ASTM_D_7751_-_14.pdf

Designation:D775114Standard Test Method forDetermination of Additive Elements in Lubricating Oils byEDXRF Analysis1This standard is issued under the fixed designation D7751;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 quantitative determinationof additive elements in unused lubricating oils and additivepackages,as shown in Table 1.The pooled limit of quantitationof this test method as obtained by statistical analysis ofinterlaboratory test results is 0.02%for magnesium,0.003%for phosphorus,0.002%for sulfur,0.001%for chlorine,0.003%for calcium,0.001%for zinc,and 0.002%formolybdenum.1.2 Additive packages require dilution with a contaminationfree diluent(base oil)prior to analysis.The dilution factor hasto be calculated from the expected concentrations to bring theconcentrations for all elements into the ranges listed in Table 1.1.3 Some lubrication oils will contain higher concentrationsthan the maximum concentrations listed in Table 1.Thesesamples require dilution with a contamination free diluent(base oil)prior to analysis.The dilution factor has to becalculated from the expected concentrations to bring theconcentrations for all elements into the ranges listed in Table 1.1.4 This test method is limited to the use of energydispersive X-ray fluorescence(EDXRF)spectrometers em-ploying an X-ray tube for excitation in conjunction with theability to separate the signals of adjacent elements by using ahigh resolution semiconductor detector.1.5 This test method uses inter-element correction factorscalculated from a fundamental parameters(FP)approach orfrom another matrix correction method.1.6 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.6.1 The preferred concentration units are mg/kg or mass%.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:2D4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System PerformanceD6300 Practice for Determination of Precision and BiasData for Use in Test Methods for Petroleum Products andLubricantsD6792 Practice for Quality System in Petroleum Productsand Lubricants Testing LaboratoriesD7343 Practice for Optimization,Sample Handling,Calibration,and Validation of X-ray Fluorescence Spec-trometry Methods for Elemental Analysis of PetroleumProducts and LubricantsE1621 Guide for Elemental Analysis by Wavelength Disper-sive X-Ray Fluorescence Spectrometry2.2 ISO Standards:3ISO 4259 Determination and application of precision data inrelation to methods of test3.Terminology3.1 Definitions:3.1.1 energy dispersive X-ray spectrometry,nXRF spec-trometry applying energy dispersive selection of radiation.3.2 Abbreviations:1This 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 Dec.1,2014.Published January 2015.Originallyapproved in 2011.Last previous edition approved in 2012 as D7751 12.DOI:10.1520/D7751-14.2For 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.3Available from International Organization for Standardization(ISO),1,ch.dela Voie-Creuse,CP 56,CH-1211 Geneva 20,Switzerland,http:/www.iso.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 3.2.1 EDXRFEnergy Dispersive X-ray FluorescenceSpectrometry.3.2.2 FPFundamental Parameters.4.Summary of Test Method4.1 A specimen is placed in the X-ray beam,and theappropriate regions of its spectrum are measured to give thefluorescent intensities of magnesium,phosphorus,sulfur,chlorine,calcium,zinc,and molybdenum.Other regions of thespectrum are measured to compensate for matrix variation.Tooptimize the sensitivity for each element or group of elements,a combination of optimized excitation and detection conditionsmay be used(no more than two conditions should be used inorder to keep the analysis time as short as possible,typicallyunder ten minutes).There may be