1、Designation: D6604 00 (Reapproved 2013)Standard Practice forGlass Transition Temperatures of Hydrocarbon Resins byDifferential Scanning Calorimetry1This standard is issued under the fixed designation D6604; the number immediately following the designation indicates the year oforiginal adoption or, i
2、n 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.1. Scope1.1 This practice covers determination of glass transitiontemperatures of hydrocarbon
3、(HC) resins by differential scan-ning calorimetry (DSC).1.2 This practice is applicable to HC resins as defined inTerminology D6640. 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
4、 be regarded asstandard. No other units of measurement are included in thisstandard.1.4 Further discussion of glass transition can be found inTest Method D3418, and Test Method E1356.1.5 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is there
5、sponsibility 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:2D3418 Test Method for Transition Temperatures and En-thalpies of Fusion and Crystallizati
6、on of Polymers byDifferential Scanning CalorimetryD6640 Practice for Collection and Handling of Soils Ob-tained in Core Barrel Samplers for Environmental Inves-tigationsE473 Terminology Relating to Thermal Analysis and Rhe-ologyE1356 Test Method for Assignment of the Glass TransitionTemperatures by
7、Differential Scanning Calorimetry3. Terminology3.1 Definitions:3.1.1 differential scanning calorimetry (DSC), nA tech-nique in which the difference in energy inputs into a substanceand a reference material is measured as a function oftemperature, while the substance and reference material aresubject
8、ed to 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 relating to thermalanalysis, see Terminology E473.4. Summary o
9、f 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 material and a testmaterial due to energy changes in the material.
10、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 transition temperatures in HC resins that possess them.5.2 This practice is
11、 useful for both quality assurance andresearch.6. Apparatus6.1 Differential Scanning CalorimeterAn instrument ca-pable 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 andprec
12、ision.6.2 Sample Tubes or PansBorosilicate glass tubes areused for certain applications and aluminum or other metal pansof high thermal conductivity for other applications.6.3 Reference MaterialGlass beads, indium, alumina, sili-con carbide, or mercury in a hermetically sealed sample pan, ora materi
13、al known to be unaffected by repeated heating and1This practice is under the jurisdiction of ASTM Committee D01 on Paint andRelated Coatings, Materials, and Applications and is the direct responsibility ofSubcommittee D01.34 on Pine Chemicals and Hydrocarbon Resins.Current edition approved June 1, 2
14、013. Published June 2013. Originallyapproved in 2000. Last previous edition approved in 2009 as D6604 00 (2009)1.DOI: 10.1520/D6604-00R13.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume
15、information, refer to the standards Document Summary page onthe ASTM website.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1cooling and free from interfering transitions may be used. Thethermal diffusivity should be as close as possi
16、ble 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 during test-ing.7.2 Indium, (9
17、9.999 + % 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 rangeof interest. For many c
18、ommercial resins, the following sub-stances cover this range:Standards Melting Point, CBenzoic acid 122.4Indium 156.6 0.4Mercury 38.9 0.49. Sample Preparation9.1 Powdered or Granular SamplesAvoid grinding ifpreliminary thermal cycle is not performed. (Grinding orsimilar techniques for size reduction
19、 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 weight is satisfactory.NOTE 1Sinc
20、e 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 Perform and record a preliminary
21、 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 3An increase or decrease in hea
22、ting 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 record the heating curve until
23、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 probably be established after thetran
24、sition. 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 Description of the instrument used
25、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; glass transition temperatures;
26、 hydrocarbon res-ins; TgD6604 00 (2013)2FIG. 1 Glass Transition of a Typical Hydrocarbon ResinD6604 00 (2013)3ASTM 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
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29、u 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 Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual
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