ASTM_D_1839_-_14_2019.pdf

Designation:D183914(Reapproved 2019)Standard Test Method forAmyl Nitrate in Diesel Fuels1This standard is issued under the fixed designation D1839;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.Scope1.1 This test method covers the determination of 0.1%to0.5%by volume amyl nitrate in diesel fuels.NOTE1This test method has been used for the determination of hexylnitrate in diesel fuels,but has not been cooperatively tested for suchsamples.For the determination of hexyl nitrate,use standards containingnitrate esters of primary hexanol.Use a density of 0.97 in calculatingresults.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.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 Products3.Summary of Test Method3.1 This test method is based on the simultaneous hydroly-sis of the ester in 62.5%sulfuric acid and nitration ofm-xylenol by the nitric acid liberated.The nitroxylenol isdistilled from the reaction mixture and reacted with sodiumhydroxide to form the yellow sodium salt.Residual diesel fuelis removed by ether extraction.The color is measured spectro-photometrically at 452 nm,and the concentration of amylnitrate is determined by reference to a standard curve.4.Significance and Use4.1 In diesel fuel,the presence of alkyl nitrates such as amylnitrate,hexyl nitrate,or octyl nitrate causes a higher residuevalue than observed in untreated fuel,which can lead toerroneous conclusions as to the coke forming propensity of thefuel.The presence of such alkyl nitrate in the fuel can bedetermined using this test method.This test method can beused to determine the amount of amyl nitrate that has beenadded to diesel fuels to improve cetane number.This testmethod is applicable as a basis for judging compliance withspecifications covering amyl nitrate.5.Interferences5.1 Nitrate esters,inorganic nitrate ions,and nitrogen oxideswill interfere to give high results.6.Apparatus6.1 Absorption Cells,matched,having a 1.000 6 0.002 cmlight path.6.2 Distillate Collector,3borosilicate glass with standardtaper joints and sealed-in funnel(Fig.1).6.3 Electric Heating Mantle,to fit a 300 mL round-bottomflask,and having a variable transformer.6.4 Lunge-type Pipet,2 mL capacity.NOTE2A 2.5 mL hypodermic syringe,with scabbard,can be usedinstead of the Lunge pipet.6.5 Reflux Condenser(Allihn-type),borosilicate glass,300 mm long,with standard-taper joints.6.6 Round-Bottom Flask,of borosilicate glass and having a300 mL capacity.6.7 Separatory Funnel,Squibb-type,125 mL capacity.1This 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 15,2019.Published April 2019.Originallyapproved in 1961.Last previous edition approved in 20141 as D1839 14.DOI:10.1520/D1839-14R19.2For 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.3The sole source of supply of the apparatus known to the committee at this timeis obtainable from Corning Glass Co.,Corning,NY,Catalog No.3320.If you areaware of alternative suppliers,please provide this information to ASTM Interna-tional Headquarters.Your comments will receive careful consideration at a meetingof the responsible technical committee,1which you may attend.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 6.8 ShakingMachine,automatic,capableof250oscillations/min.6.9 Spectrophotometer,capable of measuring abs