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1 유해물질프로세스경영시스템 (HSPM) 세미나 IEC 국제표준소개 : 전기전자제품유해물질시험분석표준 한국생산기술연구원최은경수석연구원 ekchoe@kitech.re.kr 2009 년 7 월 22 일 ( 수 ), 대한상공회의소

2 목차 1. EU 의제품함유유해물질환경규제의흐름 2. 전기전자제품함유유해물질 3. IEC 유해물질시험분석표준의구조및내용 4. IEC 개정현황 5. 결언

3 제품함유유해물질환경규제의국제동향 제품함유유해물질환경규제시행년도 섬유제품에코라벨 염료, PCP 등특정유해물질사용제한법규 ( 독일, 네덜란드등 EU RoHS China RoHS China RoHS 3C 강제인증 노르웨이 PoHS EU Directive 2006/122/EC, PFOS 규제 EU Directive 2003/53/EC, NPEO 규제 EU REACH REACH SVHC 공표

4 전기전자제품의국제환경규제 EU, RoHS 확대추진 규제물질 4 개추가 2002 년 RoHS 지침제정 : RoHS Directive 2002/95/EC Restrictions of Hazardous Substances in Electrical & Electronic Equipments 2006년 7월 EU의전기전자제품유해물질제한지침 (RoHS) 시행 : Timeline for New RoHS Directive 규제되고화학물질 : 납 (Pb), 카드뮴 (Cd), 수은 (Hg), 6가크롬 (Cr6+), 공표예정브롬계난연제 2종 (PBBs, PBDEs) -2014년시행예정 RoHS 확대 강화전망 : RoHS Novel Draft COM(2008) 809/4, 발표 년부터의료기기를 RoHS 규제에포함 - 규제화학물질에대한산업적모니터링과제어기기설치를 2015 년부터의무화 - 생체내진단장치와체내삽입의료기기에대해각 2016 년, 2020 년까지 RoHS 내에서규제 - 규제대상화학물질 : 4 개추가방침 브롬계난연제 1 개 HBCDD(hexabromocyclododecane) 프탈레이트 3 개 DEHP (Di-(2-ethylhexyl) phthalate), BBP (Butyl benzyl phthalate), DBP [Di-n-butyl phthalate)

5 EU RoHS 46 종후보리스트 ID Substance name ID Substance name 1 Antimony trioxide 24 Polychlorinated Naphthalenes 2 Antimony compounds 25 Selenium 3 Arsenic/arsenic compounds 26 Short-chained chlorinated paraffins (SCCP) (Alkanes, C10-13, chloro) 4 Beryllium metal 27 Synthetic vitreous fibres -glass fibres- mineral wool-refractory ceramic fibre (RCFs) 5 Beryllium oxide BeO 28 Tributyl Tin (TBT) compounds, Triphenyl Tin (TPT) compounds 6 Tetrabromo bisphenol A and related compounds 29 Tributyl Tin Oxide (TBTO) 7 Bisphenol A (4,4'-Isopropylidendiphenol) 30 dinickel trioxide 8 Diethylhexylphthalate(DEHP) 31 diarsenic trioxide; arsenic trioxide 9 Butylbenzylphthalate (BBP) 32 4,4'-methylenedi-o-toluidine 10 Dibutylphthalate (DBP) 33 Petrolatum; Petrolatum 11 Dioctylphthalate (DOP) 34 nickel dihydroxide 12 Dimethylformamide (DMF) 35 tributyl phosphate 13 Formaldehyde 36 divanadium pentaoxide; vanadium pentoxide 14 Gallium arsenide 37 nickel sulphate Hexabromocyclododecane (HBCDD) and further brominated flame retardants Liquid crystals, e.g. MBBA(4-methoxybenzylidene-4- butylaniline); 5CB(4-pentyl-4-cyanobiphenyl) Medium-chained chlorinated paraffins (MCCP) (Alkanes, C14-17, chloro) 38 cobalt oxide 39 cobalt 40 2-ethylhexyl acrylate 18 Nickel 41 Naphthenic acids, copper salts; copper naphthenate 19 Nonylphenol, Nonylphenolpolyglycolethers (Nonylphenolethoxylates) 42 phenyl bis(2,4,6-trimethylbenzoyl)-phosphine oxide 20 Perfluorooctane sulfonates 43 thallium 21 PVC 44 bromobenzylbromotoluene, mixture of isomers 22 PCBs, Polychlorinated Biphenyls 45 2,2'-(ethylenedioxy)diethyl diacrylate; triethylene glycol diacrylate 23 PCT, Polychlorinated Terphenyls 46 Rosin; colophony

6 EU Directive 로부터의제품군별유해물질 -1 제품군규제유해물질항목관련근거 전기전자제품 생활용품 자동차 Cd, Pb, Hg, Cr(VI), PBBs, PBDEs, PCBs, PCTs, PCNs, ODS, 석면, 포름알데히드, Chlorinated paraffins (C10~13), Azo compounds, Ni, As, Organic tin compounds(tbt, TPhT), Phthalates, PVC, Be, Other chlorinated compounds, Other brominated flame retardants, TBBP-A Cd, Pb, Hg, Cr(VI), VOC(Sick-car), 배기가스 (SOx, COx, CO, HC, NOx, PM) EU Directive 2002/95/EC(RoHS) 노르웨이 PoHS EU Directive 2000/53/EC (ELV,end-of-life vehicles) EU Directive 70/220/EEC(emissions from motor vehicles) EU Directive 2005/84/EC 완구및유아용품 BEHP, DBP, BBP, DINP, DIDP, DNOP EU Directive 98/485/EC (phthalates in toys and childcare articles) 섬유제품 Formaldehyde, Pesticides, PCP/TeCP, heavy metals (10 종 ), cleavable arylamines (22 종 ), carcinogenic (6 종 ), allergy-causing (9 종 ), chlorinated organic carriers 10 종, emission of volatiles, flame retardant finishes, APEO, ETAD EU Decision 2002/371/EC EU Decision 1999/178/EC (eco-label to textile products)

7 EU Directive 로부터의제품군별유해물질 -1 제품군규제유해물질항목관련근거 전기전자제품 생활용품 자동차 Cd, Pb, Hg, Cr(VI), PBBs, PBDEs, PCBs, PCTs, PCNs, ODS, 석면, 포름알데히드, Chlorinated paraffins (C10~13), Azo compounds, Ni, As, Organic tin compounds(tbt, TPhT), Phthalates, PVC, Be, Other chlorinated compounds, Other brominated flame retardants, TBBP-A Cd, Pb, Hg, Cr(VI), VOC(Sick-car), 배기가스 (SOx, COx, CO, HC, NOx, PM) EU Directive 2002/95/EC(RoHS) 노르웨이 PoHS EU Directive 2000/53/EC (ELV,end-of-life vehicles) EU Directive 70/220/EEC(emissions from motor vehicles) EU Directive 2005/84/EC 완구및유아용품 BEHP, DBP, BBP, DINP, DIDP, DNOP EU Directive 98/485/EC (phthalates in toys and childcare articles) 섬유제품 Formaldehyde, Pesticides, PCP/TeCP, heavy metals (10 종 ), cleavable arylamines (22 종 ), carcinogenic (6 종 ), allergy-causing (9 종 ), chlorinated organic carriers 10 종, emission of volatiles, flame retardant finishes, APEO, ETAD EU Decision 2002/371/EC EU Decision 1999/178/EC (eco-label to textile products)

8 IEC TC 111 WG3 의결과물로발간된 IEC 표준

9 IEC 국제표준의구조 (1)

10 IEC 국제표준의구조 (2)

11 CONTENTS FOREWORD INTRODUCTION 1 Scope 2 Normative references 3 Terms, definitions and abbreviations 4 Test methods: overview 5 Mechanical sample preparation 6 Screening by X-ray fluorescence spectrometry (XRF) 7 Determination of mercury in polymers, metals and electronics by CV-AAS, CVAFS, ICP-OES and ICP-MS 8 Determination of lead and cadmium in polymers by ICP-OES, ICP-MS and AAS 9 Determination of lead and cadmium in metals by ICP-OES, ICP-MS and AAS 10 Determination of lead and cadmium in electronics by ICP-OES, ICP-MS and AAS Annex A (Informative) Determination of PBB and PBDE in Polymers by GC-MS Annex B (Informative) Test for the presence of hexavalent chromium (Cr(VI)) in colourless and coloured corrosion-protection coatings on metals Annex C (Informative) Determination of hexavalent chromium (Cr(VI)) in polymers and electronics by the colorimetric method Annex D (Informative) Practical application of screening by X-ray fluorescence spectrometry (XRF) Annex E (Informative) Practical application of determination of mercury in polymers, metals and electronics by CV-AAS, AFS, ICP-OES and ICP-MS Annex F (Informative) Practical application of determination of lead and cadmium in polymers by ICP-OES, ICP-MS and AAS Annex G (Informative) Practical application of determination of lead and cadmium in metals by ICP-OES, ICP-MS and AAS Annex H (Informative) Practical application of determination of lead and cadmium in electronics by ICP-OES, ICP-MS and AAS Bibliography

12 IEC 62321는본장의시험방법 (Hg, Pb, Cd) 과 Annex에시험방법 (PBBs/PBDEs, Cr 6+ ) 으로분리됨매질은크게 3종류 (Polymers, Metals, Electronics) 로구분됨. 기존 EPA 방법등과유사함. IEC summary EPA method and others Hg 7. Determination of mercury in polymers, metals and electronics by CV-AAS, CV-AFS, ICP-OES and ICP-MS Microwave digestion Wet digestion EPA 3051, EPA Determination of lead and cadmium in polymers by ICP-OES, ICP-MS and AAS Drying ashing, Acid digestion, Microwave digestion EPA 3052, EPA 3050B, EPA 6010C Pb, Cd 9. Determination of lead and cadmium in metals by ICP-OES, ICP-MS and AAS Acid digestion EPA 3050B, EPA 6010C 10. Determination of lead and cadmium in electronics by ICP-OES, ICP-MS and AAS Microwave digestion Digestion with aqua regia EPA 3052, EPA 6010C PBBs/ PBDEs Annex A (Informative) Determination of PBBs and PBDEs in polymers by GC-MS Soxhlet extraction EPA 3540C, EPA 8270D Cr 6+ Annex B (Informative) Test for the presence of hexavalent chromium (Cr 6+ ) in colourless and coloured corrosion-protection coatings on metals Annex C (Informative) Determination of hexavalent chromium (Cr 6+ ) in polymers and electronics by the colorimetric method Spot test, Boiling water extraction Alkaline extraction ISO 3613 EPA 3060A, EPA 7196A

13 IEC 시험방법의절차도

14 IEC 세부내용들여다보기 7. Determination of mercury in polymers, metals and electronics by CV-AAS, CV-AFS, ICP-OES and ICP-MS 7.1 Scope, application and summary of method 지경부인력양성사업수행중 IEC 국제표준에의한 RoHS 6 대유해물질분석방법교육기관예 :

15 IEC 개정본 (2 nd Ed) 을위한 IEC/TC 111 WG3 의작업내용 Revision plan of IEC (2009 to 2012) 2008 년 10 월 16 일 ~17 일 IEC/TC 111 제주총회결과 IS Revision Main items Leader Major job 1 ~ 4 IEC Scope, normative references, abbreviation, Test methods Overview Scott, Joachim Editorial work PAS IEC Sample Disjointment Maarten Take comments into account received with NP, determine if -2 and -3 can be combined/harmonized, determine harmonization with -5 on CCFL preparation 5 IEC Mechanical sample preparation (TBD) Maarten See above (-2) 6 IEC Screening (e.g. XRF, total Br, total Cr) Stan Editorial work, discuss inclusion of total Br, total Cr (includes new IIS) 7 IEC Mercury Miyuki Harmonization with SC34 (Philips), new IIS, determine harmonization with -3 on CCFL preparation 8 ~10 IEC Lead and Cadmium Klaus, Joachim Editorial work, new methods to be considered (e.g. AFS) (new IIS), determine if total Cr should be in -6 or -4 Annex A IEC PBBs and PBDEs Scott Editorial work, new IIS (build on Thomas L. experience), determine if total Br (C-IC), HPLC (Mira, Michael), IAMS Annex B, C IEC Hexavalent chromium Sophia Next RoHS? : HBCDD, Phthalate (DEHP, BBP, DBP) Metallic coating: Work with DIN to determine harmonization (liaison), new IIS (with sponsored samples) Polymer: understand matrix interference, new IIS, determine if total Cr should be in -8, -6 or -4

16 IEC 개정본 (2 nd Ed) 반영에제안된분석방법 2009 년 4 월 15 일 ~16 일 IEC/TC 차 WG 3 에서각국제안 1. 한국 (LG DISPLAY] : C-IC 방법 (Total Bromine) 2. 일본 (Toshiba] : DMA 방법 (Mercury) 3. 중국 (CESI) : AFS 방법 [Pb, Cd, Total Cr & Cr(VI), PAHs 4. 독일 [Sony] : IAMS 방법 (BFRs, Phthalate] 5. 미국 [UL] : ICP. ICP-MS, AAS 방법 [Total Cr in plastics] 6. 기타

Mercury Analysis in IEC62321 Steps Substances Polymer Materials Metal Materials Electronics (PWBs/Components) Mechanical sample preparation (Chapter 5) Direct measurement Grinding Direct measurement

17 Mercury Analysis in IEC62321 Steps Substances Polymer Materials Metal Materials Electronics (PWBs/Components) Mechanical sample preparation (Chapter 5) Direct measurement Grinding Direct measurement Grinding Grinding Chemical sample preparation Microwave digestion Acid digestion with reflux cooler Thermal Decomposition (Amalgamation) Acid digestion with reflux cooler Thermal Decomposition (Amalgamation) Microwave digestion Acid digestion with reflux cooler Thermal Decomposition (Amalgamation) Analytical technique definition (incl. typical margins of errors) PBB/PBDE GC/MS (Informative) NA GC/MS (Informative) Cr 6+ Alkaline Digestion/ Colorimetric Method (Informative) Spot-test procedure/ boiling-water-extraction procedure (Informative) Alkaline Digestion/ Colorimetric Method (Informative) Hg ICP-OES, ICP-MS, CV AAS, AFS Pb/Cd ICP-OES, ICP-MS, AAS ICP-OES, ICP-MS, AAS ICP-OES, ICP-MS, AAS

18 C-IC 를이용한 Total Bromine 측정발표 Comparison of various total bromine methods Analytical methods Pretreatment Advantages vs. Disadvantages References XRF No need Non-destructive test Matrix effect or spectral interference Unsuitable for low levels of bromine IEC (screening) Oxygen flask & IC Oxygen bomb & IC Combustion-IC (C-IC) Combustion Temp. : max 500 Combustion Temp. : max 600 Batch type process Combustion Temp. : max 1100 Fully automated analysis system (from sample loading to analysis) Traditional test Lots of standards Incomplete combustion (Composite material, Solder paste..) Limitation of sample sizes and matrices Traditional test Incomplete combustion (Composite material, Solder paste..) Limitation of sample sizes and matrices Complete sample decomposition Not many published standard 3/9 JPCA-ES01:2003 IEC :2006 BS EN 14582:2007(annex) BS EN 14582:2007 ASTM D 3761 ASTM D 7359:2008 (C-IC) ERM adoption C-IC method in Dec : Analytical method used for certification Performance, of total Application bromine (EC590, EC591)

Schematic diagram of the C-IC method Advantages of Combustion-Ion Chromatography (C-IC) No chemical pre-treatment & high sensitivity & accuracy Fully automatic analysis system (from sample loading to

19 Schematic diagram of the C-IC method Advantages of Combustion-Ion Chromatography (C-IC) No chemical pre-treatment & high sensitivity & accuracy Fully automatic analysis system (from sample loading to analysis) Principle Sample in the Combustion Tube in the Absorbent Ion Chromatography Organic Halogen (C-Br) HBr, Br 2 Br - Process flow IC Adsorption unit Combustion unit Sample loading 1 2 Absorbent is set in the absorption tube Sample is burned (combustion) Absorbent absorb the combusted gas Inject the absorbent to the IC 3 5 Cleaning the absorption tube

20 IEC 개정본 (2 nd Ed) 발간일정

21 국제환경규제대응세가지전략 대응 1 : 이미시행된환경규제에적시저비용대응 대응 2 : 환경규제관련진행중인상황을한국에유리하게전개 대응 3 : 중장기적대응우위기술에있으면서생산경쟁력을보유하고있는국내산업분야에서유해물질 -free 제품을기획, 개발하여선도적그린제품으로국제경쟁력을갖도록주력 IEC 국제표준화회의에지속적으로참여, 모니터링하여, 국내기업에게유리한방향이될수있도록전개해나가야하며, 이에기업의견수렴을위한기업의참여가중요하다고사료됨

22 대응 2 사례 : 환경규제관련진행중인상황을한국에유리하게전개 IEC TC111 WG 3, 8th Meeting 2009, Berlin [Possible future standard] Combustion-Ion Chromatography (C-IC) Method for Total Bromine Analysis in IEC (Screening) 정재학책임연구원발표 April 15~16, 2009

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untitled PHTHALATES 2010 E&E Chemicals Team Laboratory Testing Services SGS Testing Korea Co., Ltd. PHTHALATES Phthalate (, plasticizer ) : (, softener) :,,,,. PVC(polyvinyl chloride) : 3 Phthalate DEHP, DBP, BBP