ASTM_E_1363_-_16.pdf

Designation:E136316Standard Test Method forTemperature Calibration of Thermomechanical Analyzers1This standard is issued under the fixed designation E1363;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.Scope*1.1 This test method describes the temperature calibrationof thermomechanical analyzers from 50 to 1500C.(See Note1.)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 is similar to ISO 113591 but addresses alarger temperature range and utilizes additional calibrationmaterials.1.4 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 Section 7 and Note 11.2.Referenced Documents2.1 ASTM Standards:2E473 Terminology Relating to Thermal Analysis and Rhe-ology2.2 Other Standards:3ISO 113591 Thermomechanical Analysis(TMA)-Part 1:General Principles3.Terminology3.1 Definitions:3.1.1 The terminology relating to thermal analysis appear-ing in Terminology E473 shall be considered applicable to thisdocument.4.Summary of Test Method4.1 An equation is developed for the linear correlation of theexperimentally observed program temperature and the actualmelting temperature for known melting standards.This isaccomplished through the use of a thermomechanical analyzerwith a penetration probe to obtain the onset temperatures fortwo melting point standards.An alternate,one-point method oftemperature calibration is also given for use over very narrowtemperature ranges.(See Note 2.)NOTE1This test method may be used for calibrating thermomechani-cal analyzers at temperatures outside this range of temperature.However,the accuracy of the calibration will be no better than that of thetemperature standards used.NOTE2It is possible to develop a more elaborate method oftemperature calibration using multiple(more than two)fusion standardsand quadratic regression analysis.Since most modern instruments arecapable of heating rates which are essentially linear in the region of use,the procedure given here is limited to a two-point calibration.5.Significance and Use5.1 Thermomechanical analyzers are employed in theirvarious modes of operation(penetration,expansion,flexure,etc.)to characterize a wide range of materials.In most cases,the value to be assigned in thermomechanical measurements isthe temperature of the transition(or event)under study.Therefore,the temperature axis(abscissa)of all TMA thermalcurves must be accurately calibrated either by direct reading ofa temperature sensor or by adjusting the programmer tempera-ture to match the actual temperature over the temperature rangeof interest.6.Apparatus6.1 Thermomechanical Analyzer(TMA),The essential in-strumentation required to provide the minimum thermome-chanical analytical or thermodilatometric capability for thismethod includes:6.1.1 A Rigid Specimen Holder or Platform,of inert,lowexpansivity material(1 m m-1K-1)to center the specimen inthe furnace and to fix the specimen to mechanical ground.6.1.2 A Rigid(expansion compression,flexure,tensile,etc.)Probe,of inert,low expansivity material(1 m m-1K-1)thatcontacts with the specimen with an applied compressive ortensile force.For this test method,the use of a penetrationprobe is recommended.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 Dec.1,2016.Published January 2017.Originallyapproved in 1990.Last previous edition approved in 2013 as E1363 13.DOI:10.1520/E1363-16.2For 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.3Available from American National Standards Institute(ANSI),25 W.43rd St.,4th Floor,New York,NY 10036,http:/www.ansi.org.*A Summary of Changes section appears at the end of this standardCopyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade(TBT)Committee.1 6.1.3 A Sensing Element,linear over a minimum range of2 mm to measure