ASTM_D_5384_-_14.pdf

Designation:D538414Standard Test Methods forChlorine in Used Petroleum Products(Field Test KitMethod)1This standard is issued under the fixed designation D5384;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.Scope*1.1 These test methods cover the determination of chlorinein used oils,fuels,and related materials,including:crankcase,hydraulic,diesel,lubricating and fuel oils,and kerosene,allcontaining 25%(mass/mass)water.1.1.1 If the sample contains greater than 25%water,thesodium metal reacts preferentially with the water rather thanwith the halogenated organics in the oil.1.1.2 Bromide and iodide are also titrated and reported on amolar basis as chlorine.The method does not detect fluorinebecause AgF remains in the solution during the titration,whileAgI,AgBr,and AgCl precipitate out and can therefore bedetected.1.1.3 Some of the chlorinated organic compounds that havebeen shown to be detectable by this method includetrichloroethane,dichloroethane,trichlorobenzene,monochlorobenzene,chlorooctadecane,methylene chloride,perchloroethylene,Freon,and polychlorinated biphenyls.These nine compounds represent the major classes of chlori-nated compounds that are found in used oils.1.2 The entire analytical sequence,including sampling,sample pretreatment,chemical reactions,extraction,andquantification,is available in kit form using predispensed andencapsulated reagents.The overall objective is to provide asimple,easy to use procedure,permitting nontechnical person-nel to perform a test in or outside of the laboratory environmentin under 10 min.The test method also gives information to runthe test without a kit.1.2.1 Test Method A is preset to provide a greater than orless than result at 1000 mg/kg(ppm)total chlorine to meetregulatory requirements for used oils.1.2.2 Test Method B provides results over a range from 200to 4000 mg/kg total chlorine.1.3 For both test methods,positive bias will result fromsamples that contain greater than 3%(mass/mass)total sulfur.While a false negative result will not occur,other analyticalmethods should be used on high sulfur oils.1.4 Test Method B,Lower Limit of QuantitationIn theround-robin study to develop statistics for this test method,participants were asked to report results to the nearest100 mg kg.The lower limit of quantification could thereforeonly be determined to be in the range from 870 mg kg5to1180 mg kg5.1.5 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 limitations prior to use.Specific safetystatements are given in Sections 3,6,and 7.2.Referenced Documents2.1 ASTM Standards:2D4057 Practice for Manual Sampling of Petroleum andPetroleum Products2.2 Federal Regulation:40 CFR 261 Identification and Listing of Hazardous Waste33.Summary of Test Methods3.1 The oil sample(approximately 0.3 g)is dispersed in ahydrocarbon solvent and reacted with a mixture of metallicsodium catalyzed with naphthalene and diglyme at ambienttemperature.This process converts organic halogens to theirrespective sodium halides.Halides in the treated mixture,including those present prior to the reaction,are then extractedinto an aqueous buffer,which is then titrated with mercuricnitrate using diphenyl carbazone as the indicator.The end point1These test methods are under the jurisdiction of ASTM Committee D02 onPetroleum Products,Liquid Fuels,and Lubricants and are the direct responsibilityof Subcommittee D02.03 on Elemental Analysis.Current edition approved June 1,2014.Published July 2014.Originally approvedin 1995.Last previous edition approved in 2011 as D5384 11.DOI:10.1520/D538414.2For 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 U.S.Government Printing Office Superintendent of Documents,732 N.Capitol St.,NW,Mail Stop:SDE,Washington,DC 20401,http:/www.access.gpo.gov.*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 of the titration is the formation of the blue-violet mercurydiphenylcarbazone complex.3.1.1 Preset reagent quantities are used for Test MethodAsothat the final result is clearly determined to be either above orbelow 1000 mg/kg total chlorine.3.1.1.1 Analysis time is approximately ten minutes,and thenecessa