ASTM_D_7679_-_13.pdf

Designation:D767913Standard Test Method forSulfur Content in Carbon Black Feedstock Oils1This standard is issued under the fixed designation D7679;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 instrumental determinationof sulfur content in samples of carbon black feedstock oils.Values obtained represent the total sulfur content.Two analysismethods are available for use:Test Method A:High-Temperature CombustionWithInfrared Absorption Detection ProceduresSections 4 10Test Method B:X-Ray FluorescenceSections 13 171.2 This test method is applicable to carbon black feedstockoils derived from petroleum,coal,and other sources whichinclude fuel oils,residues,tars,pitches,reclaimed oils,andsimilar materials that are normally handled as liquids.This testmethod is applicable to products typically containing 0 to 5mass%sulfur.1.3 The results of these tests can be expressed as mass%sulfur.1.4 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.5 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:2D1619 Test Methods for Carbon BlackSulfur ContentD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD4483 Practice for Evaluating Precision for Test MethodStandards in the Rubber and Carbon Black ManufacturingIndustries3.Significance and Use3.1 Measuring the total sulfur content of feedstock oil isoften a necessary component in calculations for sulfur dioxideemissions.3.2 The carbon black industry measures sulfur content offeedstock oils along with sulfur content of carbon blackproducts per Test Method D1619 in calculations to determinesulfur dioxide emissions for compliance with governmentalreporting requirements.TEST METHOD A:HIGH-TEMPERATURECOMBUSTION WITH INFRARED ABSORPTIONDETECTION PROCEDURES4.Summary of Test Method4.1 In this test method,a sample of feedstock oil is weighedin a combustion boat containing either a tungsten oxide basedaccelerator,sand or aluminum oxide absorbent,and the sulfurcontent is determined by placing the boat in a tube furnace at1350C in an air or oxygen-enriched atmosphere resulting incomplete combustion.Sulfur in the sample is completelyoxidized to sulfur dioxide.Moisture and particulates areremoved from the gas stream by traps filled with anhydrousmagnesium perchlorate.The gas stream is then passed througha cell in which sulfur dioxide concentration is measured by aninfrared(IR)absorption detector at a precise wavelength in theIR spectrum.The IR absorption detects sulfur dioxide through-out the entire combustion process.The integral of the detectorsignal is the basis for the total sulfur content of a sample.4.2 This test method is for use with commercially availablesulfur analyzers equipped to carry out the combustion andmeasurement operations automatically.4.3 The sulfur analyzer shall be calibrated using appropriatecalibration standards(see 6.7).4.4 The instrument may be configured to analyze more thanone element such as a carbon-sulfur analyzer.In this case,theanalyzer has individual detectors for each element that arearranged in series.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 Nov.1,2013.Published December 2013.Originallyapproved in 2010.Last previous edition approved in 2011 as D7679 11.DOI:10.1520/D7679-13.2For 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 5.Apparatus5.1 There are a number of commercially available instru-ments designed to measure sulfur content in organic materialsincluding sulfur and carbon-sulfur combustion analyzers.Thistest method makes no specifications regarding system designs.5.2 Functionally,however,the following are specified for allinstruments:5.2.1 An analytical balance,or equivalent,that is capable ofa weighing sensitivity of 0.1 mg or better resolution.5.2.2 The combustion tube and boat are made of a suitablematerial such as mullite,porcelain,or zircon.5.2.3 The sample is absorbed onto a solid which mayinclude the followin