ASTM_D_7303_-_17.pdf

Designation:D730317Standard Test Method forDetermination of Metals in Lubricating Greases byInductively Coupled Plasma Atomic Emission Spectrometry1This standard is issued under the fixed designation D7303;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 a numberof metals such as aluminum,antimony,barium,calcium,iron,lithium,magnesium,molybdenum,phosphorus,silicon,sodium,sulfur,and zinc in unused lubricating greases byinductively coupled plasma atomic emission spectrometry(ICP-AES)technique.1.1.1 The range of applicability for this test method,basedon the interlaboratory study conducted in 2005,2is aluminum(10 to 600),antimony(10 to 2300),barium(50 to 800),calcium(20 to 50 000),iron(10 to 360),lithium(300 to 3200),magnesium(30 to 10 000),molybdenum(50 to 22 000),phosphorus(50 to 2000),silicon(10 to 15 000),sodium(30 to1500),sulfur(1600 to 28 000),and zinc(300 to 2200),all inmg/kg.Lower levels of elements may be determined by usinglarger sample weights,and higher levels of elements may bedetermined by using smaller amounts of sample or by using alarger dilution factor after sample dissolution.However,thetest precision in such cases has not been determined,and maybe different than the ones given in Table 1.1.1.2 It may also be possible to determine additional metalssuch as bismuth,boron,cadmium,chromium,copper,lead,manganese,potassium,titanium,etc.by this technique.However,not enough data is available to specify the precisionfor these latter determinations.These metals may originate intogreases through contamination or as additive elements.1.1.3 During sample preparation,the grease samples aredecomposed with a variety of acid mixture(s).It is beyond thescope of this test method to specify appropriate acid mixturesfor all possible combination of metals present in the sample.But if the ash dissolution results in any visible insolublematerial,the test method may not be applicable for the type ofgrease being analyzed,assuming the insoluble material con-tains some of the analytes of interest.1.2 Elements present at concentrations above the upper limitof the calibration curves can be determined with additionalappropriate dilutions of dissolved samples and with no degra-dation of precision.1.3The development of the technique behind this testmethod is documented by Fox.31.4 The values stated in SI units are to be regarded as thestandard.The values given in parentheses are for informationonly.1.5 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.Specific warningstatements are given in Sections 8 and 10.1.6 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:4D1193 Specification for Reagent WaterD3340 Test Method for Lithium and Sodium in LubricatingGreases by Flame Photometer(Withdrawn 2013)5D4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4951 Test Method for Determination of Additive Elementsin Lubricating Oils by Inductively Coupled PlasmaAtomic Emission Spectrometry1This 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 June 1,2017.Published June 2017.Originallyapproved in 2006.Last previous edition approved in 2012 as D7303 12.DOI:10.1520/D7303-17.2Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D02-1608.ContactASTM CustomerService at serviceastm.org.3Fox,B.S.,“Elemental Analysis of Lubricating Grease by Inductively CoupledPlasm Atomic Emission Spectrometry(ICP-AES),”J.ASTM International,Vol 2,No.8,2005,pp.12966.4For 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.5The last approved version of this historical standard is referenced onwww.astm.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 StatesThis international standard was developed in accordanc