ASTM D7059-2009 3125 Standard Test Method for Determination of Methanol in Crude Oils by Multidimensional Gas Chromatography《用多维气相色谱法测定原油中甲醇的试验方法》.pdf
《ASTM D7059-2009 3125 Standard Test Method for Determination of Methanol in Crude Oils by Multidimensional Gas Chromatography《用多维气相色谱法测定原油中甲醇的试验方法》.pdf》由会员分享,可在线阅读,更多相关《ASTM D7059-2009 3125 Standard Test Method for Determination of Methanol in Crude Oils by Multidimensional Gas Chromatography《用多维气相色谱法测定原油中甲醇的试验方法》.pdf(15页珍藏版)》请在麦多课文档分享上搜索。
1、Designation: D7059 09Standard Test Method forDetermination of Methanol in Crude Oils byMultidimensional Gas Chromatography1This standard is issued under the fixed designation D7059; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, t
2、he 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. Scope*1.1 This test method covers the determination of methanolin crude oils by direct injection multidimensional ga
3、s chroma-tography in the concentration range of 15 to 900 ppm (m/m).The pooled limit of quantification (PLOQ) is 15 ppm (m/m).1.2 This test method is applicable only to crude oils con-taining less than or equal to 0.1 % (v/v) water.1.3 This test method has not been tested with crude oilsamples that
4、are solid or waxy, or both, at ambient tempera-tures.1.4 The values stated in SI units are to be regarded asstandard. Alternate units, in common usage, are also providedto increase clarity and aid the users of this test method.1.5 This standard does not purport to address all of thesafety concerns,
5、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:2D4006 Test Method for Water in Crude Oil by D
6、istillationD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4307 Practice for Preparation of Liquid Blends for Use asAnalytical StandardsD4928 Test Methods for Water in Crude Oils by Coulom-etric Karl Fischer TitrationD6596 Practice for Ampulization and Storage of Gasolineand Re
7、lated Hydrocarbon Materials3. Terminology3.1 Definitions:3.1.1 analytical column, nporous layer open tubular(PLOT) column with a stationary phase selective for oxygen-ates. It is used to resolve methanol from 1-propanol to provideaccurate quantitative results.3.1.2 cool-on-column injector, nan injec
8、tion port thatallows controlled injection of the sample at a temperature closeto or lower than the boiling point of the solvent into the gaschromatographic column or a liner within the injection portconnected to the column.3.1.2.1 DiscussionAfter the injection, the injection port isheated at a fixed
9、 rate to a temperature sufficiently high enoughto allow the transfer of sample components of interest from theinjection port to the part of the column located in the gaschromatograph (GC) oven.3.1.3 electronic pressure control, nelectronic pneumaticcontrol of carrier gas flows. It can be flow or pre
10、ssureprogrammed to speed up elution of components.3.1.4 low-volume connector, na special union for con-necting two lengths of tubing 1.6-mm inside diameter andsmaller; sometimes referred to as a zero dead-volume union.3.1.5 pre-column, na polydimethylsiloxane WCOT col-umn used to isolate the methano
11、l and 1-propanol and severallight hydrocarbons from the higher boiling portion of the crudeoil sample for transfer to the analytical column for furtherseparation and quantification.3.1.6 programmable temperature vaporizer (PTV), natemperature programmable injector similar to a cool-on-column injecto
12、r except that the sample is injected cool into aglass liner or insert instead of the WCOT (3.1.5) column andthen the temperature is programmed in a manner similar to theon-column injector.3.1.6.1 DiscussionThe liner may be replaced, as neces-sary, to remove non-volatile materials. This injector may
13、beoperated in low split mode or direct (no splitting) mode.3.1.7 split/splitless injector, na heated capillary inlet orsample introduction system that allows controlled splitting ofthe injected sample into two unequal portions, the smaller ofwhich goes to the capillary column, and the greater to a v
14、ent.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 Oct. 1, 2009. Published November 2009.Originallyapproved in 2004. Last previous e
15、dition approved in 2004 as D7059-041. DOI:10.1520/D7059-09.2For 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.1*
16、A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.3.1.7.1 DiscussionWhen the vent is closed, the entiresample enters the capillary column and the inlet is operated asa spl
17、itless injector. When the vent is open, the inlet is operatedin the split mode and only a portion of the sample reaches thecapillary column. The ratio of the split between the capillarycolumn and the vent is calculated as described in 3.1.7.2.3.1.7.2 split ratio, nin capillary gas chromatography, th
18、eratio of the total flow of carrier gas to the sample inlet versusthe flow of the carrier gas to the capillary column, expressedby:split ratio 5 S 1 C!/C (1)where:S = flow rate at the splitter vent, andC = flow rate at the column outlet.4. Summary of Test Method4.1 An internal standard, 1-propanol,
19、is added to the sample,which is then introduced into a gas chromatograph equippedwith two columns and a flow switching system between thetwo columns. The sample first passes through the polydimeth-ylsiloxane WCOT column that performs a pre-separation of themethanol and 1-propanol and eliminates unwa
20、nted hydrocar-bons. The methanol and 1-propanol are transferred to theanalytical PLOT column for oxygenates. While the methanoland 1-propanol are eluting from the analytical PLOT columnfor oxygenates, auxiliary carrier gas is used to elute higherboiling crude oil hydrocarbons from the pre-column, ei
21、ther inthe forward or backflush mode, to yield a stable baseline for thenext analysis.5. Significance and Use5.1 Methanol is used in production of crude oil to preventformation of gas hydrates. The presence of residual methanolin crude oils can lead to costly problems in refinery operations.6. Appar
22、atus6.1 ChromatographA multidimensional two-WCOT col-umn gas chromatographic system, capable of adequately re-solving methanol and the 1-propanol internal standard and ofeliminating hydrocarbon and other interferences, is requiredfor this analysis. Flow switching between the two specifiedWCOT column
23、s may be accomplished by either using a valveor pneumatic (pressure) switching to redirect flows. Theunwanted higher boiling hydrocarbons may be removed fromthe pre-column either by forward flush or backward flush. Thesystem requires that carrier gas flow controllers must becapable of precise contro
24、l for the typical pressures required.Such flow controllers are available on gas chromatographs.The precision of this test method was obtained using severalinstrument configurations described in 6.1.1-6.1.5. Other mul-tidimensional configurations may be used, provided that theymeet all of the require
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