ASTM D5599-2000(2005) Standard Test Method for Determination of Oxygenates in Gasoline by Gas Chromatography and Oxygen Selective Flame Ionization Detection《气相色谱法和氧离子燃烧法测定气体氧化反应的标准.pdf
《ASTM D5599-2000(2005) Standard Test Method for Determination of Oxygenates in Gasoline by Gas Chromatography and Oxygen Selective Flame Ionization Detection《气相色谱法和氧离子燃烧法测定气体氧化反应的标准.pdf》由会员分享,可在线阅读,更多相关《ASTM D5599-2000(2005) Standard Test Method for Determination of Oxygenates in Gasoline by Gas Chromatography and Oxygen Selective Flame Ionization Detection《气相色谱法和氧离子燃烧法测定气体氧化反应的标准.pdf(8页珍藏版)》请在麦多课文档分享上搜索。
1、Designation: D 5599 00 (Reapproved 2005)An American National StandardStandard Test Method forDetermination of Oxygenates in Gasoline by GasChromatography and Oxygen Selective Flame IonizationDetection1This standard is issued under the fixed designation D 5599; the number immediately following the de
2、signation 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 revision or reapproval.1. Scope1.1 This test method covers a g
3、as chromatographic proce-dure for the quantitative determination of organic oxygenatedcompounds in gasoline having a final boiling point not greaterthan 220C and oxygenates having a boiling point limit of130C. It is applicable when oxygenates are present in the 0.1to 20 % by mass range.1.2 This test
4、 method is intended to determine the massconcentration of each oxygenate compound present in a gaso-line. This requires knowledge of the identity of each oxygenatebeing determined (for calibration purposes). However, theoxygen-selective detector used in this test method exhibits aresponse that is pr
5、oportional to the mass of oxygen.Itis,therefore, possible to determine the mass concentration ofoxygen contributed by any oxygenate compound in the sample,whether or not it is identified. Total oxygen content in agasoline may be determined from the summation of theaccurately determined individual ox
6、ygenated compounds. Thesummed area of other, uncalibrated or unknown oxygenatedcompounds present, may be converted to a mass concentrationof oxygen and summed with the oxygen concentration of theknown oxygenated compounds.1.3 The values stated in SI units are to be regarded as thestandard. The value
7、s given in parentheses are for informationonly.1.4 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 regu
8、latory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 1744 Test Method for Determination of Water in LiquidPetroleum Products by Karl Fischer Reagent3D 4175 Terminology Relating to Petroleum, PetroleumProducts, and LubricantsD 4307 Practice for Preparation of Liquid Blends for
9、 Use asAnalytical StandardsE 594 Practice for Testing Flame Ionization Detectors Usedin Gas or Supercritical Fluid ChromatographyE 1064 Test Method for Water in Organic Liquids byCoulometric Karl Fischer TitrationE 1510 Practice for Installing Fused Silica Open TubularCapillary Columns in Gas Chroma
10、tographs3. Terminology3.1 Definitions:3.1.1 independent reference standardscalibration samplesof the oxygenates which are purchased or prepared frommaterials independent of the quality control check standardsand used for intralaboratory accuracy.3.1.2 oxygenate, nan oxygen-containing compound, sucha
11、s an alcohol or ether, which may be used as a fuel or fuelsupplement. D 41753.1.3 quality control check standardscalibration samplesof the oxygenates for intralaboratory repeatability.4. Summary of Test Method4.1 An internal standard of a noninterfering oxygenate, forexample, 1,2-dimethoxyethane (et
12、hylene glycol dimethylether) is added in quantitative proportion to the gasolinesample. A representative aliquot of the sample and internalstandard is injected into a gas chromatograph equipped with acapillary column operated to ensure separation of the oxygen-ates. Hydrocarbons and oxygenates are e
13、luted from the col-umn, but only oxygenates are detected with the oxygen-selective flame ionization detector (OFID).Adiscussion of thisdetector is presented in Section 6.4.2 Calibration mixtures are used for determining the reten-tion times and relative mass response factors of the oxygenatesof inte
14、rest. Suggested calibrant materials are listed in 8.2.1This 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, 2005. Published Novembe
15、r 2005. Originallyapproved in 1994. Last previous edition approved in 2000 as D 5599 00.2For 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 Summa
16、ry page onthe ASTM website.3Withdrawn.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.4.3 The peak area of each oxygenate in the gasoline ismeasured relative to the peak area of the internal standard. Aquadratic least-squares fit of
17、the calibrated data of eachoxygenate is applied and the concentration of each oxygenatecalculated.NOTE 1While 1,2-dimethoxyethane has been found to be an appro-priate internal standard, other oxygenates may be used provided they arenot present in the sample and do not interfere with any compound ofi
18、nterest.5. Significance and Use5.1 In gasoline blending, the determination of organicoxygenated compounds is important. Alcohols, ethers, andother oxygenates are added to gasoline to increase the octanenumber and to reduce tailpipe emissions of carbon monoxide.They must be added in the proper concen
19、tration and ratios tomeet regulatory limitations and to avoid phase separation andproblems with engine performance or efficiency.5.2 This test method provides sufficient oxygen-to-hydro-carbon selectivity and sensitivity to allow determination ofoxygenates in gasoline samples without interference fr
20、om thebulk hydrocarbon matrix.6. Theory of OFID Operation6.1 The detection system selective for organic oxygenconsists of a cracking reactor, hydrogenating reactor (metha-nizer), and a flame ionization detector (FID). The crackingreactor, connected immediately after the gas chromatographiccapillary
21、column, consists of a Pt/Rh capillary tube. Carbonmonoxide (CO) is formed from compounds containing oxygenaccording to the following reaction:CxHyOzzCO 1y/2!H21x 2 z!C (1)6.2 An excess layer of carbon is created in the Pt/Rh tube ofthe cracking reactor from the introduction of hydrocarbonsfrom the s
22、ample or, if so designed, from a hydrocarbon (forexample, pentane or hexane) doping system, or both. This layerof carbon facilitates the cracking reaction and suppresseshydrocarbon response.6.3 The carbon monoxide formed in the cracking reactor isconverted to methane in the hydrogenating reactor acc
23、ording tothe following reaction:CO 1 3H2CH41 H2O (2)The CH4is subsequently detected with an FID.6.4 The methanizer consists either of a short porous layeropen tubular (PLOT) glass capillary tube internally coated withaluminum oxide with adsorbed nickel catalyst or stainless steeltubing containing a
24、nickel-based catalyst. It is installed withinor before the FID and is operated in the range from 350 to450C, depending on the instruments manufacturer.NOTE 2Gasolines with high sulfur content may cause a loss indetector sensitivity thereby limiting the number of samples that can beanalyzed before th
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