ASTM_D_6443_-_14_2019e1.pdf

Designation:D644314(Reapproved 2019)1Standard 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.1NOTESubsection 7.5.2 was editorially corrected in July 2019.1.Scope1.1 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()unitsare to 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,health,and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.8 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade(TBT)Committee.2.Referenced Documents2.1 ASTM Standards:3D1552 Test Method for Sulfur in Petroleum Products byHigh Temperature Combustion and Infrared(IR)Detec-tion or Thermal Conductivity Detection(TCD)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 Elements1This 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 May 1,2019.Published July 2019.Originally approvedin 1999.Last previous edition approved in 2014 as D6443 14.DOI:10.1520/D6443-14R19E01.2Analytical Chemistry,Vol 55,pp.22102218.3For 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade(TBT)Committee.1 in 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