1、Designation: D 6604 00 (Reapproved 2009)1Standard 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
2、, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1NOTENote 5 was added editorially in January 2009.1. Scope1.1 This practice covers determin
3、ation of glass transitiontemperatures of hydrocarbon (HC) resins by 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 ca
4、n be extended.1.3 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.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 thesafet
5、y 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.2. Referenced Documents2.1 ASTM Standards:2D 3418 Test Method for Transition
6、 Temperatures and En-thalpies of Fusion and Crystallization of Polymers byDifferential Scanning CalorimetryD 6640 Practice for Collection and Handling of Soils Ob-tained in Core Barrel Samplers for Environmental Inves-tigationsE 473 Terminology Relating to Thermal Analysis and Rhe-ologyE 1356 Test M
7、ethod for Assignment of the Glass TransitionTemperatures by Differential Scanning Calorimetry3. Terminology3.1 Definitions:3.1.1 differential scanning calorimetry (DSC), n A tech-nique in which the difference in energy inputs into a substanceand a reference material is measured as a function of temp
8、era-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 heat-flux DSC, can bedistinguished, depending on the method of measurement used.3.2 For other definitions of terms
9、 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 atmosphere, andcontinuously monitoring with a suitable sensing device, thedifference in heat input between a reference m
10、aterial 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 heating or coolingcurve.5. Significance and Use5.1 Thermal analysis provides a rapid method for determin-ing transitio
11、n 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 of heating or cooling at rates up to 20 6 1C/minute andautomatically recording the difference in input between the
12、sample and a reference material to the required sensitivity andprecision.1This practice is under the jurisdiction of ASTM Committee D01on Paint andRelated Coatings, Materials, and Applications and is the direct responsibility ofSubcommittee D01.38 on Hydrocarbon Resins.Current edition approved Janua
13、ry 15, 2009. Published January 2009. Originallyapproved in 2000. Last previous edition approved in 2000 as D 6604 - 00.2For 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
14、to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.2 Sample Tubes or PansBorosilicate glass tubes areused for certain applications and aluminum or other metal pansof high therm
15、al conductivity for other applications.6.3 Reference MaterialGlass beads, indium, alumina, sili-con carbide, or mercury in a hermetically sealed sample pan, ora material known to be unaffected by repeated heating andcooling and free from interfering transitions may be used. Thethermal diffusivity sh
16、ould be as close as possible to that of thesample.6.4 Recording Charts or SoftwareTemperature 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 durin
17、g test-ing.7.2 Indium, (99.999 + % purity).7.3 Mercury, (99.996 + % purity).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 ran
18、geof interest. For many commercial resins, the following sub-stances cover this 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
19、 techniques for size reduction often introduce thermaleffects because of friction 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 wei
20、ght is satisfactory.NOTE 1Since milligram quantities of sample are used, it 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 Pe
21、rform and record a preliminary thermal cycle up to atemperature high enough 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 3
22、An increase or decrease in heating rate from those specifiedmay alter the results.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 r
23、ecord the heating curve until all desiredtransitions have been completed.11. Calculation11.1 Measure corrected temperatures Tf, TeT, 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 probabl
24、y be established after the transi-tion. Tgcan be defined as any of these measured values.NOTE 5In Fig. 1 the downward direction of the Heat Flow axisindicates an exotherm.12. Report12.1 Report the following information:12.1.1 Complete identification and description of the mate-rial tested,12.1.2 Des
25、cription 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 temperaturerange,12.1.4 Description of the temperature calibration procedure,and12.1.5 State the type of Tgvalues reported.13. Keywords13.1 DSC
26、; glass transition temperature; hydrocarbonresin;TgD 6604 00 (2009)12D 6604 00 (2009)13ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of
27、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 technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Y
28、our 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 consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your commen
29、ts 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 Harbor 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).D 6604 00 (2009)14
