ASTM_D_1619_-_11.pdf

Designation:D161911Standard Test Methods forCarbon BlackSulfur Content1This standard is issued under the fixed designation D1619;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.This standard has been approved for use by agencies of the U.S.Department of Defense.1.Scope1.1 These test methods cover the determination of the sulfurcontent of carbon black.The following test methods areincluded:SectionsTest Method AHigh-Temperature Combustion With In-frared Absorption Detection Procedures6 to 13Test Method BX-Ray Fluorescence14 to 191.2 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.3This 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:2D1509 Test Methods for Carbon BlackHeating LossD1799 Practice for Carbon BlackSampling PackagedShipmentsD1900 Practice for Carbon BlackSampling Bulk Ship-mentsD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustries3.Significance and Use3.1 The total sulfur content of a carbon black is useful indeterminingwhetheramaterialmeetsacustomersspecifications,providing data for performing a sulfur materialbalance around a process for environmental monitoring andreporting,and in calculations for reconstructing a rubbercomposition from analytical data.4.Reagents4.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.3Other grades may beused,provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.5.Sampling5.1 Samples of packaged materials shall be taken in accor-dance with Practice D1799 or Practice D1900.TEST METHOD A HIGH-TEMPERATURECOMBUSTION WITH INFRARED ABSORPTIONDETECTION PROCEDURES6.Summary of Test Method6.1 The specimen is burned in a tube furnace at a minimumoperating temperature of 1350C in a stream of oxygen tooxidize the sulfur.Moisture and particulates are removed fromthe gas by traps filled with anhydrous magnesium perchlorate.The gas stream is passed through a cell in which sulfur dioxideis measured by an infrared(IR)absorption detector.Sulfurdioxide absorbs IR energy at a precise wavelength within theIR spectrum.Energy is absorbed as the gas passes through thecell body in which the IR energy is being transmitted.Thus,atthe detector,less energy is received.All other IR energy iseliminated from reaching the detector by a precise wavelengthfilter.Thus,the absorption of IR energy can be attributed onlyto sulfur dioxide whose concentration is proportional to thechange in energy at the detector.One cell is used as both a1These test methods are under the jurisdiction of ASTM Committee D24 onCarbon Black and are the direct responsibility of Subcommittee D24.66 onEnvironment,Health,and Safety.Current edition approved Jan.1,2011.Published June 2011.Originally approvedin 1958.Last previous edition approved in 2010 as D1619 10.DOI:10.1520/D1619-11.2For 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 Analar Standards for LaboratoryChemicals,BDH Ltd.,Poole,Dorset,U.K.,and the United States Pharmacopeiaand National Formulary,U.S.Pharmaceutical Convention,Inc.(USPC),Rockville,MD.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 reference and a measurement chamber.Total sulfur as sulfurdioxide is detected on a continuous basis.This test method isempirical.Therefore,the apparatus must be calibrated by theuse of standard reference materials(SRM).6.2 This test method is for use with commercially availablesulfur analyzers equipped to carry out the preceding operationsautomatically and must be calibrated using standard referencematerial(carbon black)of known sulfur content based on therange of sulfur in each carbon black specimen analyzed.7.Apparatus7.1 Measurement Apparatusequipped to automaticallycombust the specimen.7.2 Comb