1、Designation:D 3417 99Standard Test Method forEnthalpies of Fusion and Crystallization of Polymers byDifferential Scanning Calorimetry(DSC)1This standard is issued under the fixed designation D 3417;the number immediately following the designation indicates the year oforiginal adoption or,in the case
2、 of revision,the year of last revision.A number in parentheses indicates the year of last reapproval.Asuperscript epsilon(e)indicates an editorial change since the last revision or reapproval.1.Scope1.1 This test method covers the determination of heat offusion and heat of crystallization of polymer
3、s by differentialscanning calorimetry.1.2 This test method is applicable to polymers in granularform(below 60 mesh preferred,avoid grinding if possible)orto any fabricated shape from which appropriate specimens canbe cut.1.3 The normal operating temperature range is from thecryogenic region to 600C.
4、1.4 The values in SI units are to be regarded as the standard.NOTE1True heats of fusion can only be determined in conjunctionwith structure investigation,and frequently,specialized crystallizationtechniques are needed.NOTE2This test method may be used in conjunction with TestMethod D 3418 or E 794 t
5、o simultaneously determine the temperatures ofmelting and crystallization.NOTE3This test method may not be applicable to all types ofpolymers as written(see 6.6).NOTE4Uncertain radiation losses at temperatures higher than 400Cmay affect the accuracy of results.1.5 This standard does not purport to a
6、ddress all of thesafety concerns,if any,associated with its use.It is theresponsibility 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.NOTE5The test method is similar but not equivalent to ISO
7、 11357-1and 11357-3.The ISO standard provides additional information notsupplied by this test method.2.Referenced Documents2.1 ASTM Standards:D 3418 Test Method for Transition Temperatures of Poly-mers by Thermal Analysis2E 473 Terminology Relating to Thermal Analysis3E 793 Test Method for Heats of
8、Fusion and Crystallizationby Differential Scanning Calorimetry3E 794 Test Method for Melting and Crystallization Tem-peratures by Thermal Analysis3E 968 Practice for Heat Flow Calibration of DifferentialScanning Calorimeters3E 1142 Terminology Relating to Thermophysical Proper-ties32.2ISO Standards:
9、411357-1 PlasticsDifferentialScanningCalorimetry(DSC)Part 1:General Principles11357-3 PlasticsDifferentialScanningCalorimetry(DSC)Part 3:Determination of Temperature and En-thalpy of Melting and Crystallization3.Terminology3.1 Specialized terms used in this test method are defined inTerminologies E
10、473 and E 1142.4.Summary of Test Method4.1 This test method consists of heating or cooling the testmaterial at a controlled rate in a specified purge gas at acontrolled flow rate and comparing the areas under the crys-tallization exotherm or fusion endotherm of the test materialagainst the respectiv
11、e areas obtained by the similar treatment ofa well-characterized standard.5.Significance and Use5.1 Differential scanning calorimetry provides a rapidmethod for determining enthalpy changes accompanied by thefirst-order transitions of materials.The heat of fusion,the heatof crystallization,and also
12、the effect of annealing can bedetermined in polymers that possess them.Differential scan-ning calorimetry may be used to assist in identifying specificpolymers,polymer alloys,and certain polymer additives thatexhibit thermal transitions.1This test method is under the jurisdiction ofASTM Committee D-
13、20 on Plasticsand is the direct responsibility of Subcommittee D20.30 on Thermal Properties(Section D20.30.07).Current edition approved April 10,1999.Published July 1999.Originallypublished as D 3417 75.Last previous edition D 3417 97.2Annual Book of ASTM Standards,Vol 08.02.3Annual Book of ASTM Sta
14、ndards,Vol 14.02.4Available from American National Standards Institute,11 W.42nd St.,13thFloor,New York,NY 10036.1Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959,United States.5.2 This test method is useful for both specification accep-tance and process
15、 control,and for research.6.Interferences6.1 An appreciable increase in particle size above thatspecified can alter the heat of fusion or crystallization.6.2 Changes in heating and cooling rate as well as in finalheating or cooling temperatures have a considerable effect onthe measured heats of fusi
16、on or crystallization.Therefore,departure from conditions specified for a given polymer is notpermitted.6.3 Since milligram quantities of a specimen are used,it isessential to ensure that specimens are homogeneous andrepresentative.6.4 Too large a specimen size above that specified can causeerror in the heat measurement.6.5 Toxic or corrosive effluents,or both,can be releasedwhen heating the material,and could be harmful to thepersonnel or to the apparatus.6.6 Not all polymers lend themselves to
