ASTM_D_4294_-_10.pdf

Designation:D429410Standard Test Method forSulfur in Petroleum and Petroleum Products by EnergyDispersive X-ray Fluorescence Spectrometry1This standard is issued under the fixed designation D4294;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 This test method covers the determination of total sulfurin petroleum and petroleum products that are single-phase andeither liquid at ambient conditions,liquefiable with moderateheat,or soluble in hydrocarbon solvents.These materials caninclude diesel fuel,jet fuel,kerosine,other distillate oil,naphtha,residual oil,lubricating base oil,hydraulic oil,crudeoil,unleaded gasoline,gasohol,biodiesel(see Note 2),andsimilar petroleum products.NOTE1Oxygenated fuels with ethanol or methanol contents exceed-ing the limits given in Table 1 can be dealt with using this test method,butthe precision and bias statements do not apply(see Appendix X3).NOTE2For samples with high oxygen contents(3 wt%)sampledilution as described in 1.3 or matrix matching must be performed toassure accurate results.1.2 Interlaboratory studies on precision revealed the scopeto be 17 mg/kg to 4.6 mass%.An estimate of this test methodspooled limit of quantitation(PLOQ)is 16.0 mg/kg as calcu-lated by the procedures in Practice D6259.However,becauseinstrumentation covered by this test method can vary insensitivity,the applicability of the test method at sulfurconcentrations below approximately 20 mg/kg must be deter-mined on an individual basis.An estimate of the limit ofdetection is three times the reproducibility standard deviation,and an estimate of the limit of quantitation2is ten times thereproducibility standard deviation.1.3 Samples containing more than 4.6 mass%sulfur can bediluted to bring the sulfur concentration of the diluted materialwithin the scope of this test method.Samples that are dilutedcan have higher errors than indicated in Section 16 thannon-diluted samples.1.4 Volatile samples(such as high vapor pressure gasolinesor light hydrocarbons)may not meet the stated precisionbecause of selective loss of light materials during the analysis.1.5 Afundamental assumption in this test method is that thestandard and sample matrices are well matched,or that thematrix differences are accounted for(see 5.2).Matrix mis-match can be caused by C/H ratio differences between samplesand standards(see Section 5)or by the presence of otherheteroatoms.1.6 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.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.2.Referenced Documents2.1 ASTM Standards:3D4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD6259 Practice for Determination of a Pooled Limit ofQuantitationD6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System PerformanceD7343 Practice for Optimization,Sample Handling,Calibration,and Validation of X-ray Fluorescence Spec-trometry Methods for Elemental Analysis of PetroleumProducts and LubricantsE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with Specifications3.Summary of Test Method3.1 The sample is placed in the beam emitted from an X-raytube.The resultant excited characteristic X radiation is1This test method is 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 Feb.15,2010.Published March 2010.Originallyapproved in 1983.Last previous edition approved in 2008 as D429408a1.DOI:10.1520/D4294-10.2Analytical Chemistry,Vol 55,1983,pp.2210-2218.3For 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 measured,and the accumulated count is compared with countsfrom previously prepared calibration samples to obtain thesulfur concentration in mass%and/or mg/kg.A minimum ofthree groups of calibration samples are required to span theconcentration range:0.0 to