ASTM_D_874_-_13a.pdf

Designation:D87413aBritish 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 Department of Defense.1.Scope*1.1 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 mass%is restricted to oils containing ashlessadditives.The lower limit of the test method is 0.005 mass%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 and health practices and determine the applica-bility of regulatory limitations prior to use.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 ashthe residue remaining after the samplehas been carbonized,and the residue subsequently treated withsulfuric 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 775C until oxidation of carbon iscomplete.The ash is then cooled,re-treated with sulfuric acid,and heated at 775C to constant weight.5.Significance and Use5.1 The sulfated ash can be used to indicate the concentra-tion of known metal-containing additives in new oils.Whenphosphorus is absent,barium,calcium,magnesium,sodium1This 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 Sept.1,2013.Published September 2013.Originallyapproved in 1946.Last previous edition approved in 2013 as D874 13.DOI:10.1520/D0874-13A.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-CENELECManagement Centre),Avenue Marnix 17,B-1000,Brussels,Belgium,http:/www.cenorm.be.*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 and potassium are converted to their sulfates and tin(stannic)and zinc to their oxides(Note 4).Sulfur and chlorine do notinterfere,but when phosphorus is present with metals,itremains partially or wholly in the sulfated ash as metalphosphates.NOTE4Since zinc sulfate slowly decomposes to its oxide at theignition temperature specified in the test method,samples containing zinccan give variable results