ASTM_D_4951_-_14_2019.pdf

Designation:D495114(Reapproved 2019)Standard Test Method forDetermination of Additive Elements in Lubricating Oils byInductively Coupled Plasma Atomic Emission Spectrometry1This standard is issued under the fixed designation D4951;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.Scope1.1 This test method covers the quantitative determinationof barium,boron,calcium,copper,magnesium,molybdenum,phosphorus,sulfur,and zinc in unused lubricating oils andadditive packages.1.2 The precision statements are valid for dilutions in whichthe mass%sample in solvent is held constant in the range of1%to 5%by mass of oil.1.3 The precision tables define the concentration rangescovered in the interlaboratory study.However,both lower andhigher concentrations can be determined by this test method.The low concentration limits are dependent on the sensitivityof the ICP instrument and the dilution factor.The highconcentration limits are determined by the product of themaximum concentration defined by the linear calibration curveand the sample dilution factor.1.4 Sulfur can be determined if the instrument can operate ata wavelength of 180 nm.1.5 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.6 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.1.7 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:2D1552 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 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 SpectroscopyD5185 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 Performance3.Summary of Test Method3.1 A sample portion is weighed and diluted by mass withmixed xylenes or other solvent.An internal standard,which isrequired,is either weighed separately into the test solution or ispreviously combined with the dilution solvent.Calibrationstandards are prepared similarly.The solutions are introducedto the ICP instrument by free aspiration or an optionalperistaltic pump.By comparing emission intensities of ele-ments in the test specimen with emission intensities measuredwith the calibration standards and by applying the appropriateinternal standard correction,the concentrations of elements inthe sample are calculable.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.1,2019.Published December 2019.Originallyapproved in 1989.Last previous edition approved in 2014 as D4951 14.DOI:10.1520/D4951-14R19.2For 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 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 4.Significance and Use4.1 This test method usually requires several minutes persample.This test method covers eight elements and t