1、Designation: D 6604 00Standard Practice forGlass Transition Temperatures of Hydrocarbon Resins byDifferential Scanning Calorimetry1This standard is issued under the fixed designation D 6604; the number immediately following the designation indicates the year oforiginal adoption or, in the case of re
2、vision, 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 practice covers determination of glass transitiontemperatures of hydrocarbon (HC) resins by
3、differential scan-ning calorimetry (DSC).1.2 This practice is applicable to HC resins as defined inTerminology D 6440. The normal operating temperature rangeis from the cryogenic region to approximately 180C. Thetemperature range can be extended.1.3 The values stated in SI units are to be regarded a
4、sstandard. The values given in parentheses are for informationonly.1.4 Further discussion of glass transition can be found inTest Method D 3418, and Test Method E 1356.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of
5、 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:D 3418 Test Method for Transition Temperatures of Poly-mers by Differential Scanning Calorimetry2D 6440 T
6、erminology Relating to Hydrocarbon Resins3E 473 Terminology Relating to Thermal Analysis4E 1356 Test Method for Glass Transition Temperatures byDifferential Scanning Calorimetry or Differential ThermalAnalysis43. Terminology3.1 Definitions:3.1.1 differential scanning calorimetry (DSC) A tech-nique i
7、n which the difference in energy inputs into a substanceand a reference material is measured as a function of tempera-ture, while the substance and reference material are subjectedto a controlled temperature program.3.1.1.1 DiscussionThe record is the DSC curve. Twomodes, power-compensation DSC and
8、heat-flux DSC, can bedistinguished, depending on the method of measurement used.3.2 For other definitions of terms relating to thermal analy-sis, see Terminology E 473.4. Summary of Practice4.1 This practice consists of heating or cooling the testmaterial at a controlled rate, in a controlled atmosp
9、here, andcontinuously monitoring with a suitable sensing device, thedifference in heat input between a reference material and a testmaterial due to energy changes in the material. Absorption orrelease of energy marks a transition in the specimen resultingin a corresponding baseline shift in the heat
10、ing or coolingcurve.5. Significance and Use5.1 Thermal analysis provides a rapid method for determin-ing transition temperatures in HC resins that possess them.5.2 This practice is useful for both quality assurance andresearch.6. Apparatus6.1 Differential Scanning Calorimeter An instrument ca-pable
11、of heating or cooling at rates up to 20 6 1C/minute andautomatically recording the difference in input between thesample and a reference material to the required sensitivity andprecision.6.2 Sample Tubes or PansBorosilicate glass tubes areused for certain applications and aluminum or other metal pan
12、sof high thermal conductivity for other applications.6.3 Reference Material Glass beads, indium, alumina,silicon carbide, or mercury in a hermetically sealed samplepan, or a material known to be unaffected by repeated heatingand cooling and free from interfering transitions may be used.The thermal d
13、iffusivity should be as close as possible to that ofthe sample.1This practice is under the jurisdiction of ASTM Committee D01 on Paint andRelated Coatings, Materials, and Applications and is the direct responsibility ofSubcommittee D01.38 on Hydrocarbon Resins.Current edition approved Nov. 10, 2000.
14、 Published January 2001.2Annual Book of ASTM Standards, Vol 08.02.3Annual Book of ASTM Standards, Vol 06.03.4Annual Book of ASTM Standards, Vol 14.02.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.D66040026.4 Recording Charts or Sof
15、tware Temperature recordingapparatus with suitable graduations for measurement of eithertemperature differential or energy differential versus tempera-ture or time.7. Reagents7.1 NitrogenInert gas for blanketing sample during test-ing.7.2 Indium, (99.999 + % purity).7.3 Mercury, (99.996 + % purity).
16、7.4 Reagent Grade Benzoic Acid.8. Calibration8.1 Using the same heating rate to be used for samples,calibrate the temperature scale of the apparatus with appropri-ate standard reference materials covering the temperature rangeof interest. For many commercial resins, the following sub-stances cover t
17、his range:Standards Melting Point, CBenzoic acid 122.4Indium 156.6 6 0.4Mercury 38.9 6 0.49. Sample Preparation9.1 Powdered or Granular Samples Avoid grinding ifpreliminary thermal cycle is not performed. (Grinding orsimilar techniques for size reduction often introduce thermaleffects because of fri
18、ction or orientation, or both, and therebychange the thermal history of the sample.)10. Procedure10.1 Use a sample weight appropriate for the material to betested and the instrument used. In most cases, 10 to 20-mgsample weight is satisfactory.NOTE 1Since milligram quantities of sample are used, it
19、is essentialto ensure that samples are homogenous and representative. Also, particlesize has an effect on the detected transition temperatures. Thereforeparticle size should be fairly consistent from sample to sample.10.2 Perform and record a preliminary thermal cycle up to atemperature high enough
20、to erase previous thermal and strainhistory, at a heating rate of 10C/min.NOTE 2Use an inert gas purge such as nitrogen since the sample mayreact with oxygen during the temperature cycle causing an incorrecttransition.NOTE 3An increase or decrease in heating rate from those specifiedmay alter the re
21、sults.10.3 Hold this temperature for 10 min.10.4 Quench cool to 50C below the expected transitiontemperature of interest.10.5 Hold this temperature for 10 min.10.6 Repeat heating on the same sample at a rate of10C/min. and record the heating curve until all desiredtransitions have been completed.11.
22、 Calculation11.1 Measure corrected temperatures Tf, Te, Tm(see Fig. 1)as follows:where:Tf= extrapolated onset temperature C,Te= extrapolated end temperature C, andTm= midpoint temperature C.NOTE 4A new baseline will probably be established after the transi-tion. Tgcan be defined as any of these meas
23、ured values.12. Report12.1 Report the following information:12.1.1 Complete identification and description of the mate-rial tested,12.1.2 Description of the instrument used for the test,12.1.3 Statement of the dimensions, geometry, and materialsof the sample holder; and the average rate of linear te
24、mperaturerange,12.1.4 Description of the temperature calibration procedure,and12.1.5 State the type of Tgvalues reported.13. Keywords13.1 DSC; glass transition temperature; hydrocarbon resin;TgASTM International takes no position respecting the validity of any patent rights asserted in connection wi
25、th any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible tech
26、nical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your comments will receive careful considerat
27、ion at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Ha
28、rbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D6604003
