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TM_D_874_
_13a_2018
Designation:D87413a(Reapproved 2018)British Standard 4716Standard Test Method forSulfated Ash from Lubricating Oils and Additives1This standard is issued under the fixed designation D874;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.Scope1.1 This test method covers the determination of the sul-fated ash from unused lubricating oils containing additives andfrom additive concentrates used in compounding.These addi-tives usually contain one or more of the following metals:barium,calcium,magnesium,zinc,potassium,sodium,and tin.The elements sulfur,phosphorus,and chlorine can also bepresent in combined form.1.2 Application of this test method to sulfated ash levelsbelow 0.02%by mass is restricted to oils containing ashlessadditives.The lower limit of the test method is 0.005%bymass sulfated ash.NOTE1This test method is not intended for the analysis of usedengine oils or oils containing lead.Neither is it recommended for theanalysis of nonadditive lubricating oils,for which Test Method D482 canbe used.NOTE2There is evidence that magnesium does not react the same asother alkali metals in this test.If magnesium additives are present,the datais interpreted with caution.NOTE3There is evidence that samples containing molybdenum cangive low results because molybdenum compounds are not fully recoveredat the temperature of ashing.1.3 Fatty acid methyl ester(FAME)conforming to EN14213 and EN 14214,when tested using this test method,wereshown to meet its precision.1.4 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.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,health,and environmental practices and deter-mine the applicability of regulatory limitations prior to use.1.6 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:2D482 Test Method for Ash from Petroleum ProductsD1193 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 Performance2.2 CEN Standards:3EN 14213 Heating FuelsFatty Acid Methyl Esters(FAME)Requirements and Test MethodsEN 14214 Automotive FuelsFatty Acid Methyl Esters(FAME)for Diesel EnginesRequirements and TestMethods3.Terminology3.1 Definitions:3.1.1 sulfated ash,nthe residue remaining after thesample has been carbonized,and the residue subsequentlytreated with sulfuric acid and heated to constant weight.4.Summary of Test Method4.1 The sample is ignited and burned until only ash andcarbon remain.After cooling,the residue is treated withsulfuric acid and heated at 775 C until oxidation of carbon is1This 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 April 1,2018.Published June 2018.Originallyapproved in 1946.Last previous edition approved in 2013 as D874 13a.DOI:10.1520/D0874-13AR18.In the IP,this test method is under the jurisdiction of the StandardizationCommittee.This test method has been approved by the sponsoring committees andaccepted by the cooperating societies in accordance with established procedures.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 European Committee for Standardization(CEN),AvenueMarnix 17,B-1000,Brussels,Belgium,http:/www.cen.eu.Copyright 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)Committee.1 complete.The ash is then cooled,re-treated with sulfuric acid,and heated at 775 C to constant wei