1、Designation:D586300a(Reapproved 2016)Standard Test Methods forDetermination of Nickel,Vanadium,Iron,and Sodium inCrude Oils and Residual Fuels by Flame Atomic AbsorptionSpectrometry1This standard is issued under the fixed designation D5863;the number immediately following the designation indicates t
2、he 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 These test methods cover the determination of nickel,van
3、adium,iron,and sodium in crude oils and residual fuels byflame atomic absorption spectrometry(AAS).Two differenttest methods are presented.1.2 Test Method A,Sections 713Flame AAS is used toanalyze a sample that is decomposed with acid for thedetermination of total Ni,V,and Fe.1.3 Test Method B,Secti
4、ons 1419Flame AAS is used toanalyze a sample diluted with an organic solvent for thedetermination of Ni,V,and Na.This test method uses oil-soluble metals for calibration to determine dissolved metalsand does not purport to quantitatively determine nor detectinsoluble particulates.Hence,this test met
5、hod may underesti-mate the metal content,especially sodium,present as inorganicsodium salts.1.4 The concentration ranges covered by these test methodsare determined by the sensitivity of the instruments,theamount of sample taken for analysis,and the dilution volume.A specific statement is given in N
6、ote 1.1.5 For each element,each test method has its own uniqueprecision.The user can select the appropriate test method basedon the precision required for the specific analysis.1.6 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.
7、1.7 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.Specific warningst
8、atements are given in 7.1,8.2,8.5,10.2,10.4,and 15.1.2.Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD6299 Practice for Applying
9、 Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System Performance3.Summary of Test Method3.1 Test Method AOne to twenty grams of sample areweighed into a beaker and decomposed with concentratedsulfuric acid by heating to dryness.The residual carbon is
10、burned off by heating at 525 C in a muffle furnace.Theinorganic residue is digested in dilute nitric acid,evaporated toincipient dryness,dissolved in dilute nitric and made up tovolume with dilute nitric acid.Interference suppressant isadded to the dilute nitric acid solution.The solution isnebulize
11、d into the flame of an atomic absorption spectrometer.A nitrous oxide/acetylene flame is used for vanadium and anair/acetylene flame is used for nickel and iron.The instrumentis calibrated with matrix-matched standard solutions.Themeasured absorption intensities are related to concentrations bythe a
12、ppropriate use of calibration data.3.2 Test Method BSample is diluted with an organicsolvent to give a test solution containing either 5%(m/m)or20%(m/m)sample.The recommended sample concentrationis dependent on the concentrations of the analytes in thesample.For the determination of vanadium,interfe
13、rence sup-pressant is added to the test solution.The test solution isnebulized into the flame of an atomic absorption spectrometer.A nitrous oxide/acetylene flame is used for vanadium and an1These test methods are under the jurisdiction of ASTM Committee D02 onPetroleum Products,Liquid Fuels,and Lub
14、ricantsand are the direct responsibility ofSubcommittee D02.03 on Elemental Analysis.Current edition approved April 1,2016.Published May 2016.Originallyapproved in 1995.Last previous edition approved in 2011 as D5863 00a(2011).DOI:10.1520/D5863-00AR16.2For referenced ASTM standards,visit the ASTM we
15、bsite,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 air/
16、acetylene flame is used for nickel and sodium.The mea-sured absorption intensities are related to concentrations by theappropriate use of calibration data.4.Significance and Use4.1 When fuels are combusted,metals present in the fuelscan form low melting compounds that are corrosive to metalparts.Metals present at trace levels in petroleum can deactivatecatalysts during processing.These test methods provide ameans of quantitatively determining the concentrations ofvanadium,nickel,iron,and sodium.
