ASTM_D_4629_-_17.pdf

Designation:D462917Designation:379/88Standard Test Method forTrace Nitrogen in Liquid Hydrocarbons by Syringe/InletOxidative Combustion and Chemiluminescence Detection1This standard is issued under the fixed designation D4629;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.Scope*1.1 This test method covers the determination of the tracetotal nitrogen naturally found in liquid hydrocarbons boiling inthe range from approximately 50 C to 400 C,with viscositiesbetween approximately 0.2 cSt and 10 cSt(mm2/s)at roomtemperature.This test method is applicable to naphthas,distillates,and oils containing 0.3 mg kg to 100 mg kg totalnitrogen.For liquid hydrocarbons containing more than100 mgkg total nitrogen,Test Method D5762 can be moreappropriate.This test method has been successfully applied,during interlaboratory studies,to sample types outside therange of the scope by dilution of the sample in an appropriatesolvent to bring the total nitrogen concentration and viscosityto within the range covered by the test method.However,it isthe responsibility of the analyst to verify the solubility of thesample in the solvent and that direct introduction of the dilutedsample by syringe into the furnace does not cause low resultsdue to pyrolysis of the sample or solvent in the syringe needle.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 and health practices and determine the applica-bility of regulatory limitations prior to use.See 6.2,6.4,6.5,6.9,and Section 7.1.4 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:2D1298 Test Method for Density,Relative Density,or APIGravity of Crude Petroleum and Liquid Petroleum Prod-ucts by Hydrometer MethodD4052 Test Method for Density,Relative Density,and APIGravity of Liquids by Digital Density MeterD5762 Test Method for Nitrogen in Liquid Hydrocarbons,Petroleum and Petroleum Products by Boat-Inlet Chemi-luminescenceD6299 Practice for Applying Statistical Quality Assuranceand Control Charting Techniques to Evaluate AnalyticalMeasurement System Performance3.Summary of Test Method3.1 The sample of liquid petroleum hydrocarbon is intro-duced either by syringe or boat inlet system,into a stream ofinert gas(helium or argon).The sample is vaporized andcarried to a high temperature zone where oxygen is introducedand organically bound nitrogen is converted to nitric oxide(NO).The NO contacts ozone,and is converted to excitednitrogen dioxide(NO2).The light emitted as the excited NO2decays is detected by a photomultiplier tube and the resultingsignal is a measure of the nitrogen contained in the sample.4.Significance and Use4.1 Some process catalysts used in petroleum and chemicalrefining may be poisoned when even trace amounts of nitrog-enous materials are contained in the feedstocks.This testmethod can be used to determine bound nitrogen in processfeeds and may also be used to control nitrogen compounds infinished products.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 Dec.15,2017.Published February 2018.Originallyapproved in 1986.Last previous edition approved in 2017 as D4629 12(2017).DOI:10.1520/D4629-17.2For 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 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 5.Apparatus5.1 Furnace,electric,held at a temperature sufficient tovolatilize and pyrolyze all of the sample and oxidize theorg