ASTM_D_5056_-_15.pdf

Designation:D505615Standard Test Method forTrace Metals in Petroleum Coke by Atomic Absorption1This standard is issued under the fixed designation D5056;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 the commonlydetermined trace metals(aluminum,calcium,iron,nickel,silicon,sodium,and vanadium)in laboratory analysis samplesof raw and calcined petroleum coke by atomic absorptionspectroscopy.1.2 The elemental concentration ranges for which this testmethod is applicable and the limits of detection of this testmethod are listed in Table 1.1.3 The values stated in SI units are to be regarded as thestandard.1.4 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.For warningstatements,see Sections 8 10.2.Referenced Documents2.1 ASTM Standards:2D346 Practice for Collection and Preparation of CokeSamples for Laboratory AnalysisD6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System PerformanceD1193 Specification for Reagent Water3.Summary of Test Method3.1 A representative sample of the petroleum coke is ashedat 525 C under specified conditions.The ash is fused withlithium tetraborate(Li2B4O7),or lithium metaborate(LiBO3).The melt is dissolved in dilute hydrochloric acid(HCl),and theresultant solution is analyzed by atomic absorption spectros-copy for the following elements:aluminum,calcium,iron,nickel,silicon,sodium,and vanadium.4.Significance and Use4.1 The presence and concentration of various metallicelements in a petroleum coke are major factors in the suitabilityof the coke for various uses.This test method provides a meansof measuring the amounts of those metallic elements in thecoke sample.4.2 The concentration of these elements is one factor indetermining the economic value of the coke.Coke used forproduction of electrodes will have different specification re-quirements dependent on what service the electrodes will beused in.Generally the fuel cokes are highest in metallicelement concentration and have the least economic value.4.3 The test method provides a standard procedure for useby the purchaser and seller in the commercial transfer ofpetroleum coke to determine whether the lot of coke meets thespecifications of the purchasing party.5.Interferences5.1 Spectral interferences can occur when using other thanthe recommended wavelength for analysis or when usingmulti-elemental hollow cathode lamps.6.Apparatus6.1 Furnace,electric,capable of regulation of temperatureat 525 C 6 10 C.6.2 Magnetic Stirring Hot Plate.6.3 Platinum Dish,50 mL to 58 mL capacity.6.4 Platinum Dish,150 mL to 200 mL capacity.6.5 Platinum-Tipped Tongs.6.6 Furnace,electric,capable of regulation of temperatureat 950 C 6 10 C or a Meker type forced air burner.6.7 Atomic Absorption Spectrophotometer(AAS),equippedas follows:6.7.1 Background Correction,using either a deuterium(D2)arc background corrector or other comparable simultaneousbackground correction system.6.7.2 Burner Head,capable of supporting a nitrous oxide-acetylene flame.1This 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 1,2015.Published June 2015.Originallyapproved in 1990.Last previous edition approved in 2010 as D5056 04(2010).DOI:10.1520/D5056-15.2For 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.*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 6.7.3 Burner Head,single or multiple-slot,capable of sup-porting an air-acetylene flame.6.7.4 Hollow Cathode Lamps,one for each of the elementsto be analyzed:aluminum,calcium,iron,nickel,silicon,sodium,and vanadium.NOTE1Multi-elemental lamps can also be used;however,spectralinterferences are possible(see 5.1).7.Reagents7.1 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 Societywhere such specifications are available.3Other grades may beused,provided it is first ascertained that the reagent is ofsufficien