ASTM_E_2509_-_14.pdf

Designation:E250914Standard Test Method forTemperature Calibration of Rheometers in Isothermal Mode1This standard is issued under the fixed designation E2509;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 calibrationor conformance of rheometers.The applicable temperaturerange is 0 to 80C however other ranges may be selected forthe purpose at hand.1.2 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.3 There are no ISO equivalents to this standard.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.2.Referenced Documents2.1 ASTM Standards:2E473 Terminology Relating to Thermal Analysis and Rhe-ologyE1142 Terminology Relating to Thermophysical Properties3.Terminology3.1 DefinitionsSpecific technical terms found in this stan-dard are defined in Terminologies E473 and E1142,includingrheometer and rheometry.4.Summary of Test Method4.1 An electronic thermometer of known characteristics isplaced in the center of a dummy test specimen in contact withthe torque applying instrument plates of a rheometer atconstant(isothermal)temperature.The difference between therheometer set temperature and that indicated by the thermom-eter is used to calibrate the rheometer temperature signal.5.Significance and Use5.1 Rheological properties such as viscosity and storage andloss modulus change rapidly with temperature.High qualitydeterminations of these properties depend upon a stable andwell-known temperature of the measuring apparatus.6.Interferences6.1 In many rheological experiments,temperature is variedwith time.The calibration in this test method is made understable and isothermal temperature conditions.Thus the effectsof changes in temperature with time are not addressed.Thisisothermal calibration does not provide any information aboutthe specimen under temperature scanning conditions.7.Apparatus7.1 An electronic thermometer that includes:7.1.1 Temperature sensor,(such as a thermocouple,plati-num resistance thermometer,thermistor,etc.)with an accuracy(traceable to a known absolute standard)and resolution of60.1C and a range of 0 to 80C.NOTE1Sensors with other temperature ranges may be used at theoperators convenience.NOTE2Some sensors are available already affixed with dummy testspecimens from section 7.27.1.2 Temperature indicator,to convert the signal presentedby the temperature sensor into a digital electronic temperaturedisplay with the accuracy and precision indicated in section7.1.1.7.2 Dummy test specimen,two polymer sheets each 1 mm inthickness of such a diameter to fill the space(that is,gap)between the instrument plates.NOTE3The dummy test specimen may be composed of the materialto be tested or some other representative polymer material.Polydimeth-ylsiloxane(PDMS)(for example,“Silly Putty”3)may be used for thispurpose.NOTE4Polydimethylsiloxane may leave a residue of silicone oil onthe surfaces of the instrument plates.This oil should be removed prior tosubsequent use.7.3 Rheometer,the essential instrumentation required pro-viding the minimum rheological analytical capabilities for thistest method include:1This test method is under the jurisdiction ofASTM Committee E37 on ThermalMeasurements and is the direct responsibility of Subcommittee E37.08 on Rheol-ogy.Current edition approved Aug.1,2014.Published August 2014.Originallyapproved in 2008.Last previous edition approved in 2008 as E2509 08.DOI:10.1520/E2509-14.2For 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.3The trademark Silly Putty is registered to Crayola Properties,inc.,Easton,PA,18042.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 7.3.1 A drive actuator,to apply torque or displacement tothe specimen in a periodic manner capable of frequencies ofoscillation from 0.01 to 10 rad/s(0.0016 to 1.6 Hz).Thisactuator may also be capable of providing static force ortransient step or displacement of the test specimen.7.3.2 Acoupling shaft,or other means to transmit the torqueor displacement from the actuator to the specimen.7.3.3 A geometry,tools or plates,to fix the specimenbetween the coupling shaft and a stationary position.For thepurposes of this test,parallel plates are the preferred configu-ration7.3.4 Either a torque sensor,to me