ASTM_D_7303_-_12.pdf

Designation:D730312Standard 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(10600),antimony(102300),barium(50800),calcium(2050 000),iron(10360),lithium(3003200),magnesium(3010 000),molybdenum(5022 000),phosphorus(502000),silicon(1015 000),sodium(301500),sulfur(160028 000),and zinc(3002200),all in mg/kg.Lowerlevels of elements may be determined by using larger sampleweights,and higher levels of elements may be determined byusing smaller amounts of sample or by using a larger dilutionfactor after sample dissolution.However,the test precision insuch cases has not been determined,and may be different thanthe 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.1.3 The values stated in SI units are to be regarded as thestandard.The values given in parentheses are for informationonly.1.4 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 10.2.Referenced Documents2.1 ASTM Standards:3D1193 Specification for Reagent WaterD3340 Test Method for Lithium and Sodium in LubricatingGreases by Flame PhotometerD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4951 Test Method for Determination of Additive Elementsin Lubricating Oils by Inductively Coupled PlasmaAtomic Emission SpectrometryD5185 Test Method for Determination ofAdditive Elements,Wear Metals,and Contaminants in Used Lubricating Oilsand Determination of Selected Elements in 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 PerformanceD6792 Practice for Quality System in Petroleum Productsand Lubricants Testing LaboratoriesD7260 Practice for Optimization,Calibration,and Valida-tion of Inductively Coupled Plasma-Atomic EmissionSpectrometry(ICP-AES)for Elemental Analysis of Petro-leum Products and Lubricants1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.03 on Elemental Analysis.Current edition approved June 1,2012.Published August 2012.Originallyapproved in 2006.Last previous edition approved in 2006 as D730306.DOI:10.1520/D7303-12.2Supporting data have been filed at ASTM International Headquarters and maybe obtained by requesting Research Report RR:D02-1608.3For 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 3.Terminology3.1 DefinitionsRefer to terminology identified in TestMethod D5185 for spectroscopy terms used in this standard.4.Summary of Test Method4.1 A weighed portion of the grease