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1、Method for Analyzing Substances Under the RoHS RestrictionsRevision 1.0Nitto Denko Corporation1. Definitions of TermsTermDescriptionThreshold value Acceptable condensation of target substanceSubstance analyzedThe following substances stipulated by the ELV and RoHS Directive:Cadmium, lead, mercury, h
2、exavalent chromium, and specified bromine-based flame retardants (PBB and PBDE)Analyzed dataResults of analysis performed according to the methods described in this instruction manualPrecision analysisAnalysis that identifies the content of the target substancesScreening analysis Analysis that ident
3、ifies the element content of the target substances (Simplified analysis)XRFAbbreviation for X-ray fluorescenceICPGeneric term for ICP-AES (inductively-coupled plasma emission spectrophotometer) and ICP-MS (inductively-coupled plasma mass spectroscope)AASAbbreviation for atomic absorption spectromete
4、rGC/MSAbbreviation for gas chromatograph-mass spectroscopeICAbbreviation for ion chromatograph analyzerPacking materials(1) Packing materials that are used for raw materials to be delivered(2) Packing materials that are used for packing products from the Nitto Denko group companies2. PurposeThe purp
5、ose of this manual is to clearly define the methods of analysis to identify six substances which are restricted for use by EU Directive such as ELV and RoHS and to control procurement activities under the legal restrictions of the industry concerning chemical substances In products3. Target Substanc
6、e for Analysis The method of analysis shall apply to cadmium, lead, mercury, hexavalent chromium, and specified bromine-based flame retardants (PBB and PBDE) concerning raw materials delivered to the Nitto Denko Group (including packing materials used for raw materials to be delivered thereto) and p
7、acking materials for packing products from the Nitto Denko Group.4. Overview of Method of AnalysisYou are requested to verify the materials for delivery to the Nitto Denko group to confirm that such materials do not include the target substances exceeding the acceptable concentration levels. Table 1
8、 shows the method of analysis and acceptable concentration levels (threshold values). As for the method of analysis, be sure to follow the instructions of the requesting department.TableMethod of AnalysisThreshold Values (ppm)Precision AnalysisScreening AnalysisRaw MaterialPacking MaterialCadmiumICP
9、 methodXRF5Total 100LeadICP methodXRF100Hexavalent chromiumDiphenylcarbazide optical density methodXRFICP method100MercuryICP methodXRF100PBBsGC/MS methodXRFIC method100-PBDEs (incl. decabromodiphenylether)100-5. Methods of Analysis and Determination5.1 CadmiumAs for the quantitative limit, methods
10、shall be permitted that guarantee the following values: Raw materials for which the “Non-Inclusion Guarantee Concerning Specified Chemical Substances” has been submitted: less than 5 ppm Other than the above: less than 20 ppm-1 XRF (1) When wavelength dispersive XRF is used, measurements shall be co
11、nducted after adequate pretreatment. It should be noted that if cadmium is added to the solution, it must be fully dissolved.(2) When energy dispersive XRF is used, measurements shall be conducted with a measured value of +.-2 ICP Method (1) PretreatmentThe following four types of pretreatment metho
12、ds can be used:Ashing method in the presence of sulfuric acid:Pressurized acid decomposition method in an airtight vessel, including microwavedecomposition methods, for example, EN 13346: 2000 and EPA3052 (1996);Acid decomposition method using nitric acid, hydrogen peroxide solution, or hydrochloric
13、 acid. For example, EPA3050B Rev. 2 (1996); or Wet decomposition method using sulfuric acid, nitric acid, or hydrogen peroxide solution. For example, BS EN1122 (2001). If any deposits (insoluble substances) are generated, it is necessary to fully resolve such deposits into solution in some way (alka
14、line elution procedure, etc.).(2) Measuring MethodFor the measuring method, the following three types of methods shall be permitted: Inductively-coupled plasma emission spectrophotometer (ICP-AES, ICP-OES). For example, EN ISO 11885 (1998) Atomic absorption spectrometer (AAS). For example, EN ISO 59
15、61 (1995). Inductively-coupled plasma mass spectroscope (ICP-MS).Note：The elution analysis method as represented by EN71-3 (1994), ASTM F963-96a, ASTM D 5117, and ISO 8124-3 cannot be applied for pretreatment.Adscript pretreatment methods are mandatory since JIS K 0102-55, which is a method for indu
16、strial wastewater analysis, only refers to measuring methods.5.2 LeadMethods shall be permitted that guarantee that the determination limit is less than 20 ppm.-1 XRF(1) When wavelength dispersive XRF is used, measurements shall be conducted after adequate pretreatment. It should be noted that if le
17、ad is added to the solution, it must be fully dissolved.(2) When energy dispersive XRF is used, measurements shall be conducted with a measured value of +.-2 ICP Method(1) PretreatmentThe following four types of pretreatment methods can be used:Ashing method in the presence of sulfuric acid;Pressuri
18、zed acid decomposition method in an airtight vessel, including the microwave decomposition methods, for example, EN 13346: 2000 and EPA3052 (1996);Acid decomposition method using nitric acid, hydrogen peroxide solution, or hydrochloric acid. For example, EPA3050B Rev. 2 (1996); orWet decomposition m
19、ethod using sulfuric acid, nitric acid, or hydrogen peroxide solution. For example, BS EN1122 (2001). If any deposits (insoluble substances) are generated, it is necessary to fully resolve such deposits in the solution in some way (alkaline elution procedure, etc.).(2) Measuring MethodFor the measur
20、ing method, the following three types of methods shall be permitted:Inductively-coupled plasma emission spectrophotometer (ICP-AES, ICP-OES). For example, EN ISO 11885 (1998);Atomic absorption spectrometer (AAS). For example, EN ISO 5961 (1995); orInductively-coupled plasma mass spectroscope (ICP-MS
21、).Note： The elution analysis method as represented by EN71-3 (1994), ASTM F963-96a, ASTM D 5117, and ISO 8124-3 cannot be applied for pretreatment.Adscript pretreatment methods are mandatory since JIS K 0102-55, which is a method for industrial wastewater analysis, only refers to measuring methods.5
22、.3 MercuryMethods shall be permitted that guarantee that the determination limit is less than 20 ppm.-1 XRF(1) When wavelength dispersive XRF is used, measurements shall be conducted after adequate pretreatment. It should be noted that if mercury is added to the solution, it must be fully dissolved.
23、(2) When energy dispersive XRF is used, measurements shall be conducted with a measured value of +.-2 ICP Method(1) PretreatmentThe following three types of pretreatment methods can be used:Pressurized acid decomposition method in a airtight vessel, includingmicrowave decomposition methods, for exam
24、ple, EPA3052 (1996);Heating vaporization - atomic absorption method;Wet decomposition method with sulfuric acid, or nitric acid by using a decomposition flask with reflux condenser (Kjeldahl method).For each of the above-stated methods, avoid allowing sublimation of mercury. In addition, if any depo
25、sits are generated, it is necessary to resolve such deposits in the solution in some way.(2) Measuring MethodMeasurements can be made with similar methods as those for cadmium or lead. However, if use of low-concentration mercury is anticipated, analysis with chemical-reduction vaporization atomic a
26、bsorption method, ICP-AES (ICP-OES) method, or ICP-MS method will be considered to be appropriate.5.4 Hexavalent ChromiumMethods shall be permitted that guarantee that the determination limit is less than 20 ppm.-1 XRF (Whole Chromium)(1) When wavelength dispersive XRF is used, measurements shall be
27、 conducted after adequate pretreatment It should be noted that if mercury is added to the solution, it must be fully dissolved.(2) When energy dispersive XRF is used, measurements shall be conducted with a measured value of +.If the determined value exceeds 100 ppm, execute precision analysis of hex
28、avalent chromium (diphenylcarbazide optical density method) for another determination.-2 ICP Method (Whole Chromium)(1) PretreatmentThe following four types of pretreatment methods can be used:Ashing method in the presence of sulfuric acid;Pressurized acid decomposition method in an airtight vessel,
29、 including microwave decomposition methods, for example, EN 13346: 2000and EPA3052 (1996);Acid decomposition method using nitric acid, hydrogen peroxide solution, or hydrochloric acid. For example, EPA3050B Rev. 2 (1996); orWet decomposition method using sulfuric acid, nitric acid, or hydrogen perox
30、ide solution. For example, BS EN1122 (2001). If any deposits (insoluble substances) are generated, it is necessary to fully resolve such deposits in the solution in some way (alkaline elution procedure, etc.).(2) Measuring MethodFor the measuring method, the following three types of methods shall be
31、 permitted:Inductively-coupled plasma emission spectrophotometer (ICP-AES, ICP-OES). For example, EN ISO 11885 (1998);Atomic absorption spectrometer (AAS). For example, EN ISO 5961 (1995); orInductively-coupled plasma mass spectroscope (ICP-MS). If the determined value exceeds 100 ppm, execute preci
32、sion analysis of hexavalent chromium (diphenylcarbazide optical density method) for another determination.-3 Diphenylcarbazide Optical Density Method(1) PretreatmentMethod for extracting purified water from inert gas conforming to DIN 53314(2) Measuring MethodDiphenylcarbazide optical density method
33、 (JIS K 0102)5.5 PBB and PBDEMethods shall be permitted that guarantee that the determination limit is less than 20 ppm.-1 XRF (Whole Bromine)(1) When wavelength dispersive XRF is used, measurements shall be conducted after adequate pretreatment. It should be noted that if mercury is added to the so
34、lution, it must be fully dissolved.(2) When energy dispersive XRF is used, measurements shall be conducted with a measured value of +. If the determined value exceeds 30 ppm, execute precision analysis of PBB and PBDE (GC/MS method) for another determination.-2 IC Method (Whole Bromine)(1) Pretreatm
35、entCombustion gas sampling(2) Measuring MethodIon chromatograph analyzerIf the determined value exceeds 30 ppm, execute precision analysis of PBB and PBDE (GC/MS method) for another determination.-3 GC/MS Method(1) PretreatmentDissolution - Extraction(2) Measuring MethodGas chromatograph-Mass Spectr
36、oscope6. Method for Judging Packing Materials(1) Screening Analysis It is judged acceptable if the total levels of cadmium, lead, mercury, and whole chromium are less than 100 ppm. If the total levels of cadmium, lead, mercury, and whole chromium are 100 ppm or over, execute precision analysis of he
37、xavalent chromium (diphenylcarbazide optical density method) and make the determination based on the total levels of cadmium, lead, mercury, and chromium. When energy dispersive XRF is used, the determination shall be made by totaling the measured value of + of each substance.(2) Precision AnalysisT
38、he determination shall be made based on the total levels of cadmium, lead, mercury, and chromium.7. Items Included in the Analysis ReportThe following items shall be included in the analysis report:Name of institution that performed the analysis (if measured by an outside analysis institute);Analysis method (pretreatment method, measuring instruments, etc.)Date of analysisAnalysis results (only for energy dispersive XRF)Analysis flow chart (cadmium and lead shall be essential)
