1、BSI Standards PublicationDetermination of certain substances in electrotechnical productsPart 3-2: Screening Total bromine in polymers and electronics by Combustion Ion ChromatographyBS EN 62321-3-2:2014National forewordT h i s B r i t i s h S t a n d a r d i s t h e U K i m p l e m e n t a t i o n
2、o f E N 6 2 3 2 1 - 3 - 2 : 2 0 14. It is identical to IEC 62321-3-2:2013. T o g e t h e r w i t h B S E N 6 2 3 2 1 - 1 : 2 0 1 3 , B S E N 6 2 3 2 1 - 2 : 2 0 14, B S E N 6 2 3 2 1 - 3 - 1 : 2 0 14, B S E N 6 2 3 2 1 - 4 : 2 0 14, B S E N 6 2 3 2 1 - 5 : 2 0 14, B S E N 6 2 3 2 1 - 6 , B S E N 6 2
3、 3 2 1 - 7 - 1 , B S E N 6 2 3 2 1 - 7 - 2 a n d B S E N 6 2 3 2 1 - 8 i t s u p e r s e d e s B S E N 6 2 3 2 1 : 2 0 0 9 , w h i c h w i l l b e w i t h d r a w n u p o n p u b l i c a t i o n o f a l l p a r t s o f t h e B S E N 6 2 3 2 1 s e r i e s .The UK participation in its preparation was
4、entrusted to TechnicalCommittee GEL/111, Electrotechnical environment committee.A list of organizations represented on this committee can be obtained onrequest to its secretary.This publication does not purport to include all the necessary provisions ofa contract. Users are responsible for its corre
5、ct application. The British Standards Institution 2014.Published by BSI Standards Limited 2014ISBN 978 0 580 71819 9ICS 13.020; 43.040.10Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of theStandards Policy and
6、Strategy Committee on 31 May 2014.Amendments/corrigenda issued since publicationDate Text affectedBRITISH STANDARDBS EN 62321-3-2:2014EUROPEAN STANDARD EN 62321-3-2 NORME EUROPENNE EUROPISCHE NORM April 2014 CENELEC European Committee for Electrotechnical Standardization Comit Europen de Normalisati
7、on Electrotechnique Europisches Komitee fr 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 ICS 13.020; 43.040.10 Su
8、persedes 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) Dtermination de certaines substances dans les produits lectrot
9、echniques - Partie 3-2: Mthodes dessai - Brome total dans les polymres et les produits lectriques par Combustion - Chromatographie dIonisation (CEI 62321-3-2:2013) Verfahren zur Bestimmung von bestimmten Substanzen in Produkten der Elektrotechnik - Teil 3-2: Screening - Gesamtbrom in Polymeren und E
10、lektronik durch Verbrennungsaufschluss - 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
11、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, G
12、erman). 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, Belg
13、ium, 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
14、, Switzerland, Turkey and the United Kingdom. BS EN 62321-3-2:2014EN 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-
15、CENELEC parallel vote and approved by CENELEC as EN 62321-3-2:2014. The following dates are fixed: latest date by which the document has to be implemented at national level by publication of an identical national standard or by endorsement (dop) 2014-10-25 latest date by which the national standards
16、 conflicting with the document have to be withdrawn (dow) 2016-11-15 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
17、 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 identif
18、ying 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 6
19、0754-2 NOTE Harmonised as EN 60754-2 (not modified). ISO 5667-1 NOTE Harmonised as EN ISO 5667-1 (not modified). BS 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,
20、 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 publ
21、ication 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 materials from cables - Part 1: Determination of the halogen acid gas content EN 60754-1 2013 IEC 62321-1 -
22、 Determination of certain substances in electrotechnical products - Part 1: Introduction and overview EN 62321-1 - IEC 62321-2 - Determination of certain substances in electrotechnical products - Part 2: Disassembly, disjunction and mechanical sample preparation EN 62321-2 - IEC 62321-3-1 - Determin
23、ation of certain substances in electrotechnical products - Part 3-1: Screening electrotechnical products for lead, mercury, cadmium, total chromium and total bromine using X-ray Fluorescence Spectrometry EN 62321-3-1 - ISO 3696 - Water for analytical laboratory use - Specification and test methods E
24、N ISO 3696 - 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 anions by liquid chromatography
25、 of ions - Part 1: Determination of bromide, chloride, fluoride, nitrate, nitrite, phosphate and sulphate EN ISO 10304-1 - BS EN 62321-3-2:2014 2 62321-3-2 IEC:2013 CONTENTS INTRODUCTION . 6 1 Scope . 7 2 Normative references . 7 3 Terms, definitions and abbreviations 8 3.1 Terms and definitions 8 3
26、.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
27、 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 f
28、lask 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
29、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 Fig
30、ure 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 BS EN 62321-3-2:201462321-3-2 IEC:2013 3 Table 1 Tested concentration ranges for bromine by C-IC in various materials . 7 Table 2 Acceptance criteria
31、 of items for quality control 15 Table 3 Students t values used for calculation of method detection limit (*MDL= t sn1) . 16 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
32、. 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 combus
33、tion 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 (WO3powder) 29 Table F.3 Additional information Difference in combustion temperatures and measured bromine values in solder paste with
34、burning aid (WO3powder) . 29 Table G.1 Typical operating conditions for IC . 30 Table G.2 Example of calibration solutions for IC . 30 BS 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 environme
35、nt. 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 (PBDEs) in electrotechnical products, i
36、s 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 basi
37、s. 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 an
38、d to ensure compliance with any national regulatory conditions BS EN 62321-3-2:201462321-3-2 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 specif
39、ies 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
40、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
41、Bromine Parameter Unit of measure mg/kg Medium/material tested ABS EMC PE Concentration or concentration range tested 124 to 890 195 to 976 96 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
42、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 reference
43、s, 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, Determina
44、tion of certain substances in electrotechnical products Part 1: Introduction and overview1IEC 62321-2, Determination of certain substances in electrotechnical products Part 2: Disassembly, disjointment and mechanical sample preparation1_ 1To be published. BS EN 62321-3-2:2014 8 62321-3-2 IEC:2013 IE
45、C 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 spectrometry2ISO 3696, Water for analytical laboratory use Specification and test methods I
46、SO 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: Det
47、ermination of bromide, chloride, fluoride, nitrate, nitrite, phosphate and sulfate 3 Terms, definitions and abbreviations Terms and definitions 3.1For the purposes of this document, the terms and definitions given in IEC 62321-1 as well as the following, apply. 3.1.1accuracy closeness of agreement b
48、etween 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 3.1.2laboratory control sample a known matrix
49、 spiked with compound(s) representative of the target analytes, used to document laboratory performance Based on US EPA SW-846 2 3.1.3repeatability 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 3.1.4reproducibility limit value less than or equal t
