1、Designation:D704004(Reapproved 2015)Standard Test Method forDetermination of Low Levels of Phosphorus in ILSAC GF 4and Similar Grade Engine Oils by Inductively CoupledPlasma Atomic Emission Spectrometry1This standard is issued under the fixed designation D7040;the number immediately following the de
2、signation 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.Scope1.1 This test method covers the quantit
3、ative determinationof phosphorus in unused lubricating oils,such as InternationalLubricant Standardization and Approval Committee(ILSAC)GF 4 and similar grade engine oils,by inductively coupledplasma atomic emission spectrometry.1.2 The precision statements are valid for dilutions in whichthe mass%s
4、ample in solvent is held constant in the range of1mass%to 5 mass%oil.1.3 The precision tables define the concentration rangescoveredintheinterlaboratorystudy(500 mg kgto800 mgkg).However,both lower and higher concentrationscan be determined by this test method.The low concentrationlimits are depende
5、nt on the sensitivity of the ICP instrumentand the dilution factor.The high concentration limits aredetermined by the product of the maximum concentrationdefined by the linear calibration curve and the sample dilutionfactor.1.4 The values stated in SI units are to be regarded as thestandard.The valu
6、es 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 regula
7、tory limitations prior to use.2.Referenced Documents2.1 ASTM Standards:2D4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4307 Practice for Preparation of Liquid Blends for Use asAnalytical StandardsD4927 Test Methods for Elemental Analysis of LubricantandAdditiveComponentsBarium
8、,Calcium,Phosphorus,Sulfur,and Zinc by Wavelength-DispersiveX-Ray Fluorescence SpectroscopyD4951 Test Method for Determination of Additive Elementsin Lubricating Oils by Inductively Coupled PlasmaAtomic Emission SpectrometryD5185 Test Method for Multielement Determination ofUsed and Unused Lubricati
9、ng 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 PerformanceD6792 Practice for Quality System in Petroleum Productsand Lubricants
10、Testing Laboratories3.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 pre
11、pared similarly.The solutions are introducedto the ICP instrument by a peristaltic pump(required).Bycomparing emission intensity of phosphorus in the test speci-men with emission intensities measured with the calibrationstandards and by applying the appropriate internal standard andbackground correc
12、tions,the concentrations of phosphorus inthe sample is calculated.4.Significance and Use4.1 This test method usually requires several minutes persample.Other test methods which can be used for the deter-mination of phosphorus in lubricating oils include WDXRFTest Method D4927 and ICPAES Test Methods
13、 D4951 andD5185.However,this test method provides more preciseresults than Test Methods D4951 or D5185.4.2 Lubricating oils are typically blends of additivepackages,and their specifications are also determined,in part,1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Prod
14、ucts,Liquid Fuels,and Lubricantsand is the direct responsibility ofSubcommittee D02.03 on Elemental Analysis.Current edition approved April 1,2015.Published June 2015.Originallyapproved in 2004.Last previous edition approved in 2010 as D7040 04(2010).DOI:10.1520/D7040-04R15.2For referenced ASTM stan
15、dards,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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2
16、959.United States1 by elemental composition.This test method can be used todetermine if unused lubricating oils meet specifications withrespect to elemental composition.4.3 It is expected that GF 4 grade engine oils marketed inthe years 2004 to 2005 will have a maximum phosphorusconcentration level of 500 mg kg to 800 mg kg.These limitsare required to minimize poisoning of automotive emissioncontrol catalysts by volatile phosphorus species.It is antici-pated that the later grades of oils may hav