ASTM_E_2105_-_00_2010.pdf

Designation:E210500(Reapproved 2010)Standard Practice forGeneral Techniques of Thermogravimetric Analysis(TGA)Coupled With Infrared Analysis(TGA/IR)1This standard is issued under the fixed designation E2105;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 practice covers techniques that are of general use inthe qualitative analysis of samples by thermogravimetric analy-sis(TGA)coupled with infrared(IR)spectrometric techniques.The combination of these techniques is often referred to asTGA/IR.1.2 A sample heated in a TGA furnace using a predeter-mined temperature profile typically undergoes one or moreweight losses.Materials evolved during these weight losses arethen analyzed using infrared spectroscopy to determine chemi-cal identity.The analysis may involve collecting discreteevolved gas samples or,more commonly,may involve passingthe evolved gas through a heated flowcell during the TGAexperiment.The general techniques of TGA/IR and othercorresponding techniques,such as TGA coupled with massspectroscopy(TGA/MS),as well as,TGA,used in conjunctionwith GC/IR,are described in the referenced literature(1-4).21.3 Some thermal analysis instruments are designed toperform both thermogravimetric analysis and differential scan-ning calorimetry simultaneously.This type of instrument issometimes called a simultaneous thermal analyzer(STA).Theevolved gas analysis performed with an STA instrument(5)issimilar to that with a TGA,and so,would be covered by thispractice.With use of a simultaneous thermal analyzer,thecoupled method typically is labeled STA/IR.1.4 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.5 This statement 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:3E131 Terminology Relating to Molecular SpectroscopyE168 Practices for General Techniques of Infrared Quanti-tative AnalysisE334 Practice for General Techniques of Infrared Micro-analysisE473 Terminology Relating to Thermal Analysis and Rhe-ologyE1131 Test Method for Compositional Analysis by Thermo-gravimetryE1252 Practice for General Techniques for Obtaining Infra-red Spectra for Qualitative AnalysisE1421 Practice for Describing and Measuring Performanceof Fourier Transform Mid-Infrared(FT-MIR)Spectrom-eters:Level Zero and Level One Tests3.Terminology3.1 DefinitionsFor general definitions of terms andsymbols,refer to Terminologies E131 and E473.3.2 Definitions of Terms Specific to This Standard:3.2.1 evolved gas,nany material(or mixture)evolvedfrom a sample during a thermogravimetric or simultaneousthermal analysis experiment.Materials evolved from thesample may be in the form of a gas,a vapor,an aerosol or asparticulate matter.For brevity,the term“evolved gas”will beused throughout this practice to indicate any material form ormixture evolved from a sample.3.2.2 evolved gas analysis(EGA),na technique in whichthe nature and amount of gas evolved from a sample ismonitored against time or temperature during a programmedchange in temperature of the sample.3.2.3 evolved gas profile(EGP),nan indication of thetotal amount of gases evolved,as a function of time ortemperature,during the thermogravimetric experiment.InTGA/IR,this profile is calculated from the infrared spectro-scopic data recorded by application of the Gram-Schmidt1This practice is under the jurisdiction of ASTM Committee E13 on MolecularSpectroscopy and Separation Science and is the direct responsibility of Subcom-mittee E13.03 on Infrared and Near Infrared Spectroscopy.Current edition approved March 1,2010.Published May 2010.Originallyapproved in 2000.Last previous edition approved in 2005 as E2105 00(2005).DOI:10.1520/E2105-00R10.2The boldface numbers in parentheses refer to a 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 reconstruction(GSR)algorithm(6,7).Because the GSR wasdesigned for use in gas chromatography coupled with infrared(GC/IR)analysis,the evolved gas profile has sometimes beenerroneously called the evolved gas chromatogram.3.2.4 functional group profile(FGP),nan indication ofthe amount of gas evolved during the thermogravimetricexperiment that contains a particular