-1: Détection du plomb, du mercure, du cadmium, du chrome total et du brome total dans les produits électrotechniques par spectrométrie par fluorescence X

La CEI 62321-3-1:2013 décrit des procédures d'analyse de détection de cinq substances, spécifiquement le plomb (Pb), le mercure (Hg), le cadmium (Cd), le chrome total (Cr) et le brome total (Br) dans des matériaux uniformes utilisés dans les produits électrotechniques en utilisant la technique d'analyse de spectrométrie par fluorescence X (XRF).

Določevanje posameznih snovi v elektrotehničnih izdelkih - 3-1. del: Presejanje elektrotehničnih izdelkov glede svinca, živega srebra, kadmija, celotnega kroma in celotnega broma z rentgensko fluorescenčno spektrometrijo (IEC 62321-3-1:2013)

Standard EN-IEC 62321-3-1opisuje presejalno analizo petih snovi, zlasti svinca (Pb), živega srebra (Hg), kadmija (Cd), skupnega kroma (Cr) in skupnega broma (Br) v homogenih materialih, ki se nahajajo v elektrotehničnih izdelkih, z rentgensko fluorescenčno spektrometrijo (XRF). Velja za polimere, kovine in keramične materiale. Preskusna metoda se lahko uporabi za surovine, posamezne materiale, pridobljene iz proizvodov, in »homogenizirane« mešanice več kot enega materiala. Presejanje vzorca se izvede z uporabo katere koli vrste spektrometra za rentgensko fluorescenčno spektrometrijo, če ima zmogljivostne lastnosti, navedene v tej preskusni metodi. Vse vrste spektrometrov za rentgensko fluorescenčno spektrometrijo niso primerne za vzorce vseh velikosti in oblik. Treba je paziti, da za izbrano nalogo izberete ustrezno zasnovan spektrometer.

General Information

Status
Published
Publication Date
18-May-2014
Current Stage
6060 - National Implementation/Publication (Adopted Project)
Start Date
05-May-2014
Due Date
10-Jul-2014
Completion Date
19-May-2014

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SLOVENSKI STANDARD
SIST EN 62321-3-1:2014
01-junij-2014
1DGRPHãþD
SIST EN 62321:2009
'RORþHYDQMHSRVDPH]QLKVQRYLYHOHNWURWHKQLþQLKL]GHONLKGHO3UHVHMDQMH
HOHNWURWHKQLþQLKL]GHONRYJOHGHVYLQFDåLYHJDVUHEUDNDGPLMDFHORWQHJDNURPDLQ
FHORWQHJDEURPD]UHQWJHQVNRIOXRUHVFHQþQRVSHNWURPHWULMR ,(&
Determination of certain substances in electrotechnical products - Part 3-1: Screening
test methods - Screening of electrotechnical products for lead, mercury, cadmium, total
chromium and total bromine using X-ray fluorescence spectrometry
Verfahren zur Bestimmung von bestimmten Substanzen in Produkten der Elektrotechnik
- Teil 3-1: Ermittlung von Blei (Pb), Quecksilber (Hg), Cadmium (Cd), Gesamtchrom (Cr)
und Brom (Br) durch Röntgenfluoreszenz-Spektrometrie in elektrotechnischen Produkten
Détermination de certaines substances dans les produits électrotechniques -- Partie 3-1:
Détection du plomb, du mercure, du cadmium, du chrome total et du brome total dans
les produits électrotechniques par spectrométrie par fluorescence X
Ta slovenski standard je istoveten z: EN 62321-3-1:2014
ICS:
29.020 Elektrotehnika na splošno Electrical engineering in
general
31.020 Elektronske komponente na Electronic components in
splošno general
SIST EN 62321-3-1:2014 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

---------------------- Page: 1 ----------------------

SIST EN 62321-3-1:2014

---------------------- Page: 2 ----------------------

SIST EN 62321-3-1:2014

EUROPEAN STANDARD
EN 62321-3-1

NORME EUROPÉENNE
April 2014
EUROPÄISCHE NORM


ICS 13.020; 43.040.10 Supersedes EN 62321:2009 (partially)


English version


Determination of certain substances in electrotechnical products -
Part 3-1: Screening -
Lead, mercury, cadmium, total chromium and total bromine by X-ray
fluorescence spectrometry
(IEC 62321-3-1:2013)


Détermination de certaines substances Verfahren zur Bestimmung von
dans les produits électrotechniques - bestimmten Substanzen in Produkten der
Partie 3-1: Méthodes d'essai - Elektrotechnik -
Plomb, du mercure, du cadmium, du Teil 3-1: Screening -
chrome total et du brome total par la Blei, Quecksilber, Cadmium,
spectrométrie par fluorescence X Gesamtchrom und Gesamtbrom durch
(CEI 62321-3-1:2013) Röntgenfluoreszenz-Spektrometrie
(IEC 62321-3-1:2013)



This European Standard was approved by CENELEC on 2013-11-15. CENELEC 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 CENELEC 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 CENELEC member into its own language and notified
to the CEN-CENELEC Management Centre has the same status as the official versions.

CENELEC members are the national electrotechnical committees of Austria, Belgium, Bulgaria, Croatia, Cyprus,
the Czech Republic, Denmark, Estonia, Finland, Former Yugoslav Republic of Macedonia, France, Germany,
Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, the Netherlands, Norway, Poland,
Portugal, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland, Turkey and the United Kingdom.

CENELEC
European Committee for Electrotechnical Standardization
Comité Européen de Normalisation Electrotechnique
Europäisches Komitee für Elektrotechnische Normung

CEN-CENELEC Management Centre: Avenue Marnix 17, B - 1000 Brussels


© 2014 CENELEC - All rights of exploitation in any form and by any means reserved worldwide for CENELEC members.
Ref. No. EN 62321-3-1:2014 E

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SIST EN 62321-3-1:2014
EN 62321-3-1:2014 - 2 -
Foreword
The text of document 111/298/FDIS, future edition 1 of IEC 62321-3-1, prepared by IEC/TC 111
"Environmental standardization for electrical and electronic products and systems" was submitted to the
IEC-CENELEC parallel vote and approved by CENELEC as EN 62321-3-1:2014.
The following dates are fixed:
(dop) 2014-10-25
• latest date by which the document has
to be implemented at national level by
publication of an identical national
standard or by endorsement
• latest date by which the national (dow) 2016-11-15
standards conflicting with the

document have to be withdrawn

EN 62321-3-1:2014 is a partial replacement of EN 62321:2009, forming a structural revision and
generally replacing Clauses 6 and Annex D.
Future parts in the EN 62321 series will gradually replace the corresponding clauses in EN 62321:2009.
Until such time as all parts are published, however, EN 62321:2009 remains valid for those clauses not
yet re-published as a separate part.
Attention is drawn to the possibility that some of the elements of this document may be the subject of
patent rights. CENELEC [and/or CEN] shall not be held responsible for identifying any or all such patent
rights.
Endorsement notice
The text of the International Standard IEC 62321-3-1:2013 was approved by CENELEC as a European
Standard without any modification.

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SIST EN 62321-3-1:2014
- 3 - EN 62321-3-1:2014
Annex ZA
(normative)

Normative references to international publications
with their corresponding European publications

The following documents, in whole or in part, are normatively referenced in this document and are
indispensable for its application. For dated references, only the edition cited applies. For undated
references, the latest edition of the referenced document (including any amendments) applies.

NOTE  When an international publication has been modified by common modifications, indicated by (mod), the relevant EN/HD
applies.

Publication Year Title EN/HD Year




IEC 62321-1 - Determination of certain substances in EN 62321-1 -
electrotechnical products -
Part 1: Introduction and overview


IEC 62321-2 - Determination of certain substances in EN 62321-2 -
electrotechnical products -
Part 2: Disassembly, disjunction and
mechanical sample preparation


ISO/IEC Guide 98-1 - Uncertainty of measurement - - -
Part 1: Introduction to the expression of
uncertainty in measurement

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SIST EN 62321-3-1:2014

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SIST EN 62321-3-1:2014




IEC 62321-3-1

®


Edition 1.0 2013-06




INTERNATIONAL



STANDARD




NORME



INTERNATIONALE
colour

inside










Determination of certain substances in electrotechnical products –

Part 3-1: Screening – Lead, mercury, cadmium, total chromium and total bromine

by X-ray fluorescence spectrometry




Détermination de certaines substances dans les produits électrotechniques –

Partie 3-1: Méthodes d'essai – Plomb, du mercure, du cadmium, du chrome total


et du brome total par la spectrométrie par fluorescence X













INTERNATIONAL

ELECTROTECHNICAL

COMMISSION


COMMISSION

ELECTROTECHNIQUE

PRICE CODE
INTERNATIONALE

CODE PRIX X


ICS 13.020; 43.040.10 ISBN 978-2-83220-839-7



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: 7 ----------------------

SIST EN 62321-3-1:2014
– 2 – 62321-3-1 © IEC:2013
CONTENTS
FOREWORD . 5
INTRODUCTION . 7
1 Scope . 8
2 Normative references . 10
3 Terms, definitions and abbreviations . 10
4 Principle . 10
4.1 Overview . 10
4.2 Principle of test . 11
4.3 Explanatory comments . 11
5 Apparatus, equipment and materials . 12
5.1 XRF spectrometer . 12
5.2 Materials and tools . 12
6 Reagents . 12
7 Sampling . 12
7.1 General . 12
7.2 Non-destructive approach . 12
7.3 Destructive approach. 12
8 Test procedure . 13
8.1 General . 13
8.2 Preparation of the spectrometer . 13
8.3 Test portion . 14
8.4 Verification of spectrometer performance . 14
8.5 Tests . 15
8.6 Calibration . 15
9 Calculations . 16
10 Precision . 17
10.1 General . 17
10.2 Lead . 17
10.3 Mercury . 17
10.4 Cadmium . 17
10.5 Chromium . 18
10.6 Bromine. 18
10.7 Repeatability statement for five tested substances sorted by type of tested
material . 18
10.7.1 General . 18
10.7.2 Material: ABS (acrylonitrile butadiene styrene), as granules and
plates . 18
10.7.3 Material: PE (low density polyethtylene), as granules . 19
10.7.4 Material: PC/ABS (polycarbonate and ABS blend), as granules . 19
10.7.5 Material: HIPS (high impact polystyrene) . 19
10.7.6 Material: PVC (polyvinyl chloride), as granules . 19
10.7.7 Material: Polyolefin, as granules . 19
10.7.8 Material: Crystal glass . 20
10.7.9 Material: Glass . 20
10.7.10 Material: Lead-free solder, chips . 20

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SIST EN 62321-3-1:2014
62321-3-1 © IEC:2013 – 3 –
10.7.11 Material: Si/Al Alloy, chips . 20
10.7.12 Material: Aluminum casting alloy, chips . 20
10.7.13 Material: PCB – Printed circuit board ground to less than 250 µm . 20
10.8 Reproducibility statement for five tested substances sorted by type of tested
material . 20
10.8.1 General . 20
10.8.2 Material: ABS (Acrylonitrile butadiene styrene), as granules and
plates . 21
10.8.3 Material: PE (low density polyethtylene), as granules . 21
10.8.4 Material: PC/ABS (Polycarbonate and ABS blend), as granules . 21
10.8.5 Material: HIPS (high impact polystyrene) . 21
10.8.6 Material: PVC (polyvinyl chloride), as granules . 22
10.8.7 Material: Polyolefin, as granules . 22
10.8.8 Material: Crystal glass . 22
10.8.9 Material: Glass . 22
10.8.10 Material: Lead-free solder, chips . 22
10.8.11 Material: Si/Al alloy, chips . 22
10.8.12 Material: Aluminum casting alloy, chips . 22
10.8.13 Material: PCB – Printed circuit board ground to less than 250 µm . 22
11 Quality control . 23
11.1 Accuracy of calibration . 23
11.2 Control samples . 23
12 Special cases . 23
13 Test report . 23
Annex A (informative) Practical aspects of screening by X-ray fluorescence
spectrometry (XRF) and interpretation of the results . 25
Annex B (informative) Practical examples of screening with XRF . 31
Bibliography . 40

Figure B.1 – AC power cord, X-ray spectra of sampled sections . 32
Figure B.2 – RS232 cable and its X-ray spectra . 33
Figure B.3 – Cell phone charger shown partially disassembled . 34
Figure B.4 – PWB and cable of cell phone charger . 35
Figure B.5 – Analysis of a single solder joint on a PWB . 36
Figure B.6 – Spectra and results obtained on printed circuit board with two collimators . 36
Figure B.7 – Examples of substance mapping on PWBs . 38
Figure B.8 – SEM-EDX image of Pb free solder with small intrusions of Pb (size = 30 µm) . 39

Table 1 – Tested concentration ranges for lead in materials . 8
Table 2 – Tested concentration ranges for mercury in materials . 9
Table 3 – Tested concentration ranges for cadmium in materials . 9
Table 4 – Tested concentration ranges for total chromium in materials . 9
Table 5 – Tested concentration ranges for total bromine in materials . 9
Table 6 – Recommended X-ray lines for individual analytes . 14
Table A.1 – Effect of matrix composition on limits of detection of some controlled
elements . 26

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SIST EN 62321-3-1:2014
– 4 – 62321-3-1 © IEC:2013
Table A.2 – Screening limits in mg/kg for regulated elements in various matrices . 27
Table A.3 – Statistical data from IIS2 . 29
Table A.4 – Statistical data from IIS4 . 30
Table B.1 – Selection of samples for analysis of AC power cord . 32
Table B.2 – Selection of samples (testing locations) for analysis after visual inspection
– Cell phone charger. 34
Table B.3 – Results of XRF analysis at spots (1) and (2) as shown in Figure B.6 . 37

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SIST EN 62321-3-1:2014
62321-3-1 © IEC:2013 – 5 –
INTERNATIONAL ELECTROTECHNICAL COMMISSION
____________

DETERMINATION OF CERTAIN SUBSTANCES
IN ELECTROTECHNICAL PRODUCTS –

Part 3-1: Screening – Lead, mercury, cadmium, total chromium
and total bromine by X-ray fluorescence spectrometry

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 62321-3-1 has been prepared by IEC technical committee 111:
Environmental standardization for electrical and electronic products and systems.
The first edition of IEC 62321:2008 was a 'stand alone' standard that included an introduction,
an overview of test methods, a mechanical sample preparation as well as various test method
clauses.
This first edition of IEC 62321-3-1 is a partial replacement of IEC 62321:2008, forming a
structural revision and generally replacing Clauses 6 and Annex D.
Future parts in the IEC 62321 series will gradually replace the corresponding clauses in
IEC 62321:2008. Until such time as all parts are published, however, IEC 62321:2008 remains
valid for those clauses not yet re-published as a separate part.

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SIST EN 62321-3-1:2014
– 6 – 62321-3-1 © IEC:2013
The text of this standard is based on the following documents:
FDIS Report on voting
111/298/FDIS 111/308/RVD

Full information on the voting for the approval of this standard can be found in the report on
voting indicated in the above table.
This publication has been drafted in accordance with the ISO/IEC Directives, Part 2.
A list of all parts in the IEC 62321 series can be found on the IEC website under the general
title: Determination of certain substances in electrotechnical products
The committee has decided that the contents of this publication will remain unchanged until
the stability date indicated on the IEC web site under "http://webstore.iec.ch" in the data
related to the specific publication. At this date, the publication will be
• reconfirmed,
• withdrawn,
• replaced by a revised edition, or
• amended.

IMPORTANT – The 'colour inside' logo on the cover page of this publication indicates
that it contains colours which are considered to be useful for the correct
understanding of its contents. Users should therefore print this document using a
colour printer.

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SIST EN 62321-3-1:2014
62321-3-1 © IEC:2013 – 7 –
INTRODUCTION
The widespread use of electrotechnical products has drawn increased attention to their impact
on the environment. In many countries 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) and polybrominated diphenyl
ethers (PBDEs)) 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 of concern in
electrotechnical products on a consistent global basis.
WARNING – Persons using this International Standard should be familiar with normal
laboratory practice. This standard 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.

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SIST EN 62321-3-1:2014
– 8 – 62321-3-1 © IEC:2013
DETERMINATION OF CERTAIN SUBSTANCES
IN ELECTROTECHNICAL PRODUCTS –

Part 3-1: Screening – Lead, mercury, cadmium, total chromium
and total bromine by X-ray fluorescence spectrometry



1 Scope
Part 3-1 of IEC 62321 describes the screening analysis of five substances, specifically lead
(Pb), mercury (Hg), cadmium (Cd), total chromium (Cr) and total bromine (Br) in uniform
materials found in electrotechnical products, using the analytical technique of X-ray
fluorescence (XRF) spectrometry.
It is applicable to polymers, metals and ceramic materials. The test method may be applied to
raw materials, individual materials taken from products and “homogenized” mixtures of more
than one material. Screening of a sample is performed using any type of XRF spectrometer,
provided it has the performance characteristics specified in this test method. Not all types of
XRF spectrometers are suitable for all sizes and shapes of sample. Care should be taken to
select the appropriate spectrometer design for the task concerned.
The performance of this test method has been tested for the following substances in various
media and within the concentration ranges as specified in Tables 1 to 5.
Table 1 – Tested concentration ranges for lead in materials
Substance/
Lead
element
Medium/material tested
Unit of
a b d
ABS PE Low- Al, Lead- Ground Crystal PVC Poly-
Parameter
measure
c
alloy Al-Si free PWB glass olefine
steel alloy solder
Concentration
15,7 14 190 22 000 390
or 380 to
e
mg/kg to to 30 to 174 to 240 000 to
concentration 640
954 108 930 23 000 665
range tested
a
Acrylonitrile butadiene styrene.
b
Polyethylene.
c
Printed wiring board.
d
Polyvinyl chloride.
e
This lead concentration was not detectable by instruments participating in tests.

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SIST EN 62321-3-1:2014
62321-3-1 © IEC:2013 – 9 –
Table 2 – Tested concentration ranges for mercury in materials
Substance/element Mercury
Medium/material tested
Parameter Unit of measure
a b
ABS PE
Concentration or concentration range
mg/kg 100 to 942 4 to 25
tested
a
Acrylonitrile butadiene styrene.
b
Polyethylene.

Table 3 – Tested concentration ranges for cadmium in materials
Substance/element Cadmium
Medium/material tested
Parameter Unit of measure
a b
Lead-free solder ABS PE
Concentration or concentration
c
mg/kg 3 10 to 183 19,6 to 141
range tested
a
Acrylonitrile butadiene styrene.
b
Polyethylene.
c
This cadmium concentration was not detectable by instruments participating in tests.

Table 4 – Tested concentration ranges for total chromium in materials
Substance/element Chromium
Medium/material tested
Unit of
Low-
Parameter
Al, Al-Si
measure a b
ABS PE alloy Glass
alloy
steel
Concentration or
concentration range mg/kg 16 to 944 16 to 115 240 130 to 1 100 94
tested
a
 Acrylonitrile butadiene styrene.
b
 Polyethylene.

Table 5 – Tested concentration ranges for total bromine in materials
Substance/element Bromine
Medium/material tested
Unit of
Parameter
measure c a d b
HIPS , ABS PC/ABS PE
Concentration or concentration
mg/kg 25 to 118 400 800 to 2 400 96 to 808
range tested
a
 Acrylonitrile butadiene styrene.
b
 Polyethylene.
c
 High impact polystyrene.
d
 Polycarbonate and ABS blend.

These substances in similar media outside of the specified concentration ranges may be
analysed according to this test method; however, the performance has not been established
for this standard.

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SIST EN 62321-3-1:2014
– 10 – 62321-3-1 © IEC:2013
2 Nor
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