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 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).

Verfahren zur Bestimmung von bestimmten Substanzen in Produkten der Elektrotechnik - Teil 3-2: Screening - Gesamtbrom in Polymeren und Elektronik durch Verbrennungsaufschluss - Ionen-Chromatographie

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

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
24-Apr-2014
Current Stage
6060 - Document made available
Due Date
25-Apr-2014
Completion Date
25-Apr-2014

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SLOVENSKI STANDARD
SIST EN 62321-3-2:2014
01-junij-2014
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SIST EN 62321:2009
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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.

---------------------- Page: 1 ----------------------
SIST EN 62321-3-2:2014
---------------------- Page: 2 ----------------------
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
---------------------- Page: 3 ----------------------
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).
---------------------- Page: 4 ----------------------
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

Table F.3 – Additional information – Difference in combustion temperatures and
powder) ............................. 29
measured bromine values in solder paste with burning aid (WO

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.
---------------------- Page: 10 ----------------------
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:

Introduction and overview

IEC 62321-2, Determination of certain substances in electrotechnical products – Part 2:

Disassembly, disjointment and mechanical sample preparation
___________
To be published.
---------------------- Page: 13 ----------------------
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

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 ]
___________
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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