ASTM_D_5600_-_14.pdf

Designation:D560014Standard Test Method forTrace Metals in Petroleum Coke by Inductively CoupledPlasma Atomic Emission Spectrometry(ICP-AES)1This standard is issued under the fixed designation D5600;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 analysis for commonlydetermined trace metals in test specimens of raw and calcinedpetroleum coke by inductively coupled plasma atomic emis-sion spectroscopy.1.2 Elements for which this test method is applicable arelisted in Table 1.Detection limits,sensitivity,and optimumranges of the metals will vary with the matrices and model ofspectrometer.1.3 This test method is applicable only to samples contain-ing less than one mass%ash.1.4 Elements present at concentrations above the upper limitof the working ranges can be determined with additional,appropriate dilutions.1.5 The values stated in SI units are to be regarded as thestandard.The values given in parentheses are for informationonly.1.6 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 AnalysisD1193 Specification for Reagent WaterD7260 Practice for Optimization,Calibration,and Valida-tion of Inductively Coupled Plasma-Atomic EmissionSpectrometry(ICP-AES)for Elemental Analysis of Petro-leum Products and LubricantsE11 Specification for Woven Wire Test Sieve Cloth and TestSieves3.Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 gross samplethe original,uncrushed,representativeportion taken from a shipment or lot of coke.3.1.2 ICP-AESInductively Coupled PlasmaAtomicEmission Spectrometry.3.1.3 petroleum cokea solid,carbonaceous residue pro-duced by thermal decomposition of heavy petroleum fractionsand cracked stocks.4.Summary of Test Method4.1 A test sample of the petroleum coke is ashed at 700C.The ash is fused with lithium borate.The melt is dissolved indilute hydrochloric acid(HCl),and the resultant solution isanalyzed by inductively coupled plasma atomic emissionspectrometry(ICP-AES)using simultaneous,or sequentialmultielemental determination of elements.The solution isintroduced to the ICP instrument by free aspiration or by anoptional peristaltic pump.The concentrations of the tracemetals are then calculated by comparing the emission intensi-ties from the sample with the emission intensities of thestandards used in calibration.5.Significance and Use5.1 The presence and concentration of various metallicelements in a petroleum coke are major factors in determiningthe suitability of the coke for various end uses.This testmethod provides a means of determining the concentrations ofthese metallic elements in a coke sample.5.2 The test method provides a standard procedure for useby buyer and seller in the commercial transfer of petroleumcoke to determine whether the petroleum coke meets thespecifications of the purchasing party.6.Interferences6.1 SpectralFollow the instrument manufacturers operat-ing guide to develop and apply correction factors to compen-sate for the interferences.To apply interference corrections,all1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products,Liquid Fuels,and Lubricantsand is the direct responsibility ofSubcommittee D02.03 on Elemental Analysis.Current edition approved June 1,2014.Published July 2014.Originally approvedin 1994.Last previous edition approved in 2009 as D5600 09.DOI:10.1520/D5600-14.2For 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 concentrations shall be within the previously established linearresponse range of each element.6.2 Spectral interferences are caused by:(1)overlap of aspectral line from another element;(2)unresolved overlap ofmolecular band spectra;(3)background contribution fromcontinuous or recombination phenomena;and(4)stray lightfrom the line emission of high-concentration elements.Spec-tral overlap can be compensated for by computer-correcting theraw data after monitoring and measuring the interfering ele-ment.Unresolved overlap requires selection of an alternatewavelength.Background contribution and stray light canusually be compensated