1、Designation:E225311Standard Test Method forTemperature and Enthalpy Measurement Validation ofDifferential Scanning Calorimeters1This standard is issued under the fixed designation E2253;the number immediately following the designation indicates the year oforiginal adoption or,in the case of revision
2、,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 provides procedures for validatingtemperature and enthalpy measurements of differential scan-
3、ning calorimeters(DSC)and analytical methods based uponthe measurement of temperature or enthalpy(or heat),or both,by DSC.Performance parameters determined include tempera-ture and calorimetric repeatability(precision),detection limit,quantitation limit,linearity,and bias.This test method isapplicab
4、le to exothermic events.1.2 Validation of apparatus performance and analyticalmethods is requested or required for quality initiatives or whereresults may be used for legal purposes.1.3 The values stated in SI units are to regarded as standard.No other units of measurement are included in this stand
5、ard.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 D
6、ocuments2.1 ASTM Standards:2E177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE473 Terminology Relating to Thermal Analysis and Rhe-ologyE967 Test Method for Temperature Calibration of Differen-tial Scanning Calorimeters and Differential Thermal Ana-lyzersE968 Practice for Hea
7、t Flow Calibration of DifferentialScanning CalorimetersE1142 Terminology Relating to Thermophysical PropertiesE1860 Test Method for Elapsed Time Calibration of Ther-mal AnalyzersE1970 Practice for Statistical Treatment of ThermoanalyticalDataE2161 Terminology Relating to Performance Validation inThe
8、rmal Analysis2.2 FDA Publications:3Q2B Validation of Analytical Procedures Methodology,62FR 27464,May 19,19973.Terminology3.1 Technical terms used in this standard are defined inPractice E177 and in Terminologies E473,E1142,and E2161including analyte,detection limit,differential scanningcalorimetry,
9、enthalpy,extrapolated onset value(temperature),linearity,mean,precision,quantitation limit,relative standarddeviation,repeatability,standard deviation,thermal curve,andvalidation.4.Summary of Test Method4.1 Temperature and time are the primary independentparameters and heat flow is the primary depen
10、dent experimen-tal parameter provided by DSC.Integration of heat flow,as afunction of time,yields enthalpy(heat).4.1.1 Time,measured by the DSC apparatus,shall conformto better than 0.1%verified by Test Method E1860 andreported.4.1.2 Temperature is directly measured by a temperaturesensor that is an
11、 integral part of the differential scanningcalorimetry apparatus.4.1.3 Heat flow,a measured value,is validated by itsintegration over time to obtain the desired calorimetric(en-thalpic)information of interest.4.2 Calorimetric validation of a differential scanning calo-rimetric apparatus at a single
12、temperature is performed usingthe indium metal melt as an analyte.4.3 Validation of a DSC method based upon enthalpicmeasurement may be performed using the test specimen as theanalyte.1This test method is under the jurisdiction ofASTM Committee E37 on ThermalMeasurements and is the direct responsibi
13、lity of Subcommittee E37.10 onFundamental,Statistical and Mechanical Properties.Current edition approved Dec.1,2011.Published February 2012.Originallyapproved in 2003.Last previous edition approved in 2008 as E2253 081.DOI:10.1520/E2253-11.2For referenced ASTM standards,visit the ASTM website,www.as
14、tm.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 Food and Drug Administration(FDA),10903 New HampshireAve.,Silver Spring,MD 20993-0002,http:/www.fda.gov.Copyri
15、ght ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 4.4 The enthalpy of three(or more)specimens(nominallyrepresenting the maximum,midpoint and minimum of therange of the test method)are measured in triplicate(or more).A fourth blank specimen,contai
16、ning no analyte,is alsomeasured in triplicate.NOTE1Repeatability is determined by performing a sufficient numberof determinations to calculate statistically valid estimates of the standarddeviation or relative standard deviation of the measurement.4.4.1 Calorimetric linearity and bias are determined fromthe best-fit straight-line correlation of the results from mea-surements of the three(or more)specimens.4.4.2 Calorimetric detection limit and quantitation limit aredetermined from the standard d
