ASTM_D_5059_-_14.pdf

Designation:D505914Standard Test Methods forLead in Gasoline by X-Ray Spectroscopy1This standard is issued under the fixed designation D5059;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.This standard has been approved for use by agencies of the U.S.Department of Defense.1.Scope*1.1 These test methods cover the determination of the totallead content of a gasoline within the following concentrationranges:0.010 to 5.0 g Pb/US gal0.012 to 6.0 g Pb/UK gal0.0026 to 1.32 g Pb/L1.1.1 Test Methods A and B cover the range of 0.10 to 5.0 gPb/US gal.Test Method C covers the range of 0.010 to 0.50 gPb/US gal.1.1.2 These test methods compensate for normal variationin gasoline composition and are independent of lead alkyl type.1.2 Test Method A(formerly in withdrawn Test MethodD2599)Sections 5 9.Test Method B(formerly in withdrawn Test MethodD2599)Sections 10 14.Test Method C(formerly in withdrawn Test MethodD3229)Sections 15 19.1.3 The values stated in SI are to be regarded as thestandard.For reporting purposes the values stated in grams perU.S.gallon are the preferred units in the United States.Notethat in other countries,other units can be preferred.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 specific hazardstatements,see Sections 5,6,11,and 18.2.Referenced Documents2.1 ASTM Standards:2D3341 Test Method for Lead in GasolineIodine Mono-chloride MethodD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System PerformanceD6792 Practice for Quality System in Petroleum Productsand Lubricants Testing Laboratories3.Summary of Test Method3.1 There are three alternative test methods,as follows.3.1.1 Test Method A(Bismuth Internal Standard MethodHigh Concentration)One volume of sample is mixed thor-oughly with an equal volume of bismuth internal standardsolution.The mixture is placed in the X-ray beam and theintensities of the lead L-1radiation at 1.175 and the bismuthL-1radiation at 1.144 are determined.The lead concentra-tion of the sample is measured by comparing the ratio of grosscounting rate at 1.175 with the gross counting rate at 1.144 to a previous prepared calibration curve of concentrationversus the same ratios.3.1.2 Test Method B(Scattered Tungsten RadiationMethod)The ratio of the net X-ray intensity of the lead L-1radiation to the net intensity of the incoherently scatteredtungsten L-1radiation is obtained on a portion of the sample.The lead content is determined by multiplying this ratio by acalibration factor obtained with a standard lead solution ofknown concentration.3.1.3 Test Method C(Bismuth Internal Standard Method,Low Concentration)Twenty millilitres of sample is mixedthoroughly with two milliliters of bismuth internal standardsolution.The mixture is placed in the X-ray beam of aspectrometer and the intensities of the lead L-1radiation at1.175,the bismuth L-1radiation at 1.144,and a back-ground at 1.194 are determined.A blank,made withiso-octane and bismuth internal standard,is run using the sameprocedure.The lead concentration is measured by determiningthe ratio of the net counting rate at 1.175 to the grosscounting rate at 1.144 for the sample,subtracting thecomparable ratio found for the blank,and comparing to apreviously prepared calibration curve of concentration versusthe same ratios.1These test methods are under the jurisdiction of Committee D02 on PetroleumProducts,Liquid Fuels,and Lubricants and are the direct responsibility ofSubcommittee D02.03 on Elemental Analysis.Current edition approved June 1,2014.Published July 2014.Originally approvedin 1990.Last previous edition approved in 2013 as D5059 13.DOI:10.1520/D5059-14.Initially published as D2599 67T and D3229 73,now withdrawn.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 4.Significance and Use4.1 These test methods determine the concentration of lead(from alkyl addition)in gasoline.These alkyl additives im-prove the antiknock properties.4.2 Test Method C is used to ensure compliance of tracelead as required by federal regulations for lead-free gasoline(40 CFR part 80).TE