ASTM_D_3677_-_10_2015.pdf

Designation:D367710(Reapproved 2015)Standard Test Methods forRubberIdentification by Infrared Spectrophotometry1This standard is issued under the fixed designation D3677;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.This standard has been approved for use by agencies of the U.S.Department of Defense.1.Scope1.1 These test methods cover rubber identification and arebased on infrared examination of pyrolysis products(pyrolyz-ates)and films.1.2 These test methods are applicable to rubbers in the rawstate and,when compounded,both in the cured and uncuredstate.1.3 Since it is customary in infrared spectrophotometry touse wavenumbers(cm1)rather than Hertz(Hz),the unit forfrequency in the SI system,the former is employed throughoutthis test method.1.4 This test method assumes that specimens and infraredspectra are prepared and analyzed by experienced personneland that the equipment is operated according to the manufac-turers direction for optimum performance.No details foroperation of infrared spectrophotometers are included in thistest 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.Specific precau-tionary statements are given in Section 17.2.Referenced Documents2.1 ASTM Standards:2D297 Test Methods for Rubber ProductsChemical Analy-sisD1418 PracticeforRubberandRubberLaticesNomenclatureD3452 Practice for RubberIdentification by Pyrolysis-GasChromatographyE168 Practices for General Techniques of Infrared Quanti-tative Analysis(Withdrawn 2015)33.Significance and Use3.1 For research,development,and quality controlpurposes,it is advantageous to determine the composition ofrubbers in cured,compounded products.3.2 This test method provides such composition analysisutilizing an infrared technique.4.Reagents4.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.4Other grades may beused,provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.4.2 Acetone.4.3 Alcohol,ethanol,denatured.4.4 2-Butanone.4.5 Chloroform.4.6 Congo Red Paper.4.7 Diatomaceous Filter AidSome grades are quite unsat-isfactory in that they will not sufficiently absorb carbon black.4.8 1,2-DichlorobenzeneA check on suitability may bemade by evaporating 50 cm3to dryness and making an infraredspectrum of the residue.Any substantial absorbance at posi-tions near those wavenumbers that will be used for rubberanalysis,indicates that the 1,2-dichlorobenzene is unsuitablefor use.1These test methods are under the jurisdiction of ASTM Committee D11 onRubber and are the direct responsibility of Subcommittee D11.11 on ChemicalAnalysis.Current edition approved June 1,2015.Published September 2015.Originallyapproved in 1978.Last previous edition approved in 2010 as D3677 101.DOI:10.1520/D3677-10R15.2For 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.3The last approved version of this historical standard is referenced onwww.astm.org.4Reagent Chemicals,American Chemical Society Specifications,AmericanChemical Society,Washington,DC.For suggestions on the testing of reagents notlisted by the American Chemical Society,see Analar Standards for LaboratoryChemicals,BDH Ltd.,Poole,Dorset,U.K.,and the United States Pharmacopeiaand National Formulary,U.S.Pharmaceutical Convention,Inc.(USPC),Rockville,MD.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 4.9 Dry Compressed Air and Nitrogen,in cylinders,orprovided as a laboratory service.4.10 Sodium Sulfate,anhydrous.4.11 Toluene.TEST METHOD A QUALITATIVE ANALYSIS5.Scope5.1 This test method,based on infrared examination ofpyrolysis products(pyrolyzates)and films,will identify therubbers in 6.1 occurring alone or in binary blends in the rangefrom 80%major component to 20%minor component.Exceptions to this will be found in 6.2.5.2 This test method is applicable to rubbers in the raw stateand,when compounded,both in the cured and uncured state.5.3 This test method implies that sample preparation andinfrared spectrum are prepared and analyzed by experiencedpersonnel and that the equipment used for the produ