UL SUBJECT 746R-2014 Outline of Investigation for Restricted Use Substances in Polymeric Materials (Issue 1).pdf

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1、UL COPYRIGHTED MATERIAL NOT AUTHORIZED FOR FURTHER REPRODUCTION ORDISTRIBUTION WITHOUT PERMISSION FROM ULDecember 8, 20141UL 746RRESTRICTED USE SUBSTANCES IN POLYMERIC MATERIALSIssue No. 1December 8, 2014Summary of TopicsThis First Issue of the Outline of Investigation for Restricted UseSubstances I

2、n Polymeric Materials is being issued to facilitate testing asdescribed in:a) DIRECTIVE 2011/65/EU OF THE EUROPEAN PARLIAMENT ANDOF THE COUNCIL of 8 June 2011,b) IEC 62321 Edition 1.0 2013-06 series standards entitled,Determination of certain substances in electrotechnical products,c) IEC 62321 Edit

3、ion 1.0 2008-12, Determination of levels of sixregulated substances (lead, mercury, cadmium, hexavalent chromium,polybrominated biphenyls, polybrominated dihphenyl ethers), AnnexA (informative), Determination of PBB and PBDE in polymers byGC-MS, andd) IEC 62321 Edition 1.0 2008-12, Determination of

4、levels of sixregulated substances (lead, mercury, cadmium, hexavalent chromium,polybrominated biphenyls, polybrominated diphhenyl ethers), AnnexC (informative), Determination of hexavalent chromium (Cr(VI) inpolymers and electronics by the colorimetric method.ULs Outlines of Investigation are copyri

5、ghted by UL. Neither a printed norelectronic copy of an Outline of Investigation should be altered in any way. All ofULs Outlines of Investigation and all copyrights, ownerships, and rights regardingthose Outlines of Investigation shall remain the sole and exclusive property of UL.COPYRIGHT 2014 UND

6、ERWRITERS LABORATORIES INC.UL COPYRIGHTED MATERIAL NOT AUTHORIZED FOR FURTHER REPRODUCTION ORDISTRIBUTION WITHOUT PERMISSION FROM ULDECEMBER 8, 2014UL 746R2No Text on This PageUL COPYRIGHTED MATERIAL NOT AUTHORIZED FOR FURTHER REPRODUCTION ORDISTRIBUTION WITHOUT PERMISSION FROM ULCONTENTSINTRODUCTIO

7、N1 Scope .42 Glossary .43 Units of Measurement .54 Undated References 55 Samples .5PERFORMANCE6 Test Apparatus & Procedure .66.1 General .66.2 Screening .66.3 Verification Testing .77 Evaluation of Test Results .77.1 Screening .77.2 Verification 88 Report 9CHARACTERIZATION TESTS9 General 910 Test Pr

8、ocedures .9DECEMBER 8, 2014 UL 746R 3UL COPYRIGHTED MATERIAL NOT AUTHORIZED FOR FURTHER REPRODUCTION ORDISTRIBUTION WITHOUT PERMISSION FROM ULINTRODUCTION1 Scope1.1 These requirements cover tests and evaluation for the assessment of polymeric materials with regardto the presence of lead, cadmium, me

9、rcury, hexavalent chromium, polybrominated biphenyls (PBBs) andpolybrominated diphenyl ethers (PBDEs) with respect to the maximum concentration levels specified inDIRECTIVE 2011/65/EU OF THE EUROPEAN PARLIAMENT AND OF THE COUNCIL of 8 June 2011on the restriction of the use of certain hazardous subst

10、ances in electrical and electronic equipment(recast).1.2 These requirements may be applied to other material types if found to be appropriate.1.3 The final acceptance of materials certified to this outline of investigation is dependent upon its use inor as a complete product that complies with the r

11、equirements in the standard applicable to such a product.1.4 This Outline does not investigate other properties of materials including flammability, toxicity orenvironmental risks.2 Glossary2.1 For the purpose of this standard, the terms and definitions in the multi-part IEC 62321 Edition 1.02013-06

12、 series standards titled, “Determination of certain substances in electrotechnical products” apply.In addition, the following definitions also apply.2.2 HOMOGENEOUS Uniform in composition.2.3 MATERIAL A compound, part or substance that is discretely homogeneous throughout itsentirety (e.g. a polyeth

13、ylene compound) or discretely used as a uniform composite or layered material(e.g. co-extruded insulation) the compositional entities of which cannot be readily separated bymechanical means. These compounds, parts or substances are constructed such that:a) Homogeneous material pieces can be cut from

14、 any portion in any fashion such that they arerepresentative of the whole and compositionally equal to pieces similarly cut from any otherportion of the part/substance.b) Uniform composite or layered material pieces can be cut from any portion in a specificfashion (e.g. cross section) such that they

15、 are representative of the whole and compositionallyequal to pieces similarly cut from any other portion of the part/substance.DECEMBER 8, 2014UL 746R4UL COPYRIGHTED MATERIAL NOT AUTHORIZED FOR FURTHER REPRODUCTION ORDISTRIBUTION WITHOUT PERMISSION FROM UL3 Units of Measurement3.1 Values stated with

16、out parentheses are the requirement. Values in parentheses are explanatory orapproximate information.4 Undated References4.1 Any undated reference to a code or standard appearing in the requirements of this Outline shall beinterpreted as referring to the latest edition of that code or standard.5 Sam

17、ples5.1 Specimens representative of the material designation(s) under evaluation are to be employed in thesetests.5.2 Special consideration is to be given for evaluation of multiple sample types for a given designationbecause of compositional differences due to variation in color, finish, constructi

18、on and printing. Coloredspecimens shall be chosen according to the following:a) The natural color and the most heavily pigmented light and dark colors.b) The heaviest organic pigment loading (unless the most heavily pigmented light and darkcolors include the highest organic pigment level.)When certa

19、in color pigments are known to be high risk for the presence of halogenated substances, theyare also to be provided.5.3 Layered or co-extruded materials that can be readily separated by mechanical means shall beseparated and evaluated individually.5.4 Layered (co-extruded) materials that cannot be r

20、eadily separated by mechanical means shall beevaluated such that if layer mass ratios vary disproportionally with thickness or composition variesotherwise, the extreme mass ratios or composition variations are to be evaluated in the investigation.5.5 A minimum of 50 grams of each material under eval

21、uation is needed for use in this test program.DECEMBER 8, 2014 UL 746R 5UL COPYRIGHTED MATERIAL NOT AUTHORIZED FOR FURTHER REPRODUCTION ORDISTRIBUTION WITHOUT PERMISSION FROM ULPERFORMANCE6 Test Apparatus & Procedure6.1 General6.1.1 The general testing approach and test methods shall consist of the

22、screening and verificationmethods depicted in the Test Methods Flow Chart in IEC 62321-1 Edition 1.0 2013-06, Determinationof certain substances in electrotechnical products - Introduction and overview. The referee method to beused shall be the verification methods.6.1.2 Testing may start with scree

23、ning or proceed directly to verification testing.6.2 Screening6.2.1 The test apparatus and procedures for each substance shall be as described in IEC 62321-3-1Edition 1.0 2013-06 “Determination of certain substances in electrotechnical products Part 3-1:Screening Lead, mercury, cadmium, total chromi

24、um and total bromine by X-ray fluorescencespectrometry”. This test method describes the screening analysis of five substances, specifically lead(Pb), mercury (Hg), cadmium (Cd), chromium (Cr) and bromine (Br) in uniform materials found inelectrotechnical products, using the analytical technique of X

25、-ray fluorescence (XRF) spectrometry.6.2.2 “Below Limit” (BL), “Inconclusive” (IN) and “Over Limit” (OL) screening test results are in referenceto the maximum concentration values specified in Annex II of DIRECTIVE 2011/65/EU OF THEEUROPEAN PARLIAMENT AND OF THE COUNCIL of 8 June 2011 on the restric

26、tion of the use of certainhazardous substances in electrical and electronic equipment (recast) and Table 6.3.1.6.2.3 X-ray fluorescence spectrometry (XRF) is unable to differentiate hexavalent chromium includinghexavalent chromium from all chromium species. Similarly, XRF is unable to differentiate

27、PBB or PBDEfrom all brominated compounds. Screening results for these elements are therefore limited to “BL” or “IN”.6.2.4 The uncertainty estimate for each analyte shall be estimated as the sum of the repeatability of theanalyser () and relative uncertainty expressed as a safety factor equal to 30%

28、 (50% for compositematerial) of the maximum allowed value of analyte concentrations indicated in Table 6.1. This uncertaintyis reflected in the values for “BL”, “IN” and “OL”.DECEMBER 8, 2014UL 746R6UL COPYRIGHTED MATERIAL NOT AUTHORIZED FOR FURTHER REPRODUCTION ORDISTRIBUTION WITHOUT PERMISSION FRO

29、M UL6.3 Verification Testing6.3.1 The test apparatus and procedures for each substance shall be as shown in Table 6.1.Table 6.1Apparatus and procedure for testsSubstance Apparatus and Procedurelead (Pb)cadmium (Cd) IEC 62321-5 Edition 1.0 2013-06, Cadmium, lead and chromium inpolymers and electronic

30、s and cadmium and lead in metals by AAS, AFS,ICP-OES and ICP-MSchromium (Cr)mercury (Hg) IEC 62321-4 Edition 1.0 2013-06, Mercury in polymers, metals andelectronics by CV-AAS, CV-AFS, ICP-OES and ICP-MShexavalent chromium (Cr(VI) IEC 62321 Edition 1.0 2008-12, Annex C (informative), Determination of

31、hexavalent chromium (Cr(VI) in polymers and electronics by thecolorimetric methodpolybrominated biphenyls (PBBs)IEC 62321 Edition 1.0 2008-12, Annex A (informative), Determination ofPBB and PBDE in polymers by GC-MSpolybrominated diphenyl ethers(PBDEs)7 Evaluation of Test Results7.1 Screening7.1.1 L

32、ead (Pb), mercury (Hg), cadmium (Cd), chromium (Cr) and bromine (Br) test results found to be“Below Limit” (BL) are acceptable and no further testing is required.7.1.2 Lead (Pb), mercury (Hg), cadmium (Cd), chromium (Cr) and bromine (Br) test results found to be“Inconclusive” (IN) shall proceed to v

33、erification testing.7.1.3 Lead (Pb), mercury (Hg) and cadmium (Cd) test results found to be “Over Limit” (OL) areunacceptable and no further testing is required.DECEMBER 8, 2014 UL 746R 7UL COPYRIGHTED MATERIAL NOT AUTHORIZED FOR FURTHER REPRODUCTION ORDISTRIBUTION WITHOUT PERMISSION FROM UL7.2 Veri

34、fication7.2.1 Table 7.1 indicates the acceptable results for each substance.Table 7.1Evaluation of test resultsSubstance Acceptable results0.1% by masslead (Pb)mercury (Hg)hexavalent chromium (Cr(VI)Total polybrominated biphenyls (PBBs)Total polybrominated diphenyl ethers (PBDEs)cadmium (Cd) 0.01% b

35、y mass7.2.2 In the event that hexavalent chromium test results are found not applicable to the sample analyzed(i.e. matrix spike recovery is 125%), inspection and analyses of the chromium formulationcomponents chemical composition shall be performed.7.2.3 All detected PBB and PBDE compounds shall be

36、 included in the total summation of PBBs andPBDEs.7.2.4 The limit of quantification for each specific compound shall be used for summation for PBB andPBDE compounds detected below the limit of quantification.DECEMBER 8, 2014UL 746R8UL COPYRIGHTED MATERIAL NOT AUTHORIZED FOR FURTHER REPRODUCTION ORDI

37、STRIBUTION WITHOUT PERMISSION FROM UL8 Report8.1 The basic reporting elements are described in IEC 62321-1 Edition 1.0 2013-06 series standardstitled, Determination of certain substances in electrotechnical products.8.2 Additional reporting elements are described in the respective IEC 62321 test met

38、hod sections.CHARACTERIZATION TESTS9 General9.1 Analytical tests are to be conducted to establish a characterization for general descriptive purposesand to provide a comparative baseline for revealing compositional changes in production lots of thematerial. Tests are to be selected from those indica

39、ted in 10.1 - 10.8. Other characterization tests maysupplement or replace those described below.10 Test Procedures10.1 QUALITATIVE INFRARED ANALYSIS (QIA) - The infrared (IR) spectrum for each material isobtained by means of a Fourier-transform infrared (FTIR) spectrometer as described in the Infrar

40、edSpectroscopy sections of the Reference Standard for Electrical Wires, Cables, and Flexible Cords, UL1581, or the Standard for Polymeric Materials - Short Term Property Evaluations, UL 746A.10.2 THERMOGRAVIMETRY (TGA) - A thermal curve of each material is obtained by means of a thermalanalyzer with

41、 a thermogravimetric module. The test method is described in the Standard Test Method forRapid Thermal Degradation of Solid Electrical Insulating Materials by Thermogravimetric Method, ASTMD 3850, except that the specimen is to be heated at 20C (36F) per minute in a nitrogen atmosphere.The upper tem

42、perature limit is material dependent, with 650C (1200F) as the minimum. The purge gasis not changed to air for the percent ash determination. This analysis is further described in theThermogravimetry sections of the Reference Standard for Electrical Wires, Cables, and Flexible Cords,UL 1581, or the

43、Standard for Polymeric Materials - Short Term Property Evaluations, UL 746A.10.3 ELEMENTAL ANALYSIS (EA) - The elements of interest are to be quantified for each material usingmicrowave assisted sample preparation techniques employing acid digestion or, if appropriate, methodssimilar to those descri

44、bed for polyvinyl chloride (PVC) compounds in the Elemental Analysis section of theReference Standard for Electrical Wires, Cables, and Flexible Cords, UL 1581, (or by other means) usingan atomic absorption (AA) spectrophotometer or Inductively Coupled Plasma (ICP) spectrometerinstrumentation, or bo

45、th.10.4 DIFFERENTIAL SCANNING CALORIMETRY (DSC) - A thermal curve is to be obtained by meansa Differential Scanning Calorimeter (DSC). The test method is described in the Standard Test Method forTransition Temperatures of Polymers by Differential Scanning Calorimetry, ASTM D 3418, except that thespe

46、cimen is to be heated at 20C (36F) per minute in a nitrogen atmosphere without a preliminarythermal cycle. The upper temperature limit is typically 300C (570F), but may be adjusted depending onthe material degradation and melt temperatures. This analysis is further described in the DifferentialScann

47、ing Calorimetry sections of the Reference Standard for Electrical Wires, Cables, and Flexible Cords,UL 1581, and the Standard for Polymeric Materials - Short Term Property Evaluations, UL 746A.DECEMBER 8, 2014 UL 746R 9UL COPYRIGHTED MATERIAL NOT AUTHORIZED FOR FURTHER REPRODUCTION ORDISTRIBUTION WI

48、THOUT PERMISSION FROM UL10.5 ASH CONTENT - The ash content is to be determined using the direct-calcination procedure(Method A) described in ISO 3451-89, Part 5, covering methods for the ash-content analysis of polyvinylchloride (PVC) materials. This analysis is further described in the Determinatio

49、n of Ash Content section ofthe Reference Standard for Electrical Wires, Cables, and Flexible Cords, UL 1581.10.6 GEL PERMEATION CHROMATOGRAPHY (GPC) - Gel Permeation Chromatography (GPC) is tobe performed for PVC materials using liquid chromatography that employs a porous gel as a separationmedium. This method is designed to analyze the organic-soluble non-resin PVC compound components(for example, plasticizers) that appear within the working range of the column bank. This analysis is furtherdescribed in the Gel Permeation Chromatography section of the Re