ASTM_D_129_-_13.pdf

Designation:D12913British Standard 4454Designation:61/99Standard Test Method forSulfur in Petroleum Products(General High PressureDecomposition Device Method)1This standard is issued under the fixed designation D129;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 sulfur inpetroleum products,including lubricating oils containingadditives,additive concentrates,and lubricating greases thatcannot be burned completely in a wick lamp.The test methodis applicable to any petroleum product sufficiently low involatility that it can be weighed accurately in an open sampleboat and containing at least 0.1%sulfur.NOTE1This test method is not applicable to samples containingelements that give residues,other than barium sulfate,which are insolublein dilute hydrochloric acid and would interfere in the precipitation step.These interfering elements include iron,aluminum,calcium,silicon,andlead which are sometimes present in greases,lube oil additives,or additiveoils.Other acid insoluble materials that interfere are silica,molybdenumdisulfide,asbestos,mica,and so forth.The test method is not applicable toused oils containing wear metals,and lead or silicates from contamination.Samples that are excluded can be analyzed by Test Method D1552.1.2 This test method is applicable to samples with the sulfurin the range 0.09 to 5.5 mass%.1.3 The values stated in SI units are to be regarded asstandard.No other units of measurement are included in thisstandard.1.4 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:2D1193 Specification for Reagent WaterD1552 Test Method for Sulfur in Petroleum Products(High-Temperature Method)D6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System PerformanceE144 Practice for Safe Use of Oxygen Combustion Bombs3.Summary of Test Method3.1 The sample is oxidized by combustion in a high pressuredecomposition device containing oxygen under pressure.Thesulfur,as sulfate in the high pressure decomposition devicewashings,is determined gravimetrically as barium sulfate.3.2(WarningStrict adherence to all of the provisionsprescribed hereafter ensures against explosive rupture of thehigh pressure decomposition device,or a blow-out,providedthe high pressure decomposition device is of proper design andconstruction and in good mechanical condition.It is desirable,however,that the high pressure decomposition device beenclosed in a shield of steel plate at least 13 mm thick,orequivalent protection be provided against unforeseeable con-tingencies.)3.3(WarningInitial testing and periodic examination ofthe pressure vessel is essential to ensure its fitness for service.This is particularly important if the pressure vessel has beendropped and has any obvious signs of physical damage.)1This 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 June 15,2013.Published August 2013.Originallyapproved in 1922.Last previous edition approved in 2011 as D129 11.DOI:10.1520/D0129-13.This test method was adopted as a joint ASTM-IP standard in 1964.In the IP,this test method is under the jurisdiction of the StandardizationCommittee.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 States1 4.Apparatus and Materials4.1 High Pressure Decomposition Device(see Note 2),3having a capacity of not less than 300 mL,so constructed thatit will not leak during the test and that quantitative recovery ofthe liquids from the high pressure decomposition device maybe achieved readily.The inner surface of the high pressuredecomposition device may be made of stainless steel or anyother material that will not be affected by the combustionprocess or products.Materials used in the high pressuredecomposition device assembly,such as the head gasket andlead-wire insulation,shall be resistant to heat and chemicalaction,and shall not undergo any reaction that will affe