ASTM_D_5292_-_99_2014.pdf

Designation:D529299(Reapproved 2014)Standard Test Method forAromatic Carbon Contents of Hydrocarbon Oils by HighResolution Nuclear Magnetic Resonance Spectroscopy1This standard is issued under the fixed designation D5292;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 the aro-matic hydrogen content(Procedures A and B)and aromaticcarbon content(Procedure C)of hydrocarbon oils usinghigh-resolution nuclear magnetic resonance(NMR)spectrom-eters.Applicable samples include kerosenes,gas oils,mineraloils,lubricating oils,coal liquids,and other distillates that arecompletely soluble in chloroform at ambient temperature.Forpulse Fourier transform(FT)spectrometers,the detection limitis typically 0.1 mol%aromatic hydrogen atoms and 0.5 mol%aromaticcarbonatoms.Forcontinuouswave(CW)spectrometers,which are suitable for measuring aromatichydrogen contents only,the detection limit is considerablyhigher and typically 0.5 mol%aromatic hydrogen atoms.1.2 The reported units are mole percent aromatic hydrogenatoms and mole percent aromatic carbon atoms.1.3 This test method is not applicable to samples containingmore than 1 mass%olefinic or phenolic compounds.1.4 This test method does not cover the determination of thepercentage mass of aromatic compounds in oils since NMRsignals from both saturated hydrocarbons and aliphatic sub-stituents on aromatic ring compounds appear in the samechemical shift region.For the determination of mass or volumepercent aromatics in hydrocarbon oils,chromatographic,ormass spectrometry methods can be used.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 problems,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 precau-tionary statements are given in 7.2 and 7.3.2.Referenced Documents2.1 ASTM Standards:2D3238 Test Method for Calculation of Carbon Distributionand Structural Group Analysis of Petroleum Oils by then-d-M MethodD3701 Test Method for Hydrogen Content of AviationTurbine Fuels by Low Resolution Nuclear MagneticResonance SpectrometryD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsE386 Practice for Data Presentation Relating to High-Resolution Nuclear Magnetic Resonance(NMR)Spec-troscopy2.2 Energy Institute Methods:IP Proposed Method BD Aromatic Hydrogen and AromaticCarbon Contents of Hydrocarbon Oils by High ResolutionNuclear Magnetic Resonance Spectroscopy33.Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 aromatic carbon contentmole percent aromatic car-bon atoms or the percentage of aromatic carbon of the totalcarbon:aromatic carbon content5 1003(1)aromatic carbon atoms!/total carbon atoms!3.1.1.1 DiscussionFor example,the aromatic carbon con-tent of toluene is 100 (6 7)or 85.7 mol%aromatic carbonatoms.3.1.2 aromatic hydrogen contentmole percent aromatichydrogen atoms or the percentage of aromatic hydrogen of thetotal hydrogen:aromatic hydrogen content5 1003(2)aromatic hydrogen atoms!/total hydrogen atoms!1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products,Liquid Fuels,and Lubricants and is the direct responsibility ofSubcommittee D02.04.0F on Absorption Spectroscopic Methods.Current edition approved June 1,2014.Published July 2014.Originally approvedin 1992.Last previous edition approved in 2009 as D529299(2009).DOI:10.1520/D5292-99R14.2For 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 Energy Institute,61 New Cavendish St.,London,WIG 7AR,U.K.Copyright ASTM International,100 Barr Harbor Drive,PO Box C700,West Conshohocken,PA 19428-2959.United States1 3.1.2.1 DiscussionFor example,the aromatic hydrogencontent of toluene is 100 (5 8)or 62.5 mol%aromatichydrogen atoms.3.2 Definitions of chemical shift(reported in parts permillion(ppm),internal reference,spectral width,and otherNMR terminology used in this test method can be found inPractice E386.3.3 Chloroform-d refers to chloroform solvent in whichhydrogen is replaced by deuterium,the heavier isotope ofhydrogen.Chloroform-d is available from a variety of chemi-cal and isotope suppliers.4.Summary of Test Method4.1 Hydrogen(1H)nuclear magnetic resonance(NMR)spectraareobtainedonsolutionsofthesampleinchloroform-d,using a CW or pulse FT high-resolution NMRspectrometer.Carbon(13C)NM