EN 62321-2009 en Electrotechnical products - Determination of levels of six regulated substances (lead mercury cadmium hexavalent chromium polybrominated biphenyls polybrominated d.pdf

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1、raising standards worldwideNO COPYING WITHOUT BSI PERMISSION EXCEPT AS PERMITTED BY COPYRIGHT LAWBSI British StandardsWB9423_BSI_StandardColCov_noK_AW:BSI FRONT COVERS 5/9/08 12:55 Page 1Electrotechnical products Determination of levels of sixregulated substances (lead,mercury, cadmium, hexavalentch

2、romium, polybrominatedbiphenyls, polybrominateddiphenyl ethers)BS EN 62321:2009National forewordThis British Standard is the UK implementation of EN 62321:2009. It is identical to IEC 62321:2008.The UK participation in its preparation was entrusted to Technical CommitteeGEL/111, Electrotechnical env

3、ironment 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 of acontract. Users are responsible for its correct application. BSI 2009ISBN 978 0 580 55500 8ICS 13.020.40;

4、31.020Compliance with a British Standard cannot confer immunity fromlegal obligations.This British Standard was published under the authority of the StandardsPolicy and Strategy Committee on 31 May 2009Amendments issued since publicationAmd. No. Date Text affectedBRITISH STANDARDBS EN 62321:2009EURO

5、PEAN STANDARD EN 62321 NORME EUROPENNE EUROPISCHE NORM April 2009 CENELEC European Committee for Electrotechnical Standardization Comit Europen de Normalisation Electrotechnique Europisches Komitee fr Elektrotechnische Normung Central Secretariat: avenue Marnix 17, B - 1000 Brussels 2009 CENELEC - A

6、ll rights of exploitation in any form and by any means reserved worldwide for CENELEC members. Ref. No. EN 62321:2009 E ICS 13.020; 43.040.10 English version Electrotechnical products - Determination of levels of six regulated substances (lead, mercury, cadmium, hexavalent chromium, polybrominated b

7、iphenyls, polybrominated diphenyl ethers) (IEC 62321:2008) Produits lectrotechniques - Dtermination des niveaux de six substances rglementes (plomb, mercure, cadmium, chrome hexavalent, diphnyles polybroms, diphnylthers polybroms) (CEI 62321:2008) Produkte in der Elektrotechnik - Bestimmung von Best

8、andteilen der sechs Inhaltsstoffe (Blei, Quecksilber, Cadmium, sechswertiges Chrom, polybromiertes Biphenyl, polybromierter Diphenylether), die einer Beschrnkung unterworfen sind (IEC 62321:2008) This European Standard was approved by CENELEC on 2009-03-01. CENELEC members are bound to comply with t

9、he 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 Central Secretariat

10、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 Central Secretariat has the same status as the offi

11、cial versions. CENELEC members are the national electrotechnical committees of Austria, Belgium, Bulgaria, Cyprus, the Czech Republic, Denmark, Estonia, Finland, France, Germany, Greece, Hungary, Iceland, Ireland, Italy, Latvia, Lithuania, Luxembourg, Malta, the Netherlands, Norway, Poland, Portugal

12、, Romania, Slovakia, Slovenia, Spain, Sweden, Switzerland and the United Kingdom. BS EN 62321:2009EN 62321:2009 2 Foreword The text of document 111/116/FDIS, future edition 1 of IEC 62321, prepared by IEC TC 111, Environmental standardization for electrical and electronic products and systems, was s

13、ubmitted to the IEC-CENELEC parallel vote and was approved by CENELEC as EN 62321 on 2009-03-01. The following dates were fixed: latest date by which the EN has to be implemented at national level by publication of an identical national standard or by endorsement (dop) 2009-12-01 latest date by whic

14、h the national standards conflicting with the EN have to be withdrawn (dow) 2012-03-01 Annex ZA has been added by CENELEC. _ Endorsement notice The text of the International Standard IEC 62321:2008 was approved by CENELEC as a European Standard without any modification. In the official version, for

15、Bibliography, the following notes have to be added for the standards indicated: IEC 60730-1 NOTE Harmonized as EN 60730-1:2000 (modified). ISO 3613 NOTE Harmonized as EN ISO 3613:2001 (not modified). ISO 17294-1 NOTE Harmonized as EN ISO 17294-1:2006 (not modified). _ BS EN 62321:2009 3 EN 62321:200

16、9 Annex ZA (normative) Normative references to international publications with their corresponding European publications The following referenced documents are indispensable for the application of this document. For dated references, only the edition cited applies. For undated references, the latest

17、 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 ISO/IEC Guide 98 1995 Guide to the expression of uncertainty in

18、measurement (GUM) - - ISO/IEC 17025 - 1)General requirements for the competence of testing and calibration laboratories EN ISO/IEC 17025 2005 2)ISO 3696 - 1)Water for analytical laboratory use - Specification and test methods EN ISO 3696 1995 2)ISO 5961 - 1)Water quality - Determination of cadmium b

19、y atomic absorption spectrometry EN ISO 5961 1995 2)1)Undated reference. 2)Valid edition at date of issue. BS EN 62321:2009 4 62321 IEC:2008 CONTENTS INTRODUCTION.8 1 Scope.9 2 Normative references .9 3 Terms, definitions and abbreviations 10 3.1 Terms and definitions 10 3.2 Abbreviations 11 4 Test

20、methods Overview .13 4.1 Field of application 13 4.2 Sample13 4.3 Test methods Flow chart 14 4.4 Adjustment to the matrix15 4.5 Limits of detection (LOD) and limits of quantification (LOQ).15 4.6 Test report 16 4.7 Alternative test methods16 5 Mechanical sample preparation 17 5.1 Overview .17 5.1.1

21、Field of application 17 5.1.2 Quality assurance17 5.2 Apparatus, equipment and materials .17 5.3 Procedure .18 5.3.1 Manual cutting.18 5.3.2 Coarse grinding/milling 18 5.3.3 Homogenizing .18 5.3.4 Fine grinding/milling 18 5.3.5 Very fine grinding of polymers and organic materials .19 6 Screening by

22、X-ray fluorescence spectrometry (XRF).19 6.1 Overview .19 6.1.1 Principle 21 6.1.2 Warnings .22 6.2 Apparatus, equipment and materials .22 6.2.1 XRF spectrometer .22 6.2.2 Materials and tools 22 6.3 Reagents.22 6.4 Sampling .22 6.4.1 Non-destructive approach22 6.4.2 Destructive approach.23 6.5 Proce

23、dure .23 6.5.1 General .23 6.5.2 Preparation of the spectrometer 23 6.5.3 Test portion .24 6.5.4 Verification of spectrometer performance.24 6.5.5 Tests .25 6.5.6 Calibration.25 6.6 Calculations 26 6.7 Evaluation of the method.27 BS EN 62321:200962321 IEC:2008 5 6.7.1 Lead27 6.7.2 Mercury .27 6.7.3

24、Cadmium .27 6.7.4 Chromium27 6.7.5 Bromine.28 6.8 Quality control.28 6.8.1 Accuracy of calibration 28 6.8.2 Control samples 28 6.9 Special cases28 6.9.1 Presentation of a sample for measurement28 6.9.2 Uniformity of the sample29 7 Determination of mercury in polymers, metals and electronics by CV-AA

25、S, CV-AFS, ICP-OES and ICP-MS 30 7.1 Overview .30 7.2 Apparatus, equipment and materials .31 7.3 Reagents.32 7.4 Sample preparation .33 7.4.1 Test portion .33 7.4.2 Wet digestion (digestion of electronics) .33 7.4.3 Microwave digestion 34 7.4.4 Preparation of laboratory reagent blank.34 7.5 Test pro

26、cedure 34 7.5.1 Preparation of calibrant solutions 34 7.5.2 Development of the calibration curve.35 7.5.3 Measurement of the sample.36 7.5.4 Calculation 36 7.6 Evaluation of the method.36 8 Determination of lead and cadmium in polymers by ICP-OES, ICP-MS and AAS 37 8.1 Overview .37 8.2 Apparatus, eq

27、uipment and materials .38 8.3 Reagents.39 8.4 Sample preparation .40 8.4.1 Test portion .40 8.4.2 Preparation of test solution40 8.4.3 Preparation of laboratory reagent blank.42 8.5 Test procedure 42 8.5.1 Preparation of calibration solution .42 8.5.2 Development of the calibration curve.43 8.5.3 Me

28、asurement of the sample.43 8.5.4 Calculation 44 8.6 Evaluation of the method.44 9 Determination of lead and cadmium in metals by ICP-OES, ICP-MS and AAS 44 9.1 Overview .44 9.2 Apparatus, equipment and materials .45 9.3 Reagents.45 9.4 Sample preparation .46 9.4.1 Test portion .46 9.4.2 Preparation

29、of the test sample solution47 9.5 Preparation of laboratory reagent blank.48 BS EN 62321:2009 6 62321 IEC:2008 9.6 Test procedure 48 9.6.1 Preparation of the calibrant .48 9.6.2 Measurement of the calibrant 49 9.6.3 Measurement of the sample.49 9.6.4 Calculation 50 9.7 Evaluation of the method.50 10

30、 Determination of lead and cadmium in electronics by ICP-OES, ICP-MS and AAS50 10.1 Overview .50 10.2 Apparatus, equipment and materials .51 10.3 Reagents.52 10.4 Sample preparation .53 10.4.1 Test portion .53 10.4.2 Digestion with aqua regia 53 10.4.3 Microwave digestion 54 10.5 Test procedure 55 1

31、0.5.1 Preparation of a calibrant solution .55 10.5.2 Standard preparation.55 10.5.3 Calibration.56 10.5.4 Development of the calibration curve.56 10.5.5 Measurement of the sample.57 10.5.6 Calculation 57 10.6 Evaluation of the method.58 Annex A (informative) Determination of PBB and PBDE in polymers

32、 by GC-MS .59 Annex B (informative) Test for the presence of hexavalent chromium (Cr(VI) in colourless and coloured corrosion-protected coatings on metals.75 Annex C (Informative) Determination of hexavalent chromium (Cr(VI) in polymers and electronics by the colorimetric method 80 Annex D (informat

33、ive) Practical application of screening by X-ray fluorescence spectrometry (XRF).88 Annex E (informative) Practical application of determination of mercury in polymers, metals and electronics by CV-AAS, CV-AFS, ICP-OES and ICP-MS .95 Annex F (informative) Practical application of determination of le

34、ad and cadmium in polymers by ICP-OES, ICP-MS and AAS 97 Annex G (informative) Practical application of determination of lead and cadmium in metals by ICP-OES, ICP-MS and AAS 99 Annex H (informative) Practical application of determination of lead and cadmium in electronics by ICP-OES, ICP-MS and AAS

35、102 Bibliography106 Figure 1 Flow chart of the test methods .14 Figure A.1 Total ion chromatogram of PBDE mixture, BDE-1 to BDE-206 (5 g/ml), BDE-209 (50 g/ml) 73 Figure A.2 Total ion chromatogram of PBB mixture (3,5 g/ml) 74 Figure A.3 Total ion chromatogram of PBB and PBDE mixtures (BDE-1 to BDE-2

36、06 5 g/ml, BDE-209 5,0 g/ml, PBBs 3,5 g/ml)74 Figure E.1 Heating digester equipped with reaction vessel, reflux cooler and absorption vessel95 Figure G.1 Background correction100 Figure H.1 Background correction104 BS EN 62321:200962321 IEC:2008 7 Table 1 Overview of the content of the verification

37、procedure 15 Table 2 Tested concentration ranges for lead in materials 20 Table 3 Tested concentration ranges for mercury in materials20 Table 4 Tested concentration ranges for cadmium in materials 20 Table 5 Tested concentration ranges for total chromium in materials .20 Table 6 Tested concentratio

38、n ranges for bromine in materials20 Table 7 Recommended X-ray lines for individual analytes24 Table 8 Mean results and recovery rates of mercury obtained in the IIS2 study37 Table A.1 Matrix spiking solution .61 Table A.2 Calibration solutions of PBBs and PBDEs 62 Table A.3 Reference masses for the

39、quantification of PBBs .67 Table A.4 Reference masses for the quantification of PBDEs.67 Table A.5 Example calculation .68 Table A.6 Example list of commercially available calibration congeners considered suitable for this analysis .71 Table A.7 PBB and PBDE congeners in the mixture .72 Table C.1 Me

40、thod detection limit = t sn186 Table D.1 Effect of matrix composition on limits of detection of some controlled elements.89 Table D.2 Screening limits in mg/kg for regulated elements in various matrices .90 Table D.3 Mean results and recovery rates for lead obtained in the IIS2 study.91 Table D.4 Me

41、an results and recovery rates for mercury obtained in the IIS2 study.92 Table D.5 Mean results and recovery rates for cadmium obtained in the IIS2 study .92 Table D.6 Mean results and recovery rates for total chromium obtained in the IIS2 study 93 Table D.7 Mean results and recovery rates for total

42、bromine obtained in the IIS2 study 94 Table E.1 Program for microwave digestion of samples (power output for five vessels) 96 Table F.1 Spectral interferences for the wavelengths of cadmium and lead97 Table F.2 Examples of mass/charge (m/z) ratios98 Table F.3 Examples of wavelengths for AAS98 Table

43、G.1 Spectral interferences for the wavelengths of cadmium and lead .99 Table G.2 Examples of mass/charge (m/z) ratios .101 Table G.3 Examples for wavelengths for AAS 101 Table H.1 Program for microwave digestion of samplesa.102 Table H.2 Spectral interferences for the wavelengths of cadmium and lead

44、 .103 Table H.3 Examples of mass/charge (m/z) ratios .105 Table H.4 Examples of wavelengths for AAS105 BS EN 62321:2009 8 62321 IEC:2008 INTRODUCTION The widespread use of electrotechnical products has drawn increased attention to their impact on the environment. In many countries all over the world

45、 this has resulted in the adaptation of regulations affecting wastes, substances and energy use of electrotechnical products. The use of certain substances such as lead (Pb), mercury (Hg), cadmium (Cd), hexavalent chromium (Cr(VI) contained in inorganic and organic compounds, and two types of bromin

46、ated flame retardants, polybrominated biphenyls (PBB) and polybrominated diphenyl ethers (PBDE) in electrotechnical products, is regulated in current and proposed regional legislation. The purpose of IEC 62321 is therefore to provide test methods that will allow the electrotechnical industry to dete

47、rmine the levels of regulated substances Pb, Hg, Cd, Cr(VI) and their compounds, as well as PBB and PBDE in electrotechnical products on a consistent global basis. BS EN 62321:200962321 IEC:2008 9 ELECTROTECHNICAL PRODUCTS DETERMINATION OF LEVELS OF SIX REGULATED SUBSTANCES (LEAD, MERCURY, CADMIUM,

48、HEXAVALENT CHROMIUM, POLYBROMINATED BIPHENYLS, POLYBROMINATED DIPHENYL ETHERS) 1 Scope IEC 62321, which is an International Standard, specifies the determination of the levels of lead (Pb), mercury (Hg), cadmium (Cd), hexavalent chromium (Cr(VI) contained in inorganic and organic compounds, and two

49、types of brominated flame retardants, polybrominated biphenyls (PBB) and polybrominated diphenyl ethers (PBDE) contained in electrotechnical products. This standard refers to the sample as the object to be processed and measured. The nature of the sample and the manner in which it is acquired is defined by the entity carrying out the tests and not by this standard. NOTE 1 Further guidance on