Determination of certain substances in electrotechnical products - Part 3-2: Screening test methods - Screening of total bromine in polymers and electronics by combustion - Ion chromatography (C-IC)

EN-IEC 62321-3-2 specifies the screening analysis of the total bromine (Br) in homogeneous materials found in polymers and electronics by using the analytical technique of combustion ion chromatography (C-IC). This test method has been evaluated for ABS (acrylonitrile butadiene styrene), EMC (epoxy molding compound), and PE (polyethylene) within the concentration ranges as specified in Table 1. The use of this method for other types of materials or concentration ranges outside those specified below has not been evaluated.

Verfahren zur Bestimmung von bestimmten Substanzen in Produkten der Elektrotechnik - Teil 3-2: Ermittlung des Gesamtbromgehalts in elektronischen und elektrischen Geräten durch Verbrennungsaufschluss - Ionen Chromatographie (C-IC)

Détermination de certaines substances dans les produits électrotechniques - Partie 3-2: Détection du brome total dans les produits électriques et électroniques par Combustion-Chromatographie d'ionisation (C-IC)

La CEI 62321-3-2:2013 définit l'analyse par détection du brome total (Br) dans des matériaux homogènes que l'on trouve dans les polymères et les produits électroniques en utilisant la technique analytique de combustion de la chromatographie d'ionisation (C-IC).

Določevanje posameznih snovi v elektrotehničnih izdelkih - 3-2. del: Presejanje skupnega broma v električnih in elektronskih izdelkih z zgorevalno ionsko kromatografijo (C-IC) (IEC 62321-3-2:2013)

Standard EN-IEC 62321-3-2 določa presejalne analize skupnega broma (Br) v homogenih materialih, ki jih najdemo v polimerih in elektroniki, s pomočjo analitične tehnike zgorevalne ionske kromatografije (C-IC). Ta preskusna metoda je bila ocenjena za ABS (akrilonitril-butadien-stiren), EMC (epoksi zmesi za oblikovanje) in PE (polietilen) v koncentracijah, določenih v tabeli 1. Uporaba te metode za druge vrste materialov ali razpon koncentracij zunaj tistih, navedenih spodaj, ni bila ocenjena.

General Information

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

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SLOVENSKI STANDARD
SIST EN 62321-3-2:2014
01-junij-2014
1DGRPHãþD
SIST EN 62321:2009
'RORþHYDQMHSRVDPH]QLKVQRYLYHOHNWURWHKQLþQLKL]GHONLKGHO3UHVHMDQMH
VNXSQHJDEURPDYHOHNWULþQLKLQHOHNWURQVNLKL]GHONLK]]JRUHYDOQRLRQVNR
NURPDWRJUDILMR &,&  ,(&
Determination of certain substances in electrotechnical products - Part 3-2: Screening
test methods - Screening of total bromine in polymers and electronics by combustion -
Ion chromatography (C-IC)
Verfahren zur Bestimmung von bestimmten Substanzen in Produkten der Elektrotechnik
- Teil 3-2: Ermittlung des Gesamtbromgehalts in elektronischen und elektrischen Geräten
durch Verbrennungsaufschluss - Ionen Chromatographie (C-IC)
Détermination de certaines substances dans les produits électrotechniques - Partie 3-2:
Détection du brome total dans les produits électriques et électroniques par Combustion-
Chromatographie d'ionisation (C-IC)
Ta slovenski standard je istoveten z: EN 62321-3-2:2014
ICS:
29.020 Elektrotehnika na splošno Electrical engineering in
general
31.020 Elektronske komponente na Electronic components in
splošno general
SIST EN 62321-3-2:2014 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN 62321-3-2:2014

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SIST EN 62321-3-2:2014

EUROPEAN STANDARD
EN 62321-3-2

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 3-2: Screening -
Total bromine in polymers and electronics
by Combustion - Ion Chromatography
(IEC 62321-3-2:2013)


Détermination de certaines substances Verfahren zur Bestimmung von
dans les produits électrotechniques - bestimmten Substanzen in Produkten der
Partie 3-2: Méthodes d'essai - Elektrotechnik -
Brome total dans les polymères et les Teil 3-2: Screening -
produits électriques par Combustion - Gesamtbrom in Polymeren und Elektronik
Chromatographie d'Ionisation durch Verbrennungsaufschluss -
(CEI 62321-3-2:2013) Ionen-Chromatographie
(IEC 62321-3-2:2013)



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 62321-3-2:2014 E

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SIST EN 62321-3-2:2014
EN 62321-3-2:2014 - 2 -

Foreword
The text of document 111/300/FDIS, future edition 1 of IEC 62321-3-2, 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 62321-3-2:2014.
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
(dow) 2016-11-15
• latest date by which the national
standards conflicting with the

document have to be withdrawn

EN 62321-3-2:2014 is a partial replacement of EN 62321:2009, introduces a new clause in the IEC 62321
series.
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 62321-3-2:2013 was approved by CENELEC as a European
Standard without any modification.
In the official version, for Bibliography, the following notes have to be added for the standards indicated:
IEC 60754-2 NOTE Harmonised as EN 60754-2 (not modified).
ISO 5667-1 NOTE Harmonised as EN ISO 5667-1 (not modified).

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SIST EN 62321-3-2:2014
- 3 - EN 62321-3-2:2014
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 60754-1 2011 Test on gases evolved during combustion of EN 60754-1 2013
materials from cables -
Part 1: Determination of the halogen acid gas
content


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


IEC 62321-3-1 - Determination of certain substances in EN 62321-3-1 -
electrotechnical products -
Part 3-1: Screening electrotechnical products
for lead, mercury, cadmium, total chromium
and total bromine using X-ray Fluorescence
Spectrometry

ISO 3696 - Water for analytical laboratory use - EN ISO 3696 -
Specification and test methods


ISO 8466-1 - Water quality - Calibration and evaluation of - -
analytical methods and estimation of
performance characteristics -
Part 1: Statistical evaluation of the linear
calibration function


ISO 10304-1 2006 Water quality - Determination of dissolved EN ISO 10304-1 -
anions by liquid chromatography of ions -
Part 1: Determination of bromide, chloride,
fluoride, nitrate, nitrite, phosphate and
sulphate

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SIST EN 62321-3-2:2014

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SIST EN 62321-3-2:2014



IEC 62321-3-2

®


Edition 1.0 2013-06




INTERNATIONAL



STANDARD




NORME



INTERNATIONALE











Determination of certain substances in electrotechnical products –

Part 3-2: Screening – Total bromine in polymers and electronics by Combustion

– Ion Chromatography




Détermination de certaines substances dans les produits électrotechniques –

Partie 3-2: Méthodes d'essai – Brome total dans les polymères et les produits


électriques par Combustion – Chromatographie d'Ionisation













INTERNATIONAL

ELECTROTECHNICAL

COMMISSION


COMMISSION

ELECTROTECHNIQUE

PRICE CODE
INTERNATIONALE

CODE PRIX V


ICS 13.020; 43.040.10 ISBN 978-2-83220-840-3



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 62321-3-2:2014
– 2 – 62321-3-2 © IEC:2013
CONTENTS
FOREWORD . 4
INTRODUCTION . 6
1 Scope . 7
2 Normative references . 7
3 Terms, definitions and abbreviations . 8
3.1 Terms and definitions . 8
3.2 Abbreviations . 9
4 Principle . 9
4.1 Overview . 9
4.2 Principle of test . 10
5 Reagents and materials . 10
6 Apparatus . 11
7 Sampling . 12
8 Procedure. 12
8.1 Combustion . 12
8.2 IC analysis . 13
8.3 Blank test . 13
8.4 Cleaning and recalibration . 13
8.5 Calibration . 13
8.6 Measurement of the sample . 14
8.7 Interference . 14
9 Calculation . 14
10 Precision . 14
11 Quality assurance and control . 15
11.1 General . 15
11.2 Limits of detection (LOD) and limits of quantification (LOQ) . 15
12 Test report . 16
Annex A (informative) Oxygen bomb combustion-ion chromatography . 17
Annex B (informative) Oxygen flask combustion-ion chromatography . 22
Annex C (informative) Example of a combustion device and IC system . 25
Annex D (informative) Results of international interlaboratory study #4A (IIS 4A) . 26
Annex E (informative) Additional results of TG 3-2 test . 27
Annex F (informative) Additional validation data. 29
Annex G (informative) Additional IC data . 30
Bibliography . 31

Figure A.1 – Example of the oxygen bomb combustion device . 21
Figure B.1 – Example of the oxygen flask combustion device. 24
Figure B.2 – Example of wrapping of sample . 24
Figure C.1 – Example of a combustion device connected to IC . 25
Figure C.2 – Example of ion chromatographic system . 25
Figure G.1 – Example of a chromatogram of the standard solution (4 mg/kg of each
standard) by IC . 30

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SIST EN 62321-3-2:2014
62321-3-2 © IEC:2013 – 3 –

Table 1 – Tested concentration ranges for bromine by C-IC in various materials . 7
Table 2 – Acceptance criteria of items for quality control . 15
Table 3 – Student’s t values used for calculation of method detection limit (*MDL=
t × s ) . 16
n–1
Table D.1 – Mean results and recovery rates for total bromine obtained in the IIS4A
study using C-IC . 26
Table D.2 – Statistical total bromine data for IIS 4A results using C-IC . 26
Table E.1 – Mean results and recovery rates for total bromine obtained in the TG 3-2
internal test study by using C-IC . 27
Table E.2 – Mean results and recovery rates for total bromine obtained in the TG 3-2
internal test study by using Oxygen bomb-IC . 28
Table F.1 – General conditions for the combustion furnace and the absorption solution . 29
Table F.2 – Additional information – Difference in sample sizes and measured bromine
values in solder paste with burning aid (WO powder) . 29
3
Table F.3 – Additional information – Difference in combustion temperatures and
powder) . 29
measured bromine values in solder paste with burning aid (WO
3
Table G.1 – Typical operating conditions for IC . 30
Table G.2 – Example of calibration solutions for IC . 30

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SIST EN 62321-3-2:2014
– 4 – 62321-3-2 © IEC:2013
INTERNATIONAL ELECTROTECHNICAL COMMISSION
____________

DETERMINATION OF CERTAIN SUBSTANCES
IN ELECTROTECHNICAL PRODUCTS –

Part 3-2: Screening – Total bromine in polymers and electronics
by Combustion – Ion Chromatography

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.
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 62321-3-2 introduces a new clause in the IEC 62321 series.
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 62321-3-2:2014
62321-3-2 © IEC:2013 – 5 –
The text of this standard is based on the following documents:
FDIS Report on voting
111/300/FDIS 111/310/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.

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SIST EN 62321-3-2:2014
– 6 – 62321-3-2 © IEC:2013
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) and polybrominated diphenyl
ethers (PBDE’s)) 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 62321-3-2:2014
62321-3-2 © IEC:2013 – 7 –
DETERMINATION OF CERTAIN SUBSTANCES
IN ELECTROTECHNICAL PRODUCTS –

Part 3-2: Screening – Total bromine in polymers and electronics
by Combustion – Ion Chromatography



1 Scope
Part 3-2 of IEC 62321 specifies the screening analysis of the total bromine (Br) in
homogeneous materials found in polymers and electronics by using the analytical technique
of combustion ion chromatography (C-IC).
This test method has been evaluated for ABS (acrylonitrile butadiene styrene), EMC (epoxy
molding compound), and PE (polyethylene) within the concentration ranges as specified in
Table 1.
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 bromine by C-IC in various materials
Substance/element Bromine
Medium/material tested
Parameter
Unit of
ABS EMC PE
measure
mg/kg
Concentration or
124 to 890 195 to 976 96
concentration range tested

This standard does not purport to address all of the safety concerns, if any, associated with
its use. It is the responsibility of the user of this standard to establish appropriate safety and
health practices and determine the applicability of regulatory limitations prior to use.
2 Normative references
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.
IEC 60754-1:2011, Test on gases evolved during combustion of materials from cables – Part
1: Determination of the halogen acid gas content
IEC 62321-1, Determination of certain substances in electrotechnical products – Part 1:
1
Introduction and overview
IEC 62321-2, Determination of certain substances in electrotechnical products – Part 2:
1
Disassembly, disjointment and mechanical sample preparation
___________
1
 To be published.

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SIST EN 62321-3-2:2014
– 8 – 62321-3-2 © IEC:2013
IEC 62321-3-1, Determination of certain substances in electrotechnical products – Part 3-1:
Screening –Lead, mercury, cadmium, total chromium and total bromine in electrotechnical
2
products using X-ray fluorescence spectrometry
ISO 3696, Water for analytical laboratory use – Specification and test methods
ISO 8466-1, Water quality – Calibration and evaluation of analytical methods and estimation
of performance characteristics – Part 1: Statistical evaluation of the linear calibration function
ISO/DIS 10304-1:2006, Water quality – Determination of dissolved anions by liquid
chromatography of ions – Part 1: Determination of bromide, chloride, fluoride, nitrate, nitrite,
phosphate and sulfate
3 Terms, definitions and abbreviations
3.1 Terms and definitions
For the purposes of this document, the terms and definitions given in IEC 62321-1 as well as
the following, apply.
3.1.1
accuracy
closeness of agreement between a test result and an accepted reference value
Note 1 to entry: The term accuracy, when applied to a set of test results, involves a combination of random
components and a common systematic error or bias component.
[ISO 5725-1:1995, definition 3.6] [1]
3.1.2
laboratory control sample
a known matrix spiked with compound(s) representative of the target analytes, used to
document laboratory performance
[Based on US EPA SW-846] [2]
3.1.3
repeatability limit
value less than or equal to which the absolute difference between two test results obtained
under repeatability conditions may be expected to be with a probability of 95 %
Note 1 to entry: The symbol used is r.
[ISO 5725-1:1994, definition 3.16]
3.1.4
reproducibility limit
value less than or equal to which the absolute difference between two test results obtained
under reproducibility conditions may be expected to be with a probability of 95 %
Note 1 to entry: The symbol used is R.
[ISO 5725-1:1994, definition 3.20 ]
___________
2
To be published.

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SIST EN 62321-3-2:2014
62321-3-2 © IEC:2013 – 9 –
3.1.5
test sample
sample prepared from the laboratory sample and from which test portions will be taken
[ISO 6206:1979, definition 3.2.13] [3]
3.1.6
test portion
the quantity of material drawn from the test sample (or from the laboratory sample if both are
the same) and on which the test or observation is actually carried out
[ISO 6206:1979, definition 3.2.14]
3.2 Abbreviations
ABS Acrylonitrile butadiene styrene
CCV Continuing calibration verification
CD Conductivity detector
C-IC Combustion – Ion chromatography
EMC Epoxy molding compound
IC Ion chromatography
IS Internal standard
IUPAC International Union of Pure and Applied Chemistry
KRISS Korea Research Institute of Standards and Science
LCS Laboratory control sample
LOD Limit of detection
LOQ Limit of quantification
MDL Method detection limit
PBBs Polybrominated biphenyls
PBDEs Polybrominated diphenyl ethers
PE Polyethylene
PP Polypropylene
XRF X-Ray fluorescence spectroscopy
US EPA United States Environmental Protection Agency
4 Principle
4.1 Overview
The concept of 'screening' has been developed to reduce the amount of testing. Executed as
a predecessor to any other test analysis, the main objective of screening is to quickly
determine whether the screened part or section of a product:
– contains a certain substance at a concentration significantly higher than its value or values
chosen as criterion, and therefore may be deemed unacceptable;
– contains a certain substance at a concentration significantly lower than its value or values
chosen as criterion, and therefore may be deemed acceptable;
contains a certain substance at a concentration so close to the value or values chosen as
criterion that when all possible errors of measurement and safety factors are considered, no
conclusive decision can be made about the acceptable absence or presence of a certain

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SIST EN 62321-3-2:2014
– 10 – 62321-3-2 © IEC:2013
substance and, therefore, a follow-up action may be required, including further analysis using
verification testing procedures.
This test method is designed specifically to screen for bromine (Br) in polymers and
electronics in electrotechnical products. C-IC provides information on the total quantity of
bromine present in the sample, but does not identify compounds or valence states of the
bromine. Therefore, special attention shall be paid when screening for bromine, where the
result will reflect only the total bromine present. The presence of brominated flame retardants
PBB or PBDE shall be confirmed by a verification test procedure. When applying this method
to electronics “as received”, which, by the nature of their design, are not uniform, care shall
be taken in interpreting the results.
4.2 Principle of test
A sample of known weight or volume is placed into a sample boat and introduced at a
controlled rate into a high-temperature combustion tube. There the sample is combusted in an
oxygen-rich pyrohydrolyti
...

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