1、Designation:D660400(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,in the
2、 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(HC)resins b
3、y 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 be regarded ass
4、tandard.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 theresponsibility of the u
5、ser 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 Crystallization of Polymers byDiffe
6、rential 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 Differential Scanning
7、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 aresubjected to a controlled tempera
8、ture 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 of Practice4.1 This practice cons
9、ists 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.Absorption orrelease of energy marks
10、 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 useful for both quality assurance an
11、dresearch.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 andprecision.6.2 Sample Tubes or PansBorosili
12、cate 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 material known to be unaffected by repeated heati
13、ng 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 1,2013.Published June 2013.Originallyapproved in
14、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 information,refer to the standards Document Summary pag
15、e onthe ASTM website.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 cooling and free from interfering transitions may be used.Thethermal diffusivity should be as close as possible to that of thesample.6.4 Recording Charts or SoftwareTemp
16、erature 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).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
