ASTM_D_5805_-_00_2014.pdf

Designation:D580500(Reapproved 2014)Standard Test Methods forRubberDetermination of Carbon Black in Masterbatches1This standard is issued under the fixed designation D5805;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 determination of theamount of carbon black in a masterbatch and cover emulsionSBR-carbon black mixtures,but may be applicable to otherpolymers.Three test methods are included:SectionsInert Atmosphere Pyrolysis3 10Vacuum Pyrolysis11 17Thermogravimetric Analyzer18 24NOTE1The nomenclature used in these test methods is in accordancewith Practice D1418.1.2 The values stated in SI units are to be regarded as thestandard.The values given in parentheses are for informationonly.1.3 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:2D1418 PracticeforRubberandRubberLaticesNomenclatureD6370 Test Method for RubberCompositional Analysisby Thermogravimetry(TGA)TEST METHOD ACARBON BLACKInert Atmosphere Pyrolysis Test Method3.Summary of Test Method3.1 The prepared dried sample and a sample of standardSBR black determinate are tested in triplicate.The samples areweighed accurately into tared crucibles and then placed in acombustion tube at 550C,which is continuously flushed withCO2until the rubber hydrocarbon is distilled.The crucibles andcontents are cooled in a desiccator,weighed,then inserted intoa muffle furnace at 550C until all carbonaceous material isburned.The crucible and contents are again cooled in adesiccator and weighed.The percentage of carbon black iscalculated from the weights.4.Significance and Use4.1 The carbon black content of an unvulcanized black oroil-black SBR masterbatch may be determined by this testmethod if an inert(CO2)atmosphere and a determinate(seeNote 2)of known carbon black content are available.NOTE2Determinate black masterbatch may be prepared by carefuladdition of exact amounts of rubber and carbon black on a mill.Analternative would be a thorough blending of a quantity of black master-batch and determination of the carbon black by use of a previouslyestablished determinate.5.Apparatus5.1 Drying Oven.5.2 Porcelain Crucibles,No.00000,tared.5.3 Weighing Bottles,tared.5.4 Fused Alumina Combustion Boats.35.5 Combustion Tubes.45.6 Combustion Furnace.6.Reagents6.1 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,where1These 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 D5805 00(2009).DOI:10.1520/D5805-00R14.2For 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.3Alundum No.3 combustion boats have been found satisfactory for this purpose.4The sole source of supply of the combustion tube known to the committee atthis time is the McDaniel high-temperature combustion tube,30 in.(762 mm)longby 1 in.(25.4 mm)in diameter available from Dunlap and Co.,623 Staring Lane,Baton Rouge,LA 70810.This tube will accommodate a maximum of twocombustion boats containing six samples each within the heated area of the furnace.If you are aware of alternative suppliers,please provide this information to ASTMInternational Headquarters.Your comments will receive careful consideration at ameeting of the responsible technical committee,1which you may attend.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 such specifications are available.5Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.7.Preparation of Sample7.1 Blend 200 g of dried sample obtained in accordancewith 4.1 or 9.1 by passing it five times between the rolls of alaboratory mill.Maintain the roll temperature at 50 6 5C(1226 9F)and a distance between the rolls of 0.5 6 0.13 mm(0.020 6 0.005 in.).After blending,sheet the sample from themill with the distance between the rolls set at 0.25 6 0.05 mm(0.010 6 0.002 in.).Dry approximately 2 g of th