ASTM D5986-1996(2006) Standard Test Method for Determination of Oxygenates Benzene Toluene C8-C 12 Aromatics and Total Aromatics in Finished Gasoline by Gas Chromatography Fourier .pdf
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1、Designation: D 5986 96 (Reapproved 2006)An American National StandardStandard Test Method forDetermination of Oxygenates, Benzene, Toluene, C8C12Aromatics and Total Aromatics in Finished Gasoline by GasChromatography/Fourier Transform Infrared Spectroscopy1This standard is issued under the fixed des
2、ignation D 5986; 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 (e) indicates an editorial change since the last revisi
3、on or reapproval.1. Scope1.1 This test method covers the quantitative determinationof oxygenates: methyl-t-butylether (MTBE), di-isopropyl ether(DIPE), ethyl-t-butylether (ETBE), t-amylmethyl ether(TAME), methanol (MeOH), ethanol (EtOH), 2-propanol (2-PrOH), t-butanol (t-BuOH), 1-propanol (1-PrOH),
4、2-butanol(2-BuOH), i-butanol (i-BuOH), 1-butanol (1-BuOH); benzene,toluene and C8C12aromatics, and total aromatics in finishedmotor gasoline by gas chromatography/Fourier Transforminfrared spectroscopy (GC/FTIR).1.2 This test method covers the following concentrationranges: 0.120 volume % per compon
5、ent for ethers andalcohols; 0.12 volume % benzene; 115 volume % fortoluene, 1040 volume % total (C6C12) aromatics.1.3 The method has not been tested by ASTM for refineryindividual hydrocarbon process streams, such as reformates,fluid catalytic cracking naphthas, etc., used in blending ofgasolines.1.
6、4 SI units of measurement are preferred and used through-out this test method.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 deter
7、mine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 1298 Test Method for Density, Relative Density (SpecificGravity), or API Gravity of Crude Petroleum and LiquidPetroleum Products by Hydrometer MethodD 4052 Test Method for Density and Relative
8、 Density ofLiquids by Digital Density MeterD 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4307 Practice for Preparation of Liquid Blends for Use asAnalytical Standards3. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 aromaticsrefers to any organic compou
9、nd contain-ing a benzene or naphthalene ring.3.1.2 calibrated aromatic componentin this test method,refers to the individual aromatic components which have aspecific calibration.3.1.3 cool on-column injectorin gas chromatography,adirect sample introduction system which is set at a temperatureat or b
10、elow the boiling point of solutes or solvent on injectionand then heated at a rate equal to or greater than the column.Normally used to eliminate boiling point discrimination oninjection or to reduce adsorption, or both, on glass liners withininjectors. The sample is injected directly into the head
11、of thecapillary column tubing or retention gap.3.1.4 Gram-Schmidt chromatograma nonselective sum-mation of total intensity from a spectral scan per unit timewhich resembles in profile a flame ionization detector chro-matogram.3.1.5 retention gapin gas chromatography, refers to adeactivated precolumn
12、 which acts as a zone of low retentionpower for reconcentrating bands in space. The polarity of theprecolumn must be similar to that of the analytical column.3.1.6 selective wavelength chromatogram (SWC)in thistest method, refers to a selective chromatogram obtained bysumming the spectral intensity
13、in a narrow spectral wavelengthor frequency range as a function of elution time which isunique to the compound being quantitated.3.1.7 uncalibrated aromatic componentin this testmethod, refers to individual aromatics for which a calibration isnot available and whose concentrations are estimated from
14、 theresponse factor of a calibrated aromatic component.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.04.0L on Gas Chromatography Methods.Current edition approved Nov. 1, 2006. Published Januar
15、y 2007. Originallyapproved in 1996. Last previous edition approved in 2001 as D 5986 96 (2001).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 Documen
16、t Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.1.8 wall coated open tubular (WCOT)a type of capil-lary column prepared by coating or bonding the inside wall ofthe capillary with a thin film of sta
17、tionary phase.4. Summary of Test Method4.1 A gas chromatograph equipped with a methylsiliconeWCOT column is interfaced to a Fourier transform infraredspectrometer. The sample is injected through a cool on-columninjector capable of injecting a small sample size withoutoverloading the column.4.2 Calib
18、ration is performed using mixtures of specifiedpure oxygenates and aromatic hydrocarbons on a mass basis.Volume % data is calculated from the densities of the indi-vidual components and the density of the sample. Multipointcalibrations consisting of at least five levels and bracketing theconcentrati
19、on of the specified individual aromatics is required.Unidentified aromatic hydrocarbons present which have notbeen specifically calibrated for are quantitated using theresponse factor of 1,2,3,5-tetramethylbenzene and summedwith the other calibrated aromatic components to obtain a totalaromatic conc
20、entration of the sample.4.3 Specified quality control mixture(s) are analyzed tomonitor the performance of the calibrated GC/FTIR system.5. Significance and Use5.1 Test methods to determine oxygenates, benzene, and thearomatic content of gasoline are necessary to assess productquality and to meet ne
21、w fuel regulations.5.2 This test method can be used for gasolines that containoxygenates (alcohols and ethers) as additives. It has beendetermined that the common oxygenates found in finishedgasoline do not interfere with the analysis of benzene and otheraromatics by this test method.6. Apparatus6.1
22、 Gas Chromatograph:6.1.1 System equipped with temperature programmable gaschromatograph suitable for cool-on-column injections. Theinjector must allow the introduction of small (for example, 0.1L) sample sizes at the head of the WCOT column or aretention gap. An autosampler is mandatory.6.1.2 WCOT c
23、olumn containing a methylsilicone stationaryphase which elutes the aromatic hydrocarbons according totheir boiling points.Acolumn containing a relatively thick filmof stationary phase, such as 4 to 5 m, is recommended toprevent column sample overload.6.2 FTIR Spectrometer:6.2.1 This test method requ
24、ires a light-pipe GC/FTIR sys-tem (Fig. 1). No data have been acquired with matrix-isolationor other deposition type systems.6.2.2 The spectrometer must be equipped with a mercury-cadmium-telluride (MCT) detector capable of detecting from atleast 4000 cm-1 to 550 cm-1.6.2.3 The lower limit of 550 cm
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