1、Designation:E206906(Reapproved 2012)Standard Test Method forTemperature Calibration on Cooling of Differential ScanningCalorimeters1This standard is issued under the fixed designation E2069;the number immediately following the designation indicates the year oforiginal adoption or,in the case of revi
2、sion,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 covers the temperature calibration ofdifferential scanning calorimeters on cooling using
3、the differ-ence between transition temperatures upon heating and coolingin the temperature range of 50 to 185C.An offset in theindicatedtemperaturebetweenheatingandcoolingexperiments,within this temperature range,may be used toprovide temperature calibration on cooling at other temperatureranges.1.2
4、 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-priat
5、e safety and health practices and determine the applica-bility of regulatory limitations prior to use.Specific precau-tionary statements are given in Section 6.2.Referenced Documents2.1 ASTM Standards:2D3418 Test Method for Transition Temperatures and En-thalpies of Fusion and Crystallization of Pol
6、ymers byDifferential Scanning CalorimetryE473 Terminology Relating to Thermal Analysis and Rhe-ologyE794 Test Method for MeltingAnd Crystallization Tempera-tures By Thermal AnalysisE928 Test Method for Purity by Differential Scanning Calo-rimetryE967 Test Method for Temperature Calibration of Differ
7、en-tial Scanning Calorimeters and Differential Thermal Ana-lyzersE1970 Practice for Statistical Treatment of ThermoanalyticalData3.Terminology3.1 Specific technical terms used in this test method aredefined in Terminology E473.4.Summary of Test Method4.1 The temperature sensor of the DSC,used to det
8、erminethe temperature of a transition,is located close to but externalto the test specimen.This arrangement causes the indicatedtemperature to lead or lag the actual specimen temperature onheating/cooling causing the reported temperature to be higheron heating and lower on cooling than the actual sp
9、ecimentransition temperature.A DSC apparatus temperature,that hasbeen calibrated for heating experiments,needs to be re-calibrated for cooling experiments.Such a calibration oncooling is performed using a liquid crystal material,thetransition(s)for which are not subject to super-heating orsuper-cool
10、ing.4.2 The transition temperature of a rapid,non-superheatingand non-supercooling transition is determined upon heatingand upon cooling.The difference between these two indicatedtemperatures provides an offset temperature value betweenheating and cooling experiments at the indicated rate.Thisoffset
11、 temperature value,when used with a precise temperaturecalibration upon heating,may serve as an instrument calibra-tion function upon cooling.5.Significance and Use5.1 This test method is useful in calibrating the temperaturesignal of a differential scanning calorimeter for cooling experi-ments such
12、 as the determination of crystallization temperaturesin Test Method D3418 and Test Method E794.5.2 Thistestmethodmaybeusedforresearch,development,analytical,specification acceptance,quality as-surance and control purposes.6.Precautions6.1 Toxic or corrosive effluents,or both,may be releasedwhen heat
13、ing the material of this test method and may beharmful to personnel and to the apparatus.1This test method is under the jurisdiction ofASTM Committee E37 on ThermalMeasurements and is the direct responsibility of Subcommittee E37.01 on Calo-rimetry and Mass Loss.Current edition approved Sept.1,2012.
14、Published September 2012.Originallyapproved in 2000.Last previous edition approved in 2006 as E2069 06.DOI:10.1520/E2069-06R12.2For referenced ASTM standards,visit the ASTM website,www.astm.org,orcontact ASTM Customer Service at serviceastm.org.For Annual Book of ASTMStandards volume information,ref
15、er 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.Apparatus7.1 Differential Scanning Calorimeter(DSC)The essentialinstrumentation required providing the minimum differentialscan
16、ning calorimeter capability for this test method includes:7.1.1 A DSC Test Chamber,composed of:7.1.1.1 A Furnace(s),to provide uniform controlled heatingand cooling of a specimen and reference material to a constanttemperature or at a constant rate within the applicable tempera-ture range of this method.7.1.1.2 A Temperature Sensor,that indicates specimen orfurnace temperature to 60.01 C.7.1.1.3 A Differential Sensor,to detect a heat flow difference(DSC)between the specimen and reference with a