ASTM_D_4527_-_99_2011.pdf

Designation:D452799(Reapproved 2011)Standard Test Method forCarbon BlackSolvent Extractables1This standard is issued under the fixed designation D4527;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 procedure for measuringcarbon black solvent extractables.1.1.1 This test method determines the total material ex-tracted from carbon black by toluene under specified condi-tions.The procedure is also applicable to other solvents such ascyclohexane,etc.1.2 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.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.For a specificprecautionary statement,see Section 7.2.Referenced Documents2.1 ASTM Standards:2D3051 Practice for Carbon BlackStating the Precision ofASTM Test Methods(Withdrawn 1990)3D3396 Practice for Carbon Black Measuring the Precisionof ASTM Test Methods(Withdrawn 1990)33.Summary of Test Method3.1 A specimen of carbon black is extracted for 48 h(orother specified time)in a Soxhlet extractor,the solvent re-moved by controlled temperature evaporation,and the ex-tracted residue determined gravimetrically.If the carbon blackextractables are to be subjected to additional analysis,seeSection 7.4.Significance and Use4.1 The carbon black extract test procedure provides auniform and precise method for the gravimetric determinationof organic-solvent extractables on carbon black.Accuracy andprecision are acceptable for most specification or regulatorypurposes,or both.However,carbon black with very low extract(less than 0.02%)may require a more rigorous extractionprocedure.The actual chemical composition of the extract canvary significantly with the type and origin of the carbon black.5.Apparatus5.1 Soxhlet Extraction Apparatus,with interchangeableground joints,40 mm I.D.extraction tube,and 250-cm3flask.45.2 Extraction Thimble,glass,35-mm diameter by 90-mmheight,with coarse porosity fritted disc.5When filled with 50cm3of toluene,drainage time for the first 40 cm3should notexceed 95 s.Discard thimbles taking longer.5.3 Heater,for extraction flask,with adjustable heat input.Ahot plate extraction heater or hemispherical heating mantle ispreferred.5.4 Filter Funnel,glass fritted disc type,with mediumporosity fritted disc.5.5 Filter Flask,125 or 250 cm3.5.6 Water Bath,or other suitable warming means for evapo-rating solvent from extract at a controlled temperature of 40 to50C.5.7 Container,suitable for final solvent removal and weigh-ing of residue.A lightweight aluminum dish 63 by 17.5 mm,aTFE-fluorocarbon cup or a 50-cm3glass beaker is suggested.61This test method is under the jurisdiction of ASTM Committee D24 on CarbonBlack and is the direct responsibility of Subcommittee D24.31 on Non-CarbonBlack Components of Carbon Black.Current edition approved May 1,2011.Published July 2011.Originally approvedin 1985.Last previous edition approved in 2004 as D4527 99(2004).DOI:10.1520/D4527-99R11.2For 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.4Fisher Scientific No.9-556B available from Fisher Scientific Co.,203 FisherAve.,Pittsburgh,PA 15219,has been found satisfactory.The use of KontasK-586100(glass jacketed)available from Kontas Glass Co.,8000 Spruce St.,Vineland,NJ 08360,simplifies insulating the apparatus and reduces the possibilityof breakage.5Fisher Scientific 9-653B available from Fisher Scientific Co.,has been foundsatisfactory.6Fisher Scientific No.8-732-5C(aluminum dish)available from Fisher Scien-tific Co.,and Ventron No.2034(teflon cup)available from Ventron InstrumentCorp.,Cahn Division,16707 S.Carmenita Rd.,Cerritos,CA 90701,have beenfound to be satisfactory.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 5.8 Vacuum Oven,gravity-convection type,capable of tem-perature regulation within 61C at 125C and temperatureuniformity within 65C.5.9 Oven,gravity-convection type,capable of temperatureregulation within 61C at 125C and temperature uniformitywithin 65C.5.10 Desiccator.5.11 Analytical Balance,with a sensitivity of 60.1 mg.6.Reagents and Materials6.1 Toluene,having a residue after evaporation less than 10ppm(preferably less than 2 ppm).76.2 Nitrogen.6.3 Glass wool,extrac