UL SUBJECT 746H-2014 UL Outline for Investigation Non-Halogenated Materials (Issue 1).pdf

1、UL COPYRIGHTED MATERIAL NOT AUTHORIZED FOR FURTHER REPRODUCTION ORDISTRIBUTION WITHOUT PERMISSION FROM ULNovember 24, 20141UL 746HOutline of Investigation for Non-Halogenated MaterialsIssue No. 1November 24, 2014Summary of TopicsThis First Issue of the Outline of Investigation for Non-HalogenatedMat

2、erials, UL 746H, is being issued to document the assessmentof non-halogen materials based on testing and or requirements describedin:a) IEC 61249-2 Series, Materials for printed boards and otherinterconnecting structures Reinforced base materials, clad and unclad(Non-halogenated Parts 21-23, 26, 27,

3、 30, 33, 34, 38, 40),b) IEC 61189-2, Test methods for electrical materials, printed boardsand other interconnection structures and assemblies Part 2: Testmethods for materials for interconnection structures - Test 2C12 (TotalHalogen content in base materials),c) ASTM D7359, Standard Test Method for

4、Total Fluorine, Chlorine andSulfur in Aromatic Hydrocarbons and their Mixtures by OxidativePyrohydrolytic Combustion followed by Ion Chromatography Detection(Combustion Ion Chromatography-CIC), andd) IEC 62321-3-2, Determination Of Certain Substances InElectrotechnical Products Part 3-2: Screening T

5、otal bromine inpolymers and electronics by Combustion Ion Chromatography.ULs Outlines of Investigation are copyrighted 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 righ

6、ts regardingthose Outlines of Investigation shall remain the sole and exclusive property of UL.COPYRIGHT 2014 UNDERWRITERS LABORATORIES INC.UL COPYRIGHTED MATERIAL NOT AUTHORIZED FOR FURTHER REPRODUCTION ORDISTRIBUTION WITHOUT PERMISSION FROM ULNOVEMBER 24, 2014UL 746H2No Text on This PageUL COPYRIG

7、HTED MATERIAL NOT AUTHORIZED FOR FURTHER REPRODUCTION ORDISTRIBUTION WITHOUT PERMISSION FROM ULCONTENTSINTRODUCTION1 Scope .42 Glossary .43 Units of Measurement .54 Undated References 55 Samples .5PERFORMANCE6 Halogen Content Determination .67 Evaluation of Test Results .68 Report 7CHARACTERIZATION

8、TESTS9 General 810 Test Procedures .8NOVEMBER 24, 2014 UL 746H 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 materials intended for variousapplicatio

9、ns as non-halogenated or non-chlorine and non-bromine.1.2 These requirements cover combustible materials including insulating materials and devices (e.g.plastics, printed-wiring boards, insulating materials and systems, labels, tape, tubing and sleeving), colorconcentrates, and wire and cable compou

10、nds.1.3 The requirements may be applied to other material types if found to be appropriate.1.4 The final acceptance of a material meeting the non-halogenated or non-chlorine and non-brominerequirements in this standard is dependent upon its use in or as a complete product that complies withthe requi

11、rements in the standard applicable to such a product.1.5 The flammability, toxicity or environmental risks associated with non-halogenated or non-chlorine andnon-bromine materials in any form, or the acceptability of these materials for uses other than indicated,are not within the scope of these req

12、uirements.2 Glossary2.1 For the purpose of this standard the following definitions apply:2.2 HALOGEN Elemental bromine, chlorine and fluorine. Other halogen elements (e.g. iodine andastatine) are not included in this definition.2.3 HOMOGENEOUS Uniform in composition.2.4 MATERIAL A compound, part or

13、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-extruded insulation) the compositional entities of which cannot be readily separated bymechanical means. These compounds, parts or subs

14、tances 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 compositionally equal to pieces similarly cut from any otherportion of the part/substance.b) Uniform composite or layered material pieces can b

15、e 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 any other portion of the part/substance.2.5 NON-HALOGENATED A material containing: a maximum of 900 mg/kg (0.09% by mass) ofelemental

16、bromine, a maximum of 900 mg/kg (0.09% by mass) of elemental chlorine, a maximum of900 mg/kg (0.09% by mass) of elemental fluorine and a maximum total halogen content of 1500 mg/kg(0.15% by mass).2.6 NON-CHLORINE AND NON-BROMINE A material containing: a maximum of 900 mg/kg (0.09%by mass) of element

17、al bromine, a maximum of 900 mg/kg (0.09% by mass) of elemental chlorine and amaximum total chlorine and bromine content of 1500 mg/kg (0.15% by mass) as indicated in IEC61249-2 series standards relating to “reinforced base materials, clad and unclad” (Non-halogenatedParts 21-23, 26, 27, 30, 33, 34,

18、 38, 40).NOVEMBER 24, 2014UL 746H4UL 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 information.4 Undated Refere

19、nces4.1 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 employed in thesetests.5.2

20、 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 natural color and the most heavil

21、y 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 halogenated substances, theyare also to be provided.5

22、.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 readily separated by mechanical means shall beevaluated such that if layer mass ratios vary disproportionally with thi

23、ckness 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 evaluation is needed for use in this test program.NOVEMBER 24, 2014 UL 746H 5UL COPYRIGHTED MATERIAL NOT AUTHORIZED FOR F

24、URTHER REPRODUCTION ORDISTRIBUTION WITHOUT PERMISSION FROM ULPERFORMANCE6 Halogen Content Determination6.1 The direct determination of total chlorine, bromine and fluorine content in materials shall bedetermined analytically by combustion - ion chromatography techniques based on the following testme

25、thods:a) IEC 61189-2 Test methods for electrical materials, printed boards and other interconnectionstructures and assemblies Part 2: Test methods for materials for interconnection structures-Test 2C12, Total Halogen Content In Base Materials;b) ASTM D7359, Standard Test Method for Total Fluorine, C

26、hlorine and Sulfur in AromaticHydrocarbons and their Mixtures by Oxidative Pyrohydrolytic Combustion followed by IonChromatography Detection (Combustion Ion Chromatography-CIC);c) IEC 62321-3-2, Determination Of Certain Substances In Electrotechnical Products Part3-2: Screening Total bromine in poly

27、mers and electronics by Combustion IonChromatography.6.2 Where not included in the test methods indicated above, calibration and qualification of the testapparatus and result calculation shall include bromine, chlorine and fluorine.6.3 This determination identifies the presence and quantity of halog

28、en elements (chlorine, bromine andfluorine) individually. The individual analyte species measured by this technique are halides (e.g. chloride,bromide, and fluoride) and are directly proportional to the respective halogen elements.6.4 The halogen content determination is suitable for the analysis of

29、 chlorine, bromine and fluorinecontent of 10 mg/kg to 1500 mg/kg or less. This method can be applied to samples containing chlorine,bromine, and fluorine at higher levels by employing dilution techniques to bring the total concentrationswithin the appropriate calibration range of the instrument.7 Ev

30、aluation of Test Results7.1 Table 7.1 below indicates the acceptable results for each non-halogenated material evaluation.NOVEMBER 24, 2014UL 746H6UL COPYRIGHTED MATERIAL NOT AUTHORIZED FOR FURTHER REPRODUCTION ORDISTRIBUTION WITHOUT PERMISSION FROM ULTable 7.1Evaluation of test resultsHalogen(s) Re

31、sults (% By Mass)chlorine (Cl) 0.09bromine (Br) 0.09fluorine (F) 0.09Total chlorine, bromine andfluorine 0.157.2 Table 7.2 below indicates the acceptable results for non-chlorine and non-bromine materialevaluation.Table 7.2Evaluation of test resultsHalogen(s) Results (% By Mass)chlorine (Cl) 0.09bro

32、mine (Br) 0.09Total chlorine and bromine 0.158 Report8.1 The report shall include:a) Reference to Outline UL 746H,b) Test method(s) performed,c) Date of the test,d) Identification and description of the specimen,e) Average individual halide content of three (3) specimens in mg/kg,f) Average total ha

33、logen content or total chlorine and bromine content of three (3) specimens inmg/kg, andg) Method detection limit.NOVEMBER 24, 2014 UL 746H 7UL COPYRIGHTED MATERIAL NOT AUTHORIZED FOR FURTHER REPRODUCTION ORDISTRIBUTION WITHOUT PERMISSION FROM ULCHARACTERIZATION TESTS9 General9.1 Analytical tests are

34、 to be conducted on specimens of the non-halogenated or non-chlorine andnon-bromine material(s) to establish a characterization for general descriptive purposes. The choice oftests is to be based on the composition of the material(s). Other identification tests appropriate for theparticular material

35、(s) composition may supplement or replace the described tests.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 InfraredSpectroscopy sections of the Ref

36、erence 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 a thermogravimetric module. The t

37、est 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 temperature limit is material depende

38、nt, 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 Standard for Polymeric Materials -

39、 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) c

40、ompounds 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 both.10.4 DIFFERENTIAL SCANNING CALO

41、RIMETRY (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 thespecimen is to be heated at 20C (36F)

42、 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 DifferentialScanning Calorimetry sections of the Re

43、ference Standard for Electrical Wires, Cables, and Flexible Cords,UL 1581, and the Standard for Polymeric Materials - Short Term Property Evaluations, UL 746A.10.5 ASH CONTENT - The ash content is to be determined using the direct-calcination procedure(Method A) described in ISO 3451-89, Part 5, cov

44、ering methods for the ash-content analysis of polyvinylchloride (PVC) materials. This analysis is further described in the Determination of Ash Content section ofthe Reference Standard for Electrical Wires, Cables, and Flexible Cords, UL 1581.NOVEMBER 24, 2014UL 746H8UL COPYRIGHTED MATERIAL NOT AUTH

45、ORIZED FOR FURTHER REPRODUCTION ORDISTRIBUTION WITHOUT PERMISSION FROM UL10.6 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

46、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 Reference Standard for Electrical Wires,Cables, and Flexible Cords, UL 1581.

47、10.7 MELT FLOW - A melt flow rate of each material is to be obtained by means of a melt flowindexer/extrusion plastometer using the method described in the Standard Test Method for Melt FlowRates of Thermoplastics by Extrusion Plastometer, ASTM D 1238.10.8 SPECIFIC GRAVITY - The specific gravity of

48、each material is to be obtained by means of ananalytical balance using the method described in the Standard Test Methods for Density and SpecificGravity (Relative Density) of Plastics by Displacement, ASTM D 792, or by other, equivalent means.10.9 HALOGEN CONTENT: X-ray fluorescence spectrometry (XRF) or Beilstein testing may optionally beperformed to confirm the presence or absence of halogen elements.NOVEMBER 24, 2014 UL 746H 9UL COPYRIGHTED MATERIAL NOT AUTHORIZED FOR FURTHER REPRODUCTION ORDISTRIBUTION WITHOUT PERMISSION FROM ULNOVEMBER 24, 2014UL 746H10No Text on This Page