ASTM_E_2402_-_11.pdf

Designation:E240211Standard Test Method forMass Loss and Residue Measurement Validation ofThermogravimetric Analyzers1This standard is issued under the fixed designation E2402;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 method provides procedures for validating massloss and residue measurements by thermogravimetric analyzers(TGA)and analytical methods based upon the measurement ofmass loss or residue content.Performance parameters deter-mined include mass loss and residue repeatability(precision),detection limit,quantitation limit,linearity and bias.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 be regarded asstandard.No other units of measurement are included in thisstandard.1.4 There is no ISO standard equivalent to this method.1.5 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:2E177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE473 Terminology Relating to Thermal Analysis and Rhe-ologyE1142 Terminology Relating to Thermophysical PropertiesE1582 Practice for Calibration of Temperature Scale forThermogravimetryE1970 Practice for Statistical Treatment of ThermoanalyticalDataE2040 Test Method for Mass Scale Calibration of Thermo-gravimetric AnalyzersE2161 Terminology Relating to Performance Validation inThermal Analysis2.2 Other Standard:United States Food and Drug Administration,Q2B Valida-tion of Analytical Procedures:Methodology,62 FR27464,May 19,199733.Terminology3.1 Technical terms used in this standard are defined inPractice E177 and in Terminologies E473,E1142,and E2161.3.2 Definitions of Terms Specific to This Standard:3.2.1 highly volatile mattermaterials(such as moisture,plasticizer,residual solvent,etc.)that boil at temperaturesbelow 200 C.3.2.2 medium volatile mattermaterials(such as oil andpolymer degradation products)that boil in the temperaturerange between 200 and 400 C.3.2.3 residuematerialremaining(suchasmetalcomponents,filler content or inert reinforcing materials)aftermore volatile components are vaporized.3.2.4 mass loss plateaua region of a thermogravimetriccurve with a relatively constant mass(that is,accompanied bya minima in the first derivative of mass with respect to time).4.Summary of Test Method4.1 Mass is the primary dependent parameter and tempera-ture is the primary independent parameter measured by TGA.4.2 Mass loss and residue measurements are validated bytheir direct measurement using thermogravimetric apparatusover a specified temperature range using reference materials ofknown volatiles content as an analyte.4.3 Alternatively,validation of a TGA method based uponmass loss and residue measurements may be performed usinga specific test specimen as the analyte.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 April 1,2011.Published May 2011.Originallyapproved in 2005.Last previous edition approved in 2005 as E2402 05.DOI:10.1520/E2402-11.2For 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 Food and Drug Administration(FDA),10903 New HampshireAve.,Silver Spring,MD 20993-0002,http:/www.fda.gov.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 4.4 The mass loss of three or more specimens(nominallyrepresenting the maximum,midpoint and minimum of therange of the test method)is measured at least in triplicate.Afourth blank specimen,containing no analyte,is also measuredat least 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 measurements.4.4.1 Mass loss and residue linearity and bias are deter-mined from the best-fit straight-line correlation of the resultsfrom measurements of the three or more specimens.4.4.2 Mass loss and residue detection limit and quantitationlimit are determined from the standard deviation of the blankspecimen measurements.4.4.3 Mass loss and residue repeatability are determinedfrom the r