UL SUBJECT 746R-2018 UL Outline for Investigation Restricted Use Substances in Polymeric Materials (Issue 3).pdf

1、UL COPYRIGHTED MATERIAL NOT AUTHORIZED FOR FURTHER REPRODUCTION ORDISTRIBUTION WITHOUT PERMISSION FROM ULApril 27, 20181UL 746RRESTRICTED USE SUBSTANCES IN POLYMERIC MATERIALSIssue No. 3April 27, 2018Summary of TopicsThis Third Issue of the Outline of Investigation for Restricted UseSubstances In Po

2、lymeric Materials is being issued to add four newrestricted substances (bis(2-ethylhexyl) phthalate (DEHP), butyl benzylphthalate (BBP), dibutyl phthalate (DBP) and diisobutyl phthalate (DIBP)per the COMMISSION DELEGATED DIRECTIVE 2015/863 amending AnnexII to Directive 2011/65/EU.ULs Outlines of Inv

3、estigation are copyrighted by UL LLC. 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

4、 of ULLLC.COPYRIGHT 2018 UL LLCUL COPYRIGHTED MATERIAL NOT AUTHORIZED FOR FURTHER REPRODUCTION ORDISTRIBUTION WITHOUT PERMISSION FROM ULAPRIL 27, 2018UL 746R2No Text on This PageUL COPYRIGHTED MATERIAL NOT AUTHORIZED FOR FURTHER REPRODUCTION ORDISTRIBUTION WITHOUT PERMISSION FROM ULCONTENTSINTRODUCT

5、ION1 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 .87.1 Screening .87.2 Verification 98 Report .10CHARACTERIZATION TESTS9 General .1010 T

6、est Procedures 10APRIL 27, 2018 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

7、, mercury, hexavalent chromium, polybrominated biphenyls (PBBs),polybrominated diphenyl ethers (PBDEs), bis(2-ethylhexyl) phthalate (DEHP), butyl benzyl phthalate(BBP), dibutyl phthalate (DBP) and diisobutyl phthalate (DIBP) with respect to the maximum concentrationlevels specified in DIRECTIVE 2011

8、/65/EU OF THE EUROPEAN PARLIAMENT AND OF THE COUNCILof 8 June 2011 on the restriction of the use of certain hazardous substances in electrical and electronicequipment (recast) and the COMMISSION DELEGATED DIRECTIVE 2015/863 amending Annex II toDirective 2011/65/EU.1.2 These requirements may be appli

9、ed 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 requirements in the standard applicable to such a product.1.4 This Outline does not inves

10、tigate 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 series standards titled, “Determination of certain substances in electrotechnical produ

11、cts” 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 polyethylene compound) or discretely used as a uniform composite or layered material(e.g. co-ex

12、truded 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 any portion in any fashion such that they arerepresentative of the whole and compositio

13、nally 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 are representative of the whole and compositionallyequal to pieces similarly cut from a

14、ny other portion of the part/substance.APRIL 27, 2018UL 746R4UL COPYRIGHTED MATERIAL NOT AUTHORIZED FOR FURTHER REPRODUCTION ORDISTRIBUTION WITHOUT PERMISSION FROM UL3 Units of Measurement3.1 Values stated without parentheses are the requirement. Values in parentheses are explanatory orapproximate i

15、nformation.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 Samples5.1 Specimens representative of the material designation(s) under evaluation are to be

16、 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, construction and printing. Coloredspecimens shall be chosen according to the following:a) The natura

17、l 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 certain color pigments are known to be high risk for the presence of lead (Pb), cadmium (Cd),me

18、rcury (Hg), hexavalent chromium (Cr+6), polybrominated biphenyls (PBBs) or polybrominated diphenylethers (PBDEs), bis(2-ethylhexyl) phthalate (DEHP), butyl benzyl phthalate (BBP), dibutyl phthalate (DBP)and diisobutyl phthalate (DIBP), they are also to be provided.5.3 Layered or co-extruded material

19、s that can be readily separated by mechanical means shall beseparated and evaluated individually.5.4 Layered (co-extruded) materials that cannot be readily separated by mechanical means shall beevaluated such that if layer mass ratios vary disproportionally with thickness or composition variesotherw

20、ise, 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 evaluation is needed for use in this test program.APRIL 27, 2018 UL 746R 5UL COPYRIGHTED MATERIAL NOT AUTHORIZED FOR FURTHER REPRODUCTION ORDISTRIBUTION WI

21、THOUT PERMISSION FROM ULPERFORMANCE6 Test Apparatus & Procedure6.1 General6.1.1 The general testing approach and test methods shall consist of the screening and verificationmethods depicted in the Test Methods Flow Chart in IEC 62321-1, Determination of certain substancesin electrotechnical products

22、 Part 1: Introduction and overview. The referee method to be used shall bethe verification methods.6.1.2 Testing may start with screening or proceed directly to verification testing.6.2 Screening6.2.1 The requirements described in items (a) (d) are applicable to lead, mercury, cadmium, totalchromium

23、 and total bromine.a) The test apparatus and procedures for each substance shall be as described in IEC 62321-3-1, Determination of certain substances in electrotechnical products Part 3-1: Screening Lead, mercury, cadmium, total chromium and total bromine by X-ray fluorescence spectrometry.This tes

24、t 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-ray fluorescence (XRF)spectrometry.b) “Below Limit” (BL), “Incon

25、clusive” (IN) and “Over Limit” (OL) screening test results are inreference to the maximum concentration values specified in Annex II of DIRECTIVE 2011/65/EU OF THE EUROPEAN PARLIAMENT AND OF THE COUNCIL of 8 June 2011 on therestriction of the use of certain hazardous substances in electrical and ele

26、ctronic equipment(recast) and Table 7.5.c) X-ray fluorescence spectrometry (XRF) is unable to differentiate hexavalent chromiumincluding hexavalent chromium from all chromium species. Similarly, XRF is unable todifferentiate PBB or PBDE from all brominated compounds. Screening results for theseeleme

27、nts are therefore limited to “BL” or “IN”.d) The uncertainty estimate for each analyte shall be estimated as the sum of the repeatabilityof the analyser () and relative uncertainty expressed as a safety factor equal to 30% (50% forcomposite material) of the maximum allowed value of analyte concentra

28、tions and the“Acceptable Results” concentrations in Table 7.5. This uncertainty is reflected in the values for“BL”, “IN” and “OL”.6.2.2 The requirements described in items (a) and (b) are applicable to bis(2-ethylhexyl) phthalate(DEHP), butyl benzyl phthalate (BBP), dibutyl phthalate (DBP) and diiso

29、butyl phthalate (DIBP).a) The test apparatus and procedures for each substance shall be as described in IEC62321-8, Determination of certain substances in electrotechnical products Part 8: Phthalatesin polymers by gas chromatography-mass spectrometry (GC-MS), gas chromatography-massspectrometry usin

30、g a pyrolyzer/thermal desorption accessory (Py/TD-GC-MS). The “Py/TD-GC-MS” method shall be used for screening.APRIL 27, 2018UL 746R6UL COPYRIGHTED MATERIAL NOT AUTHORIZED FOR FURTHER REPRODUCTION ORDISTRIBUTION WITHOUT PERMISSION FROM ULb) The “Below Limit” (BL), “Inconclusive” (IN) and “Over Limit

31、” (OL) screening test resultthresholds for DEHP, BBP, DBP and DIBP are in reference to the maxiumum concentrationvalues specified in DIRECTIVE (EU) 2015/863 of 31 March 2015 amending Annex II toDirective 2011/65/EU of the European Parliament and of the Council as regards the list ofrestricted substa

32、nces and the “Acceptable Results” concentrations in Table 7.5.6.3 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, Determination

33、of certain substances in electrotechnicalproducts Part 5: Cadmium, lead and chromium in polymers andelectronics and cadmium and lead in metals by AAS, AFS, ICP-OES andICP-MSchromium (Cr)mercury (Hg) IEC 62321-4, Determination of certain substances in electrotechnicalproducts Part 4: Mercury in polym

34、ers, metals and electronics by CV-AAS,CV-AFS, ICP-OES and ICP-MShexavalent chromium (Cr(VI) IEC 62321-7-2, Determination of certain substances in electrotechnicalproducts Part 7-2: Hexavalent chromium Determination of hexavalentchromium (Cr(VI) in polymers and electronics by the colorimetric methodp

35、olybrominated biphenyls (PBBs)IEC 62321-6, Determination of certain substances in electrotechnicalproducts Part 6: Polybrominated biphenyls and polybrominated diphenylethers in polymers by gas chromatographymass spectrometry (GC-MS)polybrominated diphenyl ethers(PBDEs)bis(2-ethylhexyl) phthalate(DEH

36、P), butyl benzyl phthalate(BBP), dibutyl phthalate (DBP)and diisobutyl phthalate (DIBP)IEC 62321-8, Determination of certain substances in electrotechnicalproducts Part 8: Phthalates in polymers by gas chromatography-massspectrometry (GC-MS), gas chromatography-mass spectrometry using apyrolyzer/the

37、rmal desorption accessory (Py/TD-GC-MS)APRIL 27, 2018 UL 746R 7UL COPYRIGHTED MATERIAL NOT AUTHORIZED FOR FURTHER REPRODUCTION ORDISTRIBUTION WITHOUT PERMISSION FROM UL7 Evaluation of Test Results7.1 Screening7.1.1 Table 7.1 describes the “Below Limit” (BL), “Inconclusive” (IN) and “Over Limit” (OL)

38、 screening testresults including substance limits and actions for lead and mercury as described in informative Annex Aof IEC 62321-3-2.Table 7.1Screening evaluation of lead and mercuryResult Individual limits for lead and mercury(mg/kg)Action“Below Limit” (BL) 700-3 Acceptable, No Further Testing Re

39、quired“Inconclusive” (IN) 700-3 and 70-3 and 700-3 Proceed to Verification Testing7.1.4 Table 7.4 describes the “Below Limit” (BL), “Inconclusive” (IN) and “Over Limit” (OL) screening testresults including substance limits and actions for bis(2-ethylhexyl) phthalate (DEHP), butyl benzylphthalate (BB

40、P), dibutyl phthalate (DBP) and diisobutyl phthalate (DIBP) as described in InformativeAnnex N of IEC 62321-8.APRIL 27, 2018UL 746R8UL COPYRIGHTED MATERIAL NOT AUTHORIZED FOR FURTHER REPRODUCTION ORDISTRIBUTION WITHOUT PERMISSION FROM ULTable 7.4Screening evaluation of chromium and bromineResult Ind

41、ividual limits for for DEHP, BBP,DBP and DIBP (mg/kg)Action“Below Limit” (BL) 500 Acceptable, No Further Testing Required“Inconclusive” (IN) 500 and 125%), inspection and analyses of the chromium formulationcomponents chemical composition shall be performed.APRIL 27, 2018 UL 746R 9UL COPYRIGHTED MAT

42、ERIAL NOT AUTHORIZED FOR FURTHER REPRODUCTION ORDISTRIBUTION WITHOUT PERMISSION FROM UL7.2.3 All detected PBB and PBDE compounds shall be 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 compound

43、s detected below the limit of quantification.8 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

44、test method 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 thos

45、e indicated 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 In

46、fraredSpectroscopy 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 athermal analyzer with

47、 a thermogravimetric module. The test method is described in the Standard TestMethod for Rapid Thermal Degradation of Solid Electrical Insulating Materials by ThermogravimetricMethod, ASTM D3850, except that the specimen is to be heated at 20C (36F) per minute in a nitrogenatmosphere. The upper temp

48、erature limit is material dependent, with 650C (1200F) as the minimum.The purge gas is not changed to air for the percent ash determination. This analysis is further describedin the Thermogravimetry sections of the Reference Standard for Electrical Wires, Cables, and FlexibleCords, UL 1581, or the S

49、tandard 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 described 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 Indu