ASTM_D_3228_-_22.pdf

Designation:D322822Standard Test Method forTotal Nitrogen in Lubricating Oils and Fuel Oils by ModifiedKjeldahl Method1This standard is issued under the fixed designation D3228;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 This test method covers the determination of nitrogen inlubricating oils when present in the concentration from 0.03%to 0.10%by mass,and for the determination of nitrogen in fueloils when present in the concentration from 0.015%to 2.0%by mass.This test method is also applicable to the analysis ofadditive concentrates and additive packages.NOTE1This test method may not be applicable to certain materialscontaining NO or NN linkage.However,the samples used in thecooperative program to establish the precision of the test method werecompounded with currently available ashless additives containing nitro-gen.Complete recovery of the nitrogen present in these additives wasobtained.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,health,and environmental practices and deter-mine the applicability of regulatory limitations prior to use.For specific warning statements,see 7.6,7.9,and 9.8.1.4 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade(TBT)Committee.2.Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent WaterD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4175 Terminology Relating to Petroleum Products,LiquidFuels,and LubricantsD6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System PerformanceE200 Practice for Preparation,Standardization,and Storageof Standard and Reagent Solutions for Chemical Analysis3.Terminology3.1 Definitions:3.1.1 For definitions of terms used in this test method,referto Terminology D4175.3.2 Definitions of Terms Specific to This Standard:3.2.1 digestion,ntreating a sample with the use of heat orelevated pressures,or both,usually in the presence of chemicaladditives,to bring analytes of interest into solution or toremove interfering matrix components,or both.3.2.1.1 DiscussionIn this test method acid,a catalyst andheat are used to break the carbon nitrogen bonds to formammonium sulfate.3.2.2 lubricating oil,na liquid lubricant,usually compris-ing several ingredients,including a major portion of base oiland minor portions of various additives.3.2.3 titration,nquantitative chemical analysis methodused to determine the unknown concentration of a specifiedelement by reacting a solution prepared from the sample to beanalyzed with a known concentration and volume of specificreagent.3.2.3.1 DiscussionSensing electrodes or color indicatorscan be used to follow titrations if they respond to either thespecies being determined or the titrant ion.3.2.4 Total Kjeldahl Nitrogen(TKN),nthe sum of thenitrogen contained in the free ammonia and other nitrogencompounds which are converted to ammonium sulfate(NH4)2SO4 under the specified digestion conditions.4.Summary of Test Method4.1 The sample is digested in a mixture of concentratedsulfuric acid,potassium sulfate,and a catalyst of mercuric1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products,Liquid Fuels,and Lubricants and is the direct responsibility ofSubcommittee D02.03 on Elemental Analysis.Current edition approved Oct.1,2022.Published November 2022.Originallyapproved in 1973.Last previous edition approved in 2020 as D3228 20.DOI:10.1520/D3228-22.2For 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.*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 StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards,Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade(TBT)Co