ASTM_D_6443_-_14.pdf

Designation:D644314Standard Test Method forDetermination of Calcium,Chlorine,Copper,Magnesium,Phosphorus,Sulfur,and Zinc in Unused Lubricating Oilsand Additives by Wavelength Dispersive X-ray FluorescenceSpectrometry(Mathematical Correction Procedure)1This standard is issued under the fixed designation D6443;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 determination of calcium,chlorine,copper,magnesium,phosphorus,sulfur,and zinc inunused lubricating oils,additives,and additive packages bywavelength dispersive X-ray fluorescence spectrometry.Ma-trix effects are handled with mathematical corrections.1.2 For each element,the upper limit of the concentrationrange covered by this test method is defined by the highestconcentration listed in Table 1.Samples containing higherconcentrations can be analyzed following dilution.1.3 For each element,the lower limit of the concentrationrange covered by this test method can be estimated by the limitof detection(LOD)2(see also 40 CFR 136 Appendix B)orlimit of quantification(LOQ),2both of which can be estimatedfrom Sr,the repeatability standard deviation.LOD and LOQvalues,determined from results obtained in the interlaboratorystudy on precision,are listed in Table 2.1.3.1 LOD and LOQ are not intrinsic constants of this testmethod.LOD and LOQ depend upon the precision attainableby a laboratory when using this test method.1.4 This test method uses regression software to determinecalibration parameters,which can include influence coeffi-cients(that is,interelement effect coefficients)(Guide E1361),herein referenced as alphas.Alphas can also be determinedfrom theory using relevant software.1.5 Setup of this test method is intended for persons trainedin the practice of X-ray spectrometry.Following setup,this testmethod can be used routinely.1.6 The values stated in either SI units or angstrom units areto be regarded separately as standard.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:3D1552 Test Method for Sulfur in Petroleum Products(High-Temperature Method)D4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD4307 Practice for Preparation of Liquid Blends for Use asAnalytical StandardsD4628 Test Method for Analysis of Barium,Calcium,Magnesium,and Zinc in Unused Lubricating Oils byAtomic Absorption SpectrometryD4927 Test Methods for Elemental Analysis of LubricantandAdditiveComponentsBarium,Calcium,Phosphorus,Sulfur,and Zinc by Wavelength-DispersiveX-Ray Fluorescence SpectroscopyD4951 Test Method for Determination of Additive Elementsin Lubricating Oils by Inductively Coupled PlasmaAtomic Emission SpectrometryD5185 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 PerformanceE29 Practice for Using Significant Digits in Test Data toDetermine Conformance with Specifications1This 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 Dec.1,2014.Published January 2015.Originallyapproved in 1999.Last previous edition approved in 2010 as D6443 04(2010).DOI:10.1520/D6443-14.2Analytical Chemistry,Vol 55,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 E1361 Guide for Correction of Interelement Effects inX-Ray Spectrometric Analysis2.2 Government Standard:440 CFR,136 Appendix B,Definition and Procedure for theDetermination of the Method Detection LimitRevision1.11,pp.265-2673.Summary of Test Method3.1 The X-ray fluorescence spectrometer is initially cali-brated by the following procedure.For each element,the slopeand intercept of the calibration curve are determined byregressing concentration data and intensities measured on a setof physical standards.Empirical alphas can also be determinedby r