ASTM_D_4047_-_13.pdf

Designation:D404713Designation:149/93Standard Test Method forPhosphorus in Lubricating Oils and Additives by QuinolinePhosphomolybdate Method1This standard is issued under the fixed designation D4047;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 Department of Defense.1.Scope*1.1 This test method covers the determination of 0.005 to10.0 mass%phosphorus in unused lubricating oil and additiveconcentrates.There is no reason to doubt its applicability tofiltered,used lubricating oils,but no systematic study of thisapplication has been made.1.2 The test method is applicable to samples containing anyof the phosphorus compounds in normal use.NOTE1This test method extends the scope of the previous version ofIP 149 and replaces IP 148 and the previous version of IP 149 as a refereemethod.1.3 This test method is free from most interferences becausethe high insolubility of the quinoline phosphomolybdate pre-cipitate leads to constant composition and freedom from mostadsorbed or occluded impurities,especially from cations whichwould otherwise interfere in the subsequent titration of theprecipitate.1.4 Barium,calcium,magnesium,zinc,iron,aluminum,alkali salts,citric acid and citrates,chromium up to 18 timesthe phosphorus content,and titanium up to 3.5 times do notinterfere with the test method.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 and health practices and determine the applica-bility of regulatory limitations prior to use.For specific hazardstatements,see 6.9.2.Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System Performance2.2 IP Standard:IP 148 Test Method for Phosphorous in Lubricating Oilsand Additives33.Summary of Test Method3.1 Additive concentrates are diluted with phosphorus-freewhite oil to produce a working blend.3.2 The sample is ignited with excess of zinc oxide wherebyphosphorus is converted to phosphate.The residue is dissolvedin hydrochloric acid and any sulfide formed is oxidized withpotassium bromate.Phosphorus is then precipitated as quino-line phosphomolybdate and determined volumetrically byaddition of excess standard alkali and back titration withstandard acid.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.5.Apparatus5.1 Silica Crucibles,40-mm internal diameter at the top and40 mm in height.The internal surface should be smooth andfree from pitting.5.2 Muffle Furnace,capable of maintaining a temperature ofapproximately 700C,and fitted with ports to allow aircirculation.1This 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 15,2013.Published August 2013.Originallyapproved in 1981.Last previous edition approved in 2011 as D4047 00(2011).DOI:10.1520/D4047-13.2For 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 Energy Institute,61 New Cavendish St.,London,WIG 7AR,U.K.,http:/www.energyinst.org.uk.*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 5.3 Beakers,25-mL capacity.5.4 Filtering Apparatus,a filter flask of capacity 500 mL,provided with a glass crucible adapter fitted in a rubber bungtogether with a rubber sleeve.5.5 Gooch Crucible,porcelain,35 mm diameter at the top,or a filter funnel fitted with a porcelain filter disk of approxi-mately 20 mm diameter.5.6 Filter Pad,approximately 20 mm diameter.6.Reagents and Materials6.1 Purity of ReagentsReagent grade chemicals shall beused in all tests.Unless otherwise indicated,it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.4Other grades may beused,provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.6.2 Pu