ASTM_D_6376_-_10.pdf

Designation:D637610Standard Test Method forDetermination of Trace Metals in Petroleum Coke byWavelength Dispersive X-ray Fluorescence Spectroscopy1This standard is issued under the fixed designation D6376;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.Scope*1.1 This test method covers the X-ray fluorescence spectro-metric determination of total sulfur and trace metals in samplesof raw or calcined petroleum coke.Elements determined usingthis test method are listed in Table 1.1.2 Detection limits,sensitivity,and optimal element rangeswill vary with matrices,spectrometer type,analyzing crystal,and other instrument conditions and parameters.1.3 All analytes are determined as the element and reportedas such.These include all elements listed in Table 1.This testmethod may be applicable to additional elements or concen-tration ranges if sufficient standards are available to produceproper calibration equations.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:2D346 Practice for Collection and Preparation of CokeSamples for Laboratory AnalysisD1552 Test Method for Sulfur in Petroleum Products(High-Temperature Method)D4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD5056 Test Method for Trace Metals in Petroleum Coke byAtomic AbsorptionD5600 Test Method for Trace Metals in Petroleum Coke byInductively Coupled Plasma Atomic Emission Spectrom-etry(ICP-AES)D6969 Practice for Preparation of Calcined Petroleum CokeSamples for AnalysisD6970 Practice for Collection of Calcined Petroleum CokeSamples for AnalysisE11 Specification for Woven Wire Test Sieve Cloth and TestSieves3.Terminology3.1 Definitions:3.1.1 calcined petroleum coke,npetroleum coke that hasbeen thermally treated to drive off the volatile matter and todevelop crystalline structure.3.1.2 green petroleum coke,nsame as raw petroleumcoke.3.1.3 petroleum coke,na solid,carbonaceous residueproduced by thermal decomposition of heavy petroleum frac-tions or cracked stocks,or both3.1.4 raw petroleum coke,npetroleum coke that has notbeen calcined.3.2 Definitions of Terms Specific to This Standard:3.2.1 alpha,ncorrection factor used to compensate forinterferences.3.2.2 analytical sample,na representative fraction takenfrom a larger mass of petroleum coke and reduced by grindingto pass a 75 m(No.200 mesh)sieve.3.2.3 pellet,na blend of dried sample and binder milledtogether and then formed into a pellet by pressure.3.2.4 reference samples,nsamples of known concentra-tions to be used in the calibration of the X-ray fluorescencespectrometer.4.Summary of Test Method4.1 A representative sample of petroleum coke is dried toconstant mass at 110 6 10C and then crushed to pass a 75 m(No.200 mesh)sieve.A weighed portion of this analyticalsample is mixed with stearic acid,or other suitable binder,andthen milled and compressed into a small,smooth pellet suitablefor analysis.The pellet is irradiated by an X-ray beam.The1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.05 on Properties of Fuels,Petroleum Coke and Carbon Material.Current edition approved July 1,2010.Published July 2010.Originally approvedin 1999.Last previous edition approved in 2009 as D637609.DOI:10.1520/D6376-10.2For 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.*A Summary of Changes section appears at the end of this standardCopyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 characteristic X rays of the elements analyzed are excited,separated,and detected by the wavelength-dispersive X-rayspectrometer.These measured X-ray intensities are convertedto elemental concentration through the use of a calibrationequation derived from analyses of standard materials.Thiscalibration equation defines the sensitivity and backgroundassociated with a particular X-ray spectrometer.4.2 The K-alpha spectral lines are used for all of theelements determined by this test method.5.Significance and Use5.1 The presence and concentration of sulfur and variousmetallic elements in a petroleum coke are major factorsdetermining the suitability of a coke f