ASTM_D_6370_-_99_2014.pdf

Designation:D637099(Reapproved 2014)Standard Test Method forRubberCompositional Analysis by Thermogravimetry(TGA)1This standard is issued under the fixed designation D6370;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 test method provides a thermogravimetric(TGA)technique to determine the amounts of organics(oil,polymer),carbon black and ash(filler)in a rubber compound.1.2 The amount of plasticizer/oil may be determined sepa-rately using Test Method D297.1.3 This test method utilizes previously calibrated,manualor computer assisted TGA instrumentation.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 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:2D297 Test Methods for Rubber ProductsChemical Analy-sisD1566 Terminology Relating to RubberD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustriesD6085 PracticeforSamplinginRubberTestingTerminology and Basic ConceptsE473 Terminology Relating to Thermal Analysis and Rhe-ologyE1953 Practice for Description of Thermal Analysis andRheology Apparatus3.Terminology3.1 Definitions:3.1.1 The definitions relating to rubber appearing in Termi-nology D1566 shall be considered applicable to this testmethod.3.1.2 The terminology relating to sampling appearing inPractice D6085 shall be considered applicable to this testmethod.3.1.3 The definitions for thermal analysis appearing inTerminology E473 shall be considered applicable to this testmethod.3.1.4 The description of thermal analysis equipment appear-ing in Practice E1953 shall be considered applicable to this testmethod.3.2 Definitions of Terms Specific to This Standard:3.2.1 ash,nnonvolatile additives(fillers),such as zincoxide,talc,etc.3.2.2 carbon black,ncarbon black.3.2.3 organics,nrubber(polymer),noncarbon black or-ganic additives,such as oil,plasticizer,antioxidants,etc.4.Summary of Test Method4.1 The mass of the rubber test sample,heated at acontrolled,specified rate in a controlled,specified environmentis recorded as a function of temperature.The mass loss over thespecified temperature range provides a compositional analysisof the sample.5.Significance and Use5.1 This test method is intended for use in quality control,material screening,and related problem solving where acompositional analysis,or comparison to a known material,isdesired.5.2 The parameters described are guidelines and may bealtered to suit the analysis of other rubber compounds.5.3 This test method is not suitable for rubber compoundscontaining filler materials which decompose in the temperaturerange of 50 to 800C,for example,CaCO3,Al(OH)3(3H2O),etc.Analysis of compounds containing fillers of this typerequires knowledge of the filler type and some correction formass loss.1This test method is under the jurisdiction of ASTM Committee D11 on Rubberand is the direct responsibility of Subcommittee D11.11 on Chemical Analysis.Current edition approved Aug.1,2014.Published November 2014.Originallyapproved in 1999.Last previous edition approved in 2009 as D6370 99(2009).DOI:10.1520/D6370-99R14.2For 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 6.Apparatus6.1 Thermogravimetric AnalyzerA system of related in-struments that are capable of continuously weighing a testsample,at a sensitivity of 62 g,and recording the change inmass of the test sample under atmospheric control over aspecified temperature range.7.Reagents and Materials7.1 An inert compressed gas,such as argon or nitrogen,anda reactive gas,such as air or oxygen.7.2 Compressed gases must be 99.99%minimum purity.7.3 The inert purge gas must not contain more than 10 g/goxygen.8.Calibration8.1 Calibrate the apparatus,according to the prescribedprocedures or appropriate operating manual,at the heat(tem-perature)and purge gas flow rates to be used.9.Procedure9.1 Place a small piece,10 to 12 mg,of the rubber testsample into the platinum pan of the calibrated Thermogravi-metric Analyzer(TGA).9.2 Apply a 75 cm3/min,or the manufacturers recom-mended flow,argon or nitrogen purge.9.3 Heat to 50C and allow the instrument to equilibrate fora minimum of 2 min.9.4 Hea