ASTM_E_1867_-_13.pdf

Designation:E186713Standard Test Method forTemperature Calibration of Dynamic Mechanical Analyzers1This standard is issued under the fixed designation E1867;the number immediately following the designation indicates the year oforiginal adoption or,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.1.Scope1.1 This test method describes the temperature calibrationof dynamic mechanical analyzers(DMA)from 150C to300C.1.2 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.3 This standard does not purport to address 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.Specific precau-tionary statements are given in Note 7.2.Referenced Documents2.1 ASTM Standards:2E473 Terminology Relating to Thermal Analysis and Rhe-ologyE1142 Terminology Relating to Thermophysical PropertiesE2161 Terminology Relating to Performance Validation inThermal Analysis3.Terminology3.1 Definitions:3.1.1 The technical terms used in this test method aredefined in Terminologies E473,E1142,and E2161,includingdynamic mechanical analysis,frequency,stress,strain andstorage modulus.4.Summary of Test Method4.1 An equation is developed for the linear correlation ofexperimentally observed program or sensor temperature andthe actual melting temperature for known melting referencematerials.This is accomplished by loading melting pointreference materials into a polymer tube,or wrapping them withpolymer tape and subjecting it to a mechanical oscillation ateither fixed or resonant frequency.The extrapolated onset ofmelting is identified by a rapid decrease in the ordinate signal(the apparent storage modulus,stress,inverse strain or probeposition).This onset is used for temperature calibration withtwo melting point reference materials.5.Significance and Use5.1 Dynamic mechanical analyzers monitor changes in theviscoelastic properties of a material as a function of tempera-ture and frequency,providing a means to quantify thesechanges.In most cases,the value to be assigned is thetemperature of the transition(or event)under study.Therefore,the temperature axis(abscissa)of all DMA thermal curvesmust be accurately calibrated by adjusting the apparent tem-perature scale to match the actual temperature over thetemperature range of interest.6.Interferences6.1 An increase or decrease in heating rates or change inpurge gas type or rate from those specified may alter results.6.2 Once the temperature calibration procedure has beenexecuted,the measuring temperature sensor position shall notbe changed,nor shall it be in contact with the specimen orspecimen holder in a way that would impede movement.If thetemperature sensor position is changed or is replaced,then theentire calibration procedure shall be repeated.6.3 Once the temperature calibration has been executed,thegeometry deformation(bending study,versus tensile,and thelike)shall not be changed.If the specimen testing geometrydiffers significantly from that of the calibrants,then thecalibration shall be repeated in the geometry matching that ofspecimen testing.6.4 This method does not apply to calibration for shear orcompressive geometries of deformation.7.Apparatus7.1 The function of the apparatus is to hold a specimen ofuniform dimension so that the specimen acts as the elastic anddissipative element in a mechanically oscillated system.Dy-namic mechanic analyzers typically operate in one of severalmodes as outlined in Table 1.1This test method is under the jurisdiction ofASTM Committee E37 on ThermalMeasurements and is the direct responsibility of Subcommittee E37.10 onFundamental,Statistical and Mechanical Properties.Current edition approved April 1,2013.Published May 2013.Originallyapproved in 1997.Last previous edition approved in 2012 as E1867 12.DOI:10.1520/E1867-13.2For 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 page onthe ASTM website.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 7.1.1 The apparatus shall consist of the following:7.1.1.1 ClampsAclamping arrangement that permits grip-ping of the specimen.This may be accomplished by clampingat both ends(most systems),one end(for example,torsionalpendulum)or neither end(for example,free bending betweenknife edges).7.1.1.2 Device to Apply Oscillatory Stress or StrainAdevice for applying an oscillatory deformation(strain)oroscillatory stress to the specimen.The deformation may beapplied and then released,as in freely vibrating devices,orcont