ASTM_D_5774_-_95_2014.pdf

Designation:D577495(Reapproved 2014)Standard Test Methods forRubberChemical Analysis of Extractables1This standard is issued under the fixed designation D5774;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 These test methods cover the chemical analysis ofextractables from synthetic rubbers and are intended forgeneral use on solid uncompounded styrene-butadiene copoly-mers commonly referred to as SBR.Analysis of other syntheticrubbers is also possible with some of these test methods.Thetest methods and the sections in which they are covered are asfollows:SectionsTotal Extractables4 11Organic Acid12 19Soap20 26Oil27 42NOTE1The nomenclature used in these test methods is in accordancewith Practice D1418.1.2 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-sisD1418 PracticeforRubberandRubberLaticesNomenclatureD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustries3.Reagents3.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society,wheresuch specifications are available.3Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without decreasing the accuracy ofthe determination.TEST METHOD ATOTAL EXTRACTABLES4.Summary of Test Method4.1 Thin,narrow strips of the dried rubber are extractedthree times with 100 cm3of hot solvent for 10,20,and 40-minperiods,respectively.The extracted rubber is then extracted for5 min in 100 cm3of hot acetone to thoroughly remove theextraction solvent and aid drying of the rubber.The extractedrubber is then dried to constant mass.The difference in massbetween the original sample and the extracted sample is thetotal extractables.5.Significance and Use5.1 This procedure is intended to determine the total ex-tractable materials in rubber.It will give the combined amountof rosin and fatty acids,soaps,extender oils,defoamer tars,antioxidants,and other uncombined organic constituents thatare extractable in the solvent used.The rubber hydrocarbon canbe estimated by subtracting the sum of the total extract,thetotal ash,the volatile matter,and carbon black content(forcarbon black masterbatch)from 100.6.Apparatus6.1 Wide-Mouth Flask,400 to 500 cm3.6.2 Hot Plate and Reflux Condenser.NOTE2Extraction apparatus in Fig.1 of Test Methods D297 may beused,but without the extraction siphon cup.6.3 Filter Paper and Wire Gauze.6.4 Weighing Dish or Watch Glass.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 Aug.1,2014.Published November 2014.Originallyapproved in 1995.Last previous edition approved in 2009 as D5774 95(2009).DOI:10.1520/D5774-95R14.2For 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.3Reagent Chemicals,American Chemical Society Specifications,AmericanChemical Society,Washington,DC.For Suggestions on the testing of reagents notlisted by the American Chemical Society,see Annual Standards for LaboratoryChemicals,BDH Ltd.,Poole,Dorset,U.K.,and the United States Pharmacopeiaand National Formulary,U.S.Pharmacopeial Convention,Inc.(USPC),Rockville,MD.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 6.5 Vacuum Oven,capable of maintaining a temperature of105C and a pressure of 3.0 kPa(23 mm Hg)or less.7.Reagents7.1 Solvents:7.1.1 ETA(Ethanol-Toluene-Azeotrope)Prepare by mix-ing 70 volumes of ethyl alcohol and 30 volumes of toluene,refluxing the mixture for 4 h over calcium oxide and distilling.Discard the first and last portions,keeping only that distillatecoming over within a range of 1C.Distilling may be omittedif absolute grain alcohol or anhydrous formula 3A alcohol isused.7.1.2 H-ITM(Hydrous Isopropanol-Toluene Mixture)Prepare by mixing 75 volumes of anhydrous isopropanol with25 volumes of toluene and then mixing 92 volumes of thissolution with 8 volumes of water.7.1.3 Acetone.8.Preparation of Sample8.1 Dry the sample in accordance with the proceduredescribed in