ASTM_D_6854_-_15a.pdf

Designation:D685415aStandard Test Method forSilicaOil Absorption Number(OAN)1This standard is issued under the fixed designation D6854;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 covers the determination of the oilabsorption number(OAN)of silica.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:2D1799 Practice for Carbon BlackSampling PackagedShipmentsD1900 Practice for Carbon BlackSampling Bulk Ship-mentsD2414 Test Method for Carbon BlackOil AbsorptionNumber(OAN)D6738 Test Method for Precipitated SilicaVolatile Con-tentE177 Practice for Use of the Terms Precision and Bias inASTM Test MethodsE691 Practice for Conducting an Interlaboratory Study toDetermine the Precision of a Test Method3.Summary of Test Method3.1 In this test method,oil is added by means of aconstant-rate burette to a sample of silica in the mixer chamberof an absorptometer.As the sample absorbs the oil,the mixturechanges from a free-flowing state to one of a semiplasticagglomeration,with an accompanying increase in viscosity.This increased viscosity is transmitted to the torque-sensingsystem of the absorptometer.The test is stopped when a torquelevel has been reached.Preferably the torque versus volume ofoil is recorded by a penwriter or by a data acquisition systemallowing a reliable determination of the endpoint.The volumeof oil per unit mass of silica is the oil absorption number(OAN).4.Significance and Use4.1 The oil absorption number of a specific silica is relatedto the processing and vulcanizate properties of rubber com-pounds containing the silica.5.Apparatus35.1 Balance,analytical,with a sensitivity of 0.001 g.5.2 Sieve,500 m(U.S.standard No.35),having a diameterof 200 mm(8 in.)and a height of 25 mm(1 in.).5.3 Bottom Receiver Pan.5.4 Oven,gravity-convection type,capable of temperatureregulation within 61C at 105C and temperature uniformitywithin 65C.5.5 Spatula,rubber,100-mm.5.6 Absorptometer,4equipped with a constant-rate burettethat delivers 4 6 0.024 cm3/min.5.7 Desiccator,with silica gel as desiccant.6.Reagents and Standards6.1 Oil:6.1.1 n-Dibutyl Phthalate,5having a density of 1.042 to1.047 mg/m3(g/cm3)at 25C.6.1.2 di-octyl-adipate(DOA),having a density of 0.9255g/cm3at 20C,a refractive index of 1.447 at 20 C,and akinematic viscosity of 10 to 34 mm2/s(cSt)at 40C.6.1.3 Epoxidized fatty acid ester(EFA),meeting the speci-fications listed in Test Method D2414,Annex A4.1This test method is under the jurisdiction of ASTM Committee D11 on Rubberand is the direct responsibility of Subcommittee D11.20 on Compounding Materialsand Procedures.Current edition approved Nov.1,2015.Published December 2015.Originallyapproved in 2003.Last previous edition approved in 2015 as D6854 15.DOI:10.1520/D6854-15A.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.3All apparatus is to be operated and maintained in accordance with themanufacturers directions for optimum performance.4Available from C.W.Brabender Instruments,Inc.,50 E.Wesley St.,Hackensack,NJ 07606,website:,and HITEC Luxembourg,5 rue de lEglise,L-1458 Luxembourg,website:www.hitec.lu.5Technical grade has turned out to be suitable for the test,provided that thedensity is in the specified range.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 6.2 Silica,commercial grade with a nitrogen surface area of175 6 10 m2/g.7.Sampling7.1 Samples shall be taken in accordance with PracticesD1799 and D1900.8.Calibration8.1 Absorptometer6The absorptometer is composed ofcomponents that influence calibration:the dynamometer torquespring or the load cell,the torque-limit or the indicator setpoint,the oil damper(absorptometers Type C,E,and H areequipped with electronic damping),and the mixer-measuringhead.7It is necessary that each of the components be in goodcondition or proper adjustment to achieve acceptable calibra-tion.NOTE1Stainless steel mixing chambers8have been found satisfactoryfor this test when they are manufactured to a roughness average(Ra)of2.5 6 0.4 m(100 6 15 in.)based upon eight measurements.No singlemeasurement should be greater than 3.6 m(140 in.)or less than 1.5 m(60 in.).Stainless steel