ASTM_D_7771_-_15.pdf

Designation:D777115Standard Test Method forDetermination of Benzo-Pyrene(BaP)Content in CarbonBlack1This standard is issued under the fixed designation D7771;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 qualitative and quantitativedetermination of only benzo-pyrene(BaP),a specific poly-cyclic aromatic hydrocarbon(PAH),on carbon black.Theprocedure involves Soxhlet extraction with toluene and analy-sis by gas chromatography with mass spectrometry(GC/MS).This method is not intended to test for U.S.Food and DrugAdministration(FDA21 CFR 178.3297)compliance of carbonblacks used for indirect food contact applications.1.2 UnitsThe values stated in SI units are to be regardedas the standard.No other units of measurement are included inthis standard.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:2D4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustries2.2 EPA Standard:3Method 8270D Semivolatile Organic Compounds by GasChromatography/Mass Spectrometry(GC/MS)2.3 Federal Standard:21 CFR 178.3297 Indirect Food Additives:Adjuvants,Pro-ductions Aids,and Sanitizers,Colorants for Polymers43.Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 benzo-pyrene,BaP,nalsoknownas3,4-benzopyrene or benzo-a-pyrene is a specific polycyclic aro-matic hydrocarbon(PAH)or polynuclear aromatic hydrocar-bon that consist of fused aromatic rings with no heteroatom orsubstituent.3.1.1.1 DiscussionPAHs naturally occur in oil,coal,andtar deposits;are produced by the incomplete combustion ofhydrocarbons;and occur in many other products and processes.BaP is a pentacyclic PAH with the formula C20H12,related topyrene by fusion of a phenylene group in the alpha position.4.Summary of Test Method4.1 A portion of carbon black is Soxhlet-extracted withtoluene for 16 h.The extract is concentrated and subsequentlyanalyzed for BaP by gas chromatography with mass spectrom-etry(GC/MS).The BaP quantification is performed by themeans of an internal standard.5.Significance and Use5.1 This test procedure is used to determine the concentra-tion of BaP extracted from carbon black by the means of aSoxhlet extraction apparatus with toluene.6.Apparatus6.1 Soxhlet Extractor with Reflux Condenser,50-or 100-cm3capacity.6.2 Extraction Thimbles,glass or cellulose,approximately50-to 70-cm3capacity.For instance,glass extraction thimbleof 35-mm diameter by 90-mm height with course porosity(70to 100 m similar to Ace Glass Size C,Porosity B,Code-14).1This test method is under the jurisdiction of ASTM Committee D24 on CarbonBlack and is the direct responsibility of Subcommittee D24.66 on Environment,Health,and Safety.Current edition approved Jan.1,2015.Published February 2015.Originallyapproved in 2011.Last previous edition approved in 2013 as D7771 13.DOI:10.1520/D7771-15.2For 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.3Available from United States Environmental Protection Agency(EPA),ArielRios Bldg.,1200 Pennsylvania Ave.,NW,Washington,DC 20004,http:/www.epa.gov/epaoswer/hazwaste/test/new-meth.htm#8270D.4Available from the U.S.Government Printing Office,Superintendent ofDocuments,732 N.Capital St.,NW.,Washington,DC 20402-0001.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 6.3 Heating Mantle,compatible with boiling flask describedin 6.4.6.4 Boiling Flasks for Soxhlet,for example,250 cm3.6.5 Glass Beads,approximately 180 to 250 m(60/80mesh)if glass thimbles are used.Need to be very clean ortoluene extracted.6.6 PTFE or Glass Boiling Beads,approximately 3 mm.6.7 Glass Wool,need to be very clean or toluene extracted.6.8 Rotary Evaporator,with temperature-controlled waterbath,automatic pressure regulation,and solvent-proof mem-brane vacuum pump.6.9 Nitrogen Blow-Down Apparatus,equipped with a con-trolled water bath and nitrogen pressure control.6.10 Pear-Shaped Flasks for Rotary Evaporator,forexample,25,50,and 100 cm3.6.11 GC/MS,with autosampler.6.11.1 MS with electron impact(EI)capability and single-ion monitoring(SIM)mode.6.11.2 GC Capillary Column,usually a nonpolar GC col-umn composed of 5%phenyl-methyl silicone coating is usedfor PAH analysis.6.11.3 Deactivated Straight Borosilicate Liner with SmallPiece