ASTM_D_5622_-_95_2011.pdf

Designation:D562295(Reapproved 2011)Standard Test Methods forDetermination of Total Oxygen in Gasoline and MethanolFuels by Reductive Pyrolysis1This standard is issued under the fixed designation D5622;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 These test methods cover the quantitative determinationof total oxygen in gasoline and methanol fuels by reductivepyrolysis.1.2 Precision data are provided for 1.0 to 5.0 mass%oxygen in gasoline and for 40 to 50 mass%oxygen inmethanol fuels.1.3 Several types of instruments can be satisfactory forthese test methods.Instruments can differ in the way that theoxygen-containing species is detected and quantitated.How-ever,these test methods are similar in that the fuel is pyrolyzedin a carbon-rich environment.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:2D1298 Test Method for Density,Relative Density(SpecificGravity),or API Gravity of Crude Petroleum and LiquidPetroleum Products by Hydrometer MethodD4052 Test Method for Density,Relative Density,and APIGravity of Liquids by Digital Density MeterD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4815 Test Method for Determination of MTBE,ETBE,TAME,DIPE,tertiary-Amyl Alcohol and C1to C4Alco-hols in Gasoline by Gas Chromatography2.2 Other Standards:Clean Air Act(1992)33.Summary of Test Method3.1 Afuel specimen of 1 to 10 L is injected by syringe intoa 950 to 1300C high-temperature tube furnace that containsmetallized carbon.Oxygen-containing compounds are pyro-lyzed,and the oxygen is quantitatively converted into carbonmonoxide.3.2 A carrier gas,such as nitrogen,helium,or a helium/hydrogen mixture,sweeps the pyrolysis gases into any of fourdownstream systems of reactors,scrubbers,separators,anddetectors for the determination of the carbon monoxide con-tent,hence of the oxygen in the original fuel sample.The resultis reported as mass%oxygen in the fuel.4.Significance and Use4.1 These test methods cover the determination of totaloxygen in gasoline and methanol fuels,and they complementTest Method D4815,which covers the determination of severalspecific oxygen-containing compounds in gasoline.4.2 The presence of oxygen-containing compounds in gaso-line can promote more complete combustion,which reducescarbon monoxide emissions.The CleanAirAct(1992)requiresthat gasoline sold within certain,specified geographical areascontain a minimum percent of oxygen by mass(presently 2.7mass%)during certain portions of the year.The requirementcan be met by blending compounds such as methyl tertiarybutyl ether,ethyl tertiary butyl ether,and ethanol into thegasoline.These test methods cover the quantitative determina-tion of total oxygen which is the regulated parameter.1These test methods are under the jurisdiction of Committee D02 on PetroleumProducts and Lubricants and are the direct responsibility of Subcommittee D02.03on Elemental Analysis.Current edition approved May 1,2011.Published August 2011.Originallyapproved in 1994.Last previous edition approved in 2005 as D562295(2005).DOI:10.1520/D5622-95R11.2For 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.3Federal Register,Vol 57,No.24,Feb.5,1992,p.4408.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 5.Apparatus5.1 Oxygen Elemental Analyzer4,5,6,7,8A variety of instru-mentation can be satisfactory.However,the instrument mustreductively pyrolize the specimen and convert oxygen tocarbon monoxide.5.1.1 Test Method A4,8Helium carrier gas transports thepyrolysis products through a combination scrubber to removeacidic gases and water vapor.The products are then transportedto a molecular sieve gas chromatographic column where thecarbon monoxide is separated from the other pyrolysis prod-ucts.A thermal conductivity detector generates a response thatis proportional to the amount of carbon monoxide.5.1.2 Test Method B5,8Nitrogen carrier gas transports thepyrolysis products through a scrubber to remove water vapor.The pyrolysis products then flow through tandem infrareddetectors that measure carbon monoxide and carbon dioxide,respectively.5.1.3 Test Method C6,8A mixture of helium and hydrogen(95:5%