最新电子电气产品中有毒有害物质检测方法

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1、电子电气产品中有毒有害物质检测方法Determination of Levels of Six Regulated Substances (Lead, Mercury, Hexavalent Chrominum, Polybrominated Biphenyls, Polybrominated Biphenyl Ether) in Electrotechnical Products 郑建国 博士Dr. Zheng JianguoGuangdong Entry-Exit Inspection & Quarantine Bureau, P.R.China Comparisons of Testin

2、g methods of ISO/IEC, GB and SN for RoHS 13 methods in ISO/IEC 62321 12 methods in GB series standards 22 methods in SN series standards Details in Table 1.SN series Standards for RoHS TestingMethodsProcedures of the mechanical disjointment for the determination of regulated substances in electrotec

3、hnical productsGeneral RequirementsConformity Assessmentlead, mercury, cadmium, chromiumChromium（VI）PBB、PBDEscreeningXRFXRFSpot-testSpot-testSparkSparkIRIRICP-AESAASICP-MSCVAASAFSUV-VISICGC-MSGC-MSLC-MSLC-MSGC-ECDGC-ECDGC-FIDGC-FIDHPLCHPLC15 methods in SN series standards for RoHS have been finished

4、: 1、Determination of Chromium（VI）in electrical and electronic equipment1,5-Diphenylcarbohydrazide spectrophotometry Cr (VI) compound was extracted from sample using basic extract solution with shaking at 9095 water bath for 1.5 hours, which can react with 1,5-Diphenylcarbohydrazide to appear a kind

5、of amaranthine complex in acid medium. Then, this complex was detected at wavelength 540 nm with UV spectrometry. 15 methods in SN series standards for RoHS have been finished: 、Determination of mercury in electrical and electronic equipmentHydride generation-atomic fluorescence spectrometry As to m

6、etal material in electrical and electronic equipment, it was digested with routine acid digestion. And to the other material, it was digested with airtight high-temperature press bomb. After digestion, mercury in sample material can be digested into dissoluble salt. And finally, obtained digestion s

7、olution was detected using Hydride generation-atomic fluorescence spectrometry.15 methods in SN series standards for RoHS have been finished: 、Determination of lead, cadmium and chromium in electrical and electronic equipmentFlame atomic absorption spectrometryAs to metal material in electrical and

8、electronic equipment, it was digested with routine acid digestion with concentrated nitric acid,and for the other material, it was digested with concentrated HNO3、H2O2 and HF（specially for the glass and chinaware material）at 1805 for 4 hours by using airtight high-temperature press bomb. After diges

9、tion, lead, cadmium and chromium in sample material can be digested into dissoluble salt. And finally, obtained digestion solution was detected using flame atomic absorption spectrometry. 15 methods in SN series standards for RoHS have been finished: 、Qualitative screening of lead, mercury, cadmium,

10、 chromium and bromine in electrical and electronic equipmentWavelength dispersive X-ray fluorescence spectrometryBased on the lead, mercury, cadmium, chromium and bromines characteristic X-ray lines, the wavelength dispersive x-ray fluorescence spectrometry (WDXRF) can be used for qualitative screen

11、ing the prepared sample. When the elements characteristic X-ray peak appears in the qualitative screening result, it approve that the element exist in the sample. When the elements characteristic X-ray peak doesnt appear in the qualitative screening result, it approve that the elements content is lo

12、wer than the detection limit of WDXRF. 15 methods in SN series standards for RoHS have been finished: 、Determination of polybrominated biphenyls and polyborminated biphenyl ethers in electrical and electronic equipmentHigh Performance Liquid chromatographyTechnical flame retardants such as polybromo

13、 biphenyls and polybromo biphenyl ethers in electrical and electronic equipment were separated and determined by high performance liquid chromatography method. The samples were extracted with 150mL toluene in a soxhlet apparatus for three hours. The HPLC separation was achieved on a reversed-phase C

14、18 column, applying gradient elution using a mixture of aqueous phosphate buffer and methanol with ultraviolet detection in the scanning mode at 226nm. 15 methods in SN series standards for RoHS have been finished: 、Determination of polybrominated biphenyls and polyborminated biphenyl ethers in elec

15、trical and electronic equipmentGas chromatography/Mass spectrometry The electrical and electronic equipment samples were extracted with 150mL toluene in a soxhlet apparatus for three hours. The extracted solution was purified by silica gel column and then concentrated in rotary vacuum evaporator. Th

16、e residue was taken up in 2.0 mL toluene. Polybromo biphenyls and polybromo biphenyl ethers were separated and determined by Gas chromatography/Mass spectrometry.15 methods in SN series standards for RoHS have been finished: 、Determination of polybrominated biphenyls and polyborminated biphenyl ethe

17、rs in electrical and electronic equipmentGCFIDThe electrical and electronic equipment samples were extracted with 150mL toluene in a soxhlet apparatus for three hours. The extracted solution was purified by silica gel column and then concentrated in rotary vacuum evaporator. Internal standard in 1.0

18、 mL toluene was added to the residue, polybromo biphenyls and polybromo biphenyl ethers in the mixture were separated and determined by Gas chromatography with flame ion detector. 15 methods in SN series standards for RoHS have been finished: 、Qualitative screening of polybrominated biphenyls and po

19、lyborminated biphenyl ether in electrical and electronic equipment by infra-red spectrometric methodThe method is to collect the infra-red spectrum of plastic part of the electric or electronic equipments, analyzing the polymeric component. Comparing the spectrum of the sample with the reference spe

20、ctrum of the relative polymer, to determine whether the sample spectrum contains the characteristic peaks of the C-Br bond within the 650cm-1500cm-1 region, and, to figure out whether the sample contains PBB or PBDE. 15 methods in SN series standards for RoHS have been finished: 、Quantitative Screen

21、ing of Lead, Mercury, Chromium, Cadmium and Bromine in Electrical and Electronic EquipmentX-Ray Fluorescence Spectrometric MethodWavelength dispersive X-ray fluorescence spectrometry (WD-XRF) has been applied to the direct quantitative screening of lead(Pb), mercury(Hg), chromium(Cr), cadmium(Cd), b

22、romine(Br) in electrical and electronic equipments. It covers all material types such as polymers, metals, and other electronic assembly materials. A series of six polymers reference materials and other matrix reference materials were prepared to make calibration curves. Determination of the element

23、al concentrations for the references and samples was analyzed by WD-XRF. 15 methods in SN series standards for RoHS have been finished: 、Determination of polybrominated biphenyls and polybrominated diphenyl ethers in electrical and electronic equipment With HPLC/MS-MS A HPLC/MS-MS method for the det

24、ermination of polybrominated biphenyls and polybrominated diphenyl ethers in electrical and electronic equipments was established. The polybrominated biphenyls and polybrominated diphenyl ethers was extracted with toluene using ultrasonator from samples and detected by HPLC/MS-MS.15 methods in SN se

25、ries standards for RoHS have been finished: 11、Determination of Lead and Cadmium in in electrical and electronic equipment by AFSThe method is used for he determination of lead and Cadmium in a) polymers; b) metal materials made from aluminium, iron and zinc matrices and c) electronics. The sample i

26、s digested and heated to exhausting the acids, then diluted properly. Ionic Cd in the sample solution reacts with KBH4 and generates volatile gas, which is introduced to atomizer with carrier gas (Ar). The content of cadmium is determined on the basis of fluorescence intensity of the element.Ionic P

27、b() in the sample solution is oxidized into Pb() by potassium ferricyanide, then reacts with KBH4 and generates volatile hydride PbH4, which is introduced to atomizer with carrier gas (Ar). The content of lead is determined on the basis of fluorescence intensity of the element. 15 methods in SN seri

28、es standards for RoHS have been finished: 12、Determination of Lead, Cadmium, Chromium and Mercury in electrical and electronic equipmentInductively coupled plasma atomic emission spectrometry The samples of polymer materials (such as PP, PE, PS, ABS, PVC, etc.) and electronics (such as glasses and c

29、eramics, etc.) from Electronic and electrical equipment were digested under pressure with nitric acid, tetrafluoroborate solution and hydrogen peroxide in a tightly sealed PTFE vessel which was then put into the corrosion resisting steel pressure dissolution can. The pressure dissolution can as a wh

30、ole was heated at 180 for 4h in a constant temperature heating oven. The samples of metallic materials (such as iron alloys, copper alloys, aluminum alloys, zinc alloys and solder alloys, etc.) from Electronic and electrical equipment were digested by heating with reflux cooler and absorption vessel

31、s. The samples of polymer materials and electronics from Electronic and electrical equipment were digested under pressure with microwave sample preparation system. The method for the simultaneous determination of Pb, Cd, Cr, Hg in polymer materials, metallic materials and electronics from Electronic

32、 and electrical equipment have been developed 15 methods in SN series standards for RoHS have been finished: 、Determination Of Mercury In Electrical And Electronic Equipment Cold Vapor Atomic Absorption SpectrometryThis standard provides the procedure for the determination of materials used in Elect

33、rical And Electronic Equipment. These materials are polymer materials, metal materials and electronics. Metal materials in electrotechnical equipment are treated by traditional digestion using acids. Other materials, such as polymers and electronics, were digested with acids, in microwave oven or in

34、 a sealed and high pressure autoclave. The mercury in the digestion solution is reduced to the atomic state before it is analyzed, then mercury is determined by Cold Vapor Atomic Absorption Spectrometry. 15 methods in SN series standards for RoHS have been finished: 14、Technical Requirements for the

35、 Conformity Assessment of Certain Hazardous Substances in Electrical and Electronic EquipmentThis standard specifies the general technical requirements for the conformity assessment of certain hazardous substances in electrical and electronic equipments. For the purpose of determining the conformity

36、 of the products with relevant laws and regulations and evaluating the validity of the test results, the following items should be assessed and certified to be fully in compliance with specific technical requirements. 15 methods in SN series standards for RoHS have been finished: 、Procedures of the

37、mechanical disjointment for the determination of regulated substances in electrotechnical productsThis part specifies the procedures and requirements of the mechanical disjointment of electrotechnical products into test units for chemical determination of certain regulated substances.This part deals

38、 with the mechanical disjointment of electrical and electronic products (including their parts and components) with rated voltage not exceeding 1 000 volts for alternating current and 1 500 volts for direct current;Thank you for your attention!This part deals with but is not limited to the following

39、 categories of products:large household electrical appliancessmall household electrical appliancesinformation technology equipment and telecommunication equipmentConsumer equipmentLighting equipmentElectrical and electronic toolsToys, leisure and sports equipmentMedical devicesMonitoring and control

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