1、Designation:D151995(Reapproved 2014)Standard Test Methods forRubber ChemicalsDetermination of Melting Range1This standard is issued under the fixed designation D1519;the number immediately following the designation indicates the year oforiginal adoption or,in the case of revision,the year of last re
2、vision.A number in parentheses indicates the year of last reapproval.Asuperscript epsilon()indicates an editorial change since the last revision or reapproval.1.Scope1.1 These test methods cover the determination of themelting range of commercial rubber processing chemicalseither by use of capillary
3、 melting point tubes or by differentialscanning calorimetry(DSC).1.2 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.3 This standard does not purport to address all of thesafety concerns,if any,associated with its use.It is the
4、responsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:2D4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbo
5、n Black ManufacturingIndustriesE1 Specification for ASTM Liquid-in-Glass ThermometersE324 Test Method for Relative Initial and Final MeltingPoints and the Melting Range of Organic Chemicals(Discontinued 2001)(Withdrawn 2001)3E473 Terminology Relating to Thermal Analysis and Rhe-ologyE967 Test Method
6、 for Temperature Calibration of Differen-tial Scanning Calorimeters and Differential Thermal Ana-lyzers3.Terminology3.1 Definitions:3.1.1 differential scanning calorimetrysee TerminologyE473.4.Significance and Use4.1 This test method may be used for research and devel-opment.It also may be used for
7、quality assurance,provided astandard has been agreed upon between a producer and a user.4.2 For identification purposes,melting range should besupplemented by measurements of a more specific physical andchemical property.4.3 This test method is not recommended for rubber chemi-cals that decompose at
8、 their melting ranges.4.4 The melting range as determined by Test MethodACapillary Tube Melting Range is not recommended as acriterion of purity of a rubber chemical.5.Sampling5.1 Grind a representative sample of the chemical to betested with a mortar and pestle,if necessary,to pass completelythroug
9、h a 150-m(No.100)sieve.Use the sample withoutfurther treatment.TEST METHOD ACAPILLARY TUBE MELTINGRANGE6.Apparatus6.1 Melting ApparatusAny electric melting apparatus thatsatisfies the requirements of Test Method E324 may be used orany suitable manually heated oil bath such as Hershberg tube.6.2 Capi
10、llary TubeThe capillary tube to contain thesample shall be a glass tube approximately 150 mm long and1.2 to 1.4 mm in internal diameter with walls 0.2 to 0.3 mmthick and closed at one end.6.3 ThermometerThe thermometer shall be of the partialimmersion type and of suitable range selected from Specifi
11、ca-tion E1,or of an equivalent range as specified by the ChemicalManufacturers Association.It shall be divided into subdivi-sions of 0.5C(1F)or less.Corrections for the thermometershall be determined by calibration against a thermometercertified by National Institute of Standards and Technology.6.4
12、SieveA150-m(No.100)sieve for screening thesample shall be provided.1These test methods are under the jurisdiction of ASTM Committee D11 onRubber and is the direct responsibility of Subcommittee D11.11 on ChemicalAnalysis.Current edition approved Aug.1,2014.Published November 2014.Originallyapproved
13、in 1995.Last previous edition approved in 2009 as D1519 95(2009)1.DOI:10.1520/D1519-95R14.2For referenced ASTM standards,visit the ASTM website,www.astm.org,orcontact ASTM Customer Service at serviceastm.org.For Annual Book of ASTMStandards volume information,refer to the standards Document Summary
14、page onthe ASTM website.3The last approved version of this historical standard is referenced onwww.astm.org.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 7.Procedure7.1 Select the thermometer of the proper range and supportit so that it
15、 is immersed to the immersion mark in the liquid ofthe bath.7.2 Charge the capillary glass tube with sufficient powder toform a column in the bottom of the tube about 3 to 6-mm highwhen packed down as closely as possible by moderate tappingon a solid surface.7.3 Heat the bath until a temperature app
16、roximately 25Cbelow the expected melting range is reached.Then regulate therate of rise so that it averages about 3C/min for the rest of thedetermination except that the rate of rise is 1 6 0.2C/minduring the actual melting of the sample.When the temperaturehas risen to about 10C below the expected melting range,insert the capillary in the bath and adjust the height of the tubeso that the material in the capillary is beside the center of thethermometer bulb.The capillary tube is not placed in th