ASTM_D_5708_-_15.pdf

Designation:D570815Standard Test Methods forDetermination of Nickel,Vanadium,and Iron in Crude Oilsand Residual Fuels by Inductively Coupled Plasma(ICP)Atomic Emission Spectrometry1This standard is issued under the fixed designation D5708;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 These test methods cover the determination of nickel,vanadium,and iron in crude oils and residual fuels byinductively coupled plasma(ICP)atomic emission spectrom-etry.Two different test methods are presented.1.2 Test Method A(Sections 7 11 and 18 22)ICP isused to analyze a sample dissolved in an organic solvent.Thistest method uses oil-soluble metals for calibration and does notpurport to quantitatively determine or detect insoluble particu-lates.1.3 Test Method B(Sections 12 22)ICP is used toanalyze a sample that is decomposed with acid.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 15.2.Typically,the lowconcentration limits are a few tenths of a milligram perkilogram.Precision data are provided for the concentrationranges specified in Section 21.1.5 The values stated in SI units are to be regarded asstandard.1.5.1 ExceptionThe values given in parentheses are forinformation only1.6 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Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD1548 Test Method for Vanadium in Heavy Fuel Oil1(Withdrawn 1997)3D4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD5185 Test Method for Multielement Determination ofUsed and Unused Lubricating Oils and Base Oils byInductively Coupled Plasma Atomic Emission Spectrom-etry(ICP-AES)D6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System PerformanceD7260 Practice for Optimization,Calibration,and Valida-tion of Inductively Coupled Plasma-Atomic EmissionSpectrometry(ICP-AES)for Elemental Analysis of Petro-leum Products and Lubricants3.Summary of Test Method3.1 Test Method AApproximately 10 g of the sample aredissolved in an organic solvent(WarningCombustible.Va-por is harmful.)to give a specimen solution containing 10%(m/m)of sample.The solution is nebulized into the plasma,and the intensities of the emitted light at wavelengths charac-teristic of the analytes are measured sequentially or simultane-ously.The intensities are related to concentrations by theappropriate use of calibration data.1These test methods are under the jurisdiction of ASTM Committee D02 onPetroleum Products,Liquid Fuels,and Lubricants and is the direct responsibility ofSubcommittee D02.03 on Elemental Analysis.Current edition approved Dec.1,2015.Published December 2015.Originallyapproved in 1995.Last previous edition approved in 2012 as D5708 121.DOI:10.1520/D5708-15.2For 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.3The last approved version of this historical standard is referenced onwww.astm.org.*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 3.2 Test Method BOne to 20 g of sample are weighed intoa beaker and decomposed with concentrated sulfuric acid(WarningPoison.Causes severe burns.Harmful or fatal ifswallowed or inhaled.)by heating to dryness.Great care mustbe used in this decomposition because the acid fumes arecorrosive and the mixture is potentially flammable.The re-sidual carbon is burned off by heating at 525 C in a mufflefurnace.The inorganic residue is digested with nitricacid(WarningPoison.Causes severe burns.Harmful or fatalif swallowed or inhaled.),evaporated to incipient dryness,dissolved in dilute nitric acid,and made up to volume.Thesolution is nebulized into the plasma of an atomic emissionspectrometer.The intensities of light emitted at characteristicwavelengths of the metals are measured sequentially or simul-taneously.These intensities are related to concentrations by theappropriate use of calibration data.4.Significance and Use4.1 These test methods cover,in single procedures,thedetermination of Ni,V,and Fe in crude oils and resid