ASTM_E_2890_-_12e1.pdf

Designation:E2890121Standard Test Method forKinetic Parameters for Thermally Unstable Materials byDifferential Scanning Calorimetry Using the KissingerMethod1This standard is issued under the fixed designation E2890;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.1NOTEResearch report information was editorially added to 14.1 in September 2015.1.Scope1.1 This test method describes the determination of thekinetic parameters of Arrhenius activation energy and pre-exponential factor using the Kissinger variable heating rateiso-conversion method(1,2)2and activation energy andreaction order by the Farjas method(3)for thermally unstablematerials.The test method is applicable to the temperaturerange from 300 to 900 K(27 to 627C).1.2 Both nth order and accelerating reactions are addressedby this method over the range of 0.5 n 4 and 1 p 4where n is the nth order reaction order and p is the Avramireaction order(4).Reaction orders n and p are determined bythe Farjas method(3).1.3 This test method uses the same experimental conditionsas Test Method E698.The Flynn/Wall/Ozawa data treatment ofTest Method E698 may be simultaneously applied to theseexperimental results.1.4 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.5 There is no ISO equivalent to this standard.1.6 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:3E473 Terminology Relating to Thermal Analysis and Rhe-ologyE537 Test Method for The Thermal Stability of Chemicalsby Differential Scanning CalorimetryE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test MethodE698 Test Method for Arrhenius Kinetic Constants forThermally Unstable Materials Using Differential Scan-ning Calorimetry and the Flynn/Wall/Ozawa MethodE967 Test Method for Temperature Calibration of Differen-tial Scanning Calorimeters and Differential Thermal Ana-lyzersE968 Practice for Heat Flow Calibration of DifferentialScanning CalorimetersE1142 Terminology Relating to Thermophysical PropertiesE1231 Practice for Calculation of Hazard Potential Figures-of-Merit for Thermally Unstable MaterialsE1860 Test Method for Elapsed Time Calibration of Ther-mal AnalyzersE1970 Practice for Statistical Treatment of ThermoanalyticalDataE2041 Test Method for Estimating Kinetic Parameters byDifferential Scanning Calorimeter Using the Borchardtand Daniels Method1This 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.Published October 2012.DOI:10.1520/E2890-12E01.2The boldface numbers in parentheses refer to the list of references at the end ofthis standard.3For 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 E2161 Terminology Relating to Performance Validation inThermal Analysis and Rheology3.Terminology3.1 Technical terms used in this test method are defined inTerminologies E473,E1142,and E2161.Referenced termsinclude Arrhenius equation,baseline,calibration,Celsius,dif-ferential scanning calorimeter,endotherm,enthalpy,figure-of-merit,first-deviation-frombaseline,full-width-at-half-maximum,Kelvin,onset point,peak,peak value,relativestandard deviation,standard deviation,thermal analysis andthermal curve.4.Summary of Test Method4.1 A series of test specimens are heated at a minimum offour different linear rates in a differential scanning calorimeterthrough a region of exothermic reaction behavior.The rate ofheat evolution,created by a chemical reaction,is proportionalto the rate of reaction and is measured as a function oftemperature and time.4.2 The temperature corresponding to the maximum rate ofreaction(measured at the heat flow maximum of the exother-mic reaction peak)is recorded at each linear heating rate.Thisobserved temperature is corrected for instrument thermalresistance.Activation energy and pre-exponential factor arederived from the linear regression of the natural logarithm ofthe heating rate,normalized to the square of the absolutetemperature,versus the reciprocal absolute temperature of heatflow at the peak maximum.The approach is known as theKissinger m