ASTM_D_3525_-_04_2016.pdf

Designation:D352504(Reapproved 2016)Standard Test Method forGasoline Diluent in Used Gasoline Engine Oils by GasChromatography1This standard is issued under the fixed designation D3525;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.Scope1.1 This test method covers the use of gas chromatographyto determine the amount of gasoline in used lubricating oilsarising from their use in gasoline engines.1.2 There is no limitation for the determination of thedilution range,provided that the amount of sample plusinternal standard is within the linear range of the gas chro-matograph detector.1.3 This test method is limited to gas chromatographsequipped with flame ionization detectors and programmableovens.NOTE1The use of other detectors and instrumentation has beenreported.However,the precision statement applies only when the instru-mentation specified is employed.1.4 The applicability of this method to gelled used engineoils has not been adequately investigated in order to ensurecompliance with the indicated repeatability and reproducibility.Gelled oils are defined as oils that develop structure onstanding,but that return to their original fluidity with lightagitation.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 requirements prior to use.2.Referenced Documents2.1 ASTM Standards:2E260 Practice for Packed Column Gas ChromatographyE355 Practice for Gas Chromatography Terms and Relation-shipsE594 Practice for Testing Flame Ionization Detectors Usedin Gas or Supercritical Fluid ChromatographyE1510 Practice for Installing Fused Silica Open TubularCapillary Columns in Gas Chromatographs3.Terminology3.1 Definitions:3.1.1 For definition of gas chromatography terms,refer toPractice E355.3.2 Definitions of Terms Specific to This Standard:3.2.1 fuel diluent,nin used oil analysis,unburned fuelcomponents that enter the engine crankcase cause dilution ofthe oil.3.2.1.1 DiscussionIn this method,the fuel diluent compo-nents being determined originate from gasoline.3.2.2 fuel dilution,nthe amount,expressed as apercentage,of gasoline found in engine lubricating oil.3.2.2.1 DiscussionFuel dilution may be the result ofengine wear or improper performance.3.3 Abbreviations:3.3.1 Acommon abbreviation of hydrocarbon compounds isto designate the number of carbon atoms in the compound.Aprefix is used to indicate the carbon chain form,while asubscripted suffix denotes the number of carbon atoms.Example:normal decanen-C10iso-tetradecanei-C144.Summary of Test Method4.1 A gas chromatographic technique is used for analyzingthe samples,by adding a known percentage of n-tetradecane asan internal standard,in order to determine the weight percentof gasoline fuel in the lubricating oil.A calibration curve ispreviously constructed which plots the gasoline fuel ton-tetradecane response ratio versus the weight percent ofgasoline fuel in lubricating oil mixtures containing a constantamount of internal standard.Mass percent of gasoline fuel inthe samples is determined by interpolation from the calibrationcurve.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products,Liquid Fuels,and Lubricants and is the direct responsibility ofSubcommittee D02.B0 on Automotive Lubricants.Current edition approved April 1,2016.Published May 2016.Originallyapproved in 1976.Last previous edition approved in 2010 as D3525 04(2010).DOI:10.1520/D3525-04R16.2For 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.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 5.Significance and Use5.1 Some fuel dilution of the engine oil may take placeduring normal operation.However,excessive fuel dilution is ofconcern in terms of possible performance problems.Thismethod provides a means to determine the magnitude of thefuel dilution,providing the user with the ability to predictperformance problems and to take appropriate action.6.Apparatus6.1 Gas ChromatographAny gas chromatograph may beused that has the following performance characteristics:6.1.1 DetectorOnly a flame ionization detector can beused in this method.The detector must have sufficient sensi-tivity to detect 1.0%n-tetradecane with a peak height of atleast 40%of full scale on the data acquisition devis