ASTM_D_1091_-_11.pdf

Designation:D109111Standard Test Methods forPhosphorus in Lubricating Oils and Additives1This standard is issued under the fixed designation D1091;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.Scope*1.1 These test methods cover the determination of phospho-rus in unused lubricating oils and lubricating oil additives andtheir concentrates.The test methods are not restricted withrespect to the type of phosphorus compounds that may bepresentfor example,trivalent or pentavalent phosphoruscompounds,phosphines,phosphates,phosphonates,phospho-rus sulfides,and so forthsince all are quantitatively con-verted to an aqueous solution of orthophosphate ion byoxidation of the sample during the course of analysis.1.2 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.3 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:2D1193 Specification for Reagent WaterD4057 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 Performance3.Summary of Test Method3.1 Organic material in the sample is removed and thephosphorus is converted to phosphate ion by oxidation withsulfuric acid,nitric acid,and hydrogen peroxide.One of theseprocedures is then followed:SectionsOxidation of the Sample7 11Photometric(Molydivanado)Method12 18Gravimetric Method19 253.2 The photometric method is used where the phosphoruscontent is estimated to be under 2%,and the gravimetricmethod is used for phosphorus contents of 2%or over.4.Significance and Use4.1 Knowledge of the phosphorus content,and thus thephosphorus-containing additives,in a lubricating oil or addi-tive can be used to predict performance characteristics.Thistest method is suitable for most applications requiring thedetermination of phosphorus.5.Purity of Reagents5.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society wheresuch specifications are available.3Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.5.2 Purity of WaterUnless otherwise indicated,referencesto water shall be understood to mean reagent water as definedby Type II or Type III of Specification D1193.6.Sampling6.1 Obtain samples in accordance with the instructions inPractices D4057 or D4177.1These test methods are under the jurisdiction of ASTM Committee D02 onPetroleum Products,Liquid Fuels,and Lubricants and are the responsibility ofSubcommittee D02.03 on Elemental Analysis.Current edition approved June 1,2011.Published July 2011.Originally approvedin 1950.Last previous edition approved in 2005 as D109100(2005).DOI:10.1520/D1091-11.This test method has been adopted for use by government agencies to replaceMethod 5661 of Federal Test Method Standard No.791b.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.3Reagent Chemicals,American Chemical Society Specifications,AmericanChemical Society,Washington,D.C.For suggestions on the testing of reagents notlisted by the American Chemical Society,see Analar Standards for LaboratoryChemicals,BDH Ltd.,Poole,Dorset,U.K.,and the United States Pharmacopeiaand National Formulary,U.S.Pharmacopeial Convention,Inc.(USPC),Rockville,MD.*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 6.2 Take care that the test specimen is thoroughly represen-tative of the material to be tested and that the portion of thesample is thoroughly representative of the test unit.OXIDATION OF THE SAMPLE7.Scope7.1 This test method covers a procedure for removal oforganic material and subsequent conversion of phosphorus tophosphate ion in samples of unused lubricating oils,lubricatingoil additives,and their concentrates.8.Summary of Test Method8.1 Organic