1、Designation: D 2887 06aDesignation: 406An American National StandardStandard Test Method forBoiling Range Distribution of Petroleum Fractions by GasChromatography1, 2This standard is issued under the fixed designation D 2887; the number immediately following the designation indicates the year oforig
2、inal 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.This standard has been approved for use by agencies of the Department of D
3、efense.1. Scope*1.1 This test method covers the determination of the boilingrange distribution of petroleum products. The test method isapplicable to petroleum products and fractions having a finalboiling point of 538C (1000F) or lower at atmosphericpressure as measured by this test method. This tes
4、t method islimited to samples having a boiling range greater than 55C(100F), and having a vapor pressure sufficiently low to permitsampling at ambient temperature.1.2 This test method is not to be used for the analysis ofgasoline samples or gasoline components. These types ofsamples must be analyzed
5、 by Test Method D 3710.1.3 The values stated in SI units are to be regarded asstandard. The inch-pound units given in parentheses are forinformation only.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 t
6、his 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:3D86 Test Method for Distillation of Petroleum Products atAtmospheric PressureD 1160 Test Method for Distillation of Pe
7、troleum Productsat Reduced PressureD 2892 Test Method for Distillation of Crude Petroleum(15-Theoretical Plate Column)D 3710 Test Method for Boiling Range Distribution ofGasoline and Gasoline Fractions by Gas ChromatographyD 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4626
8、Practice for Calculation of Gas ChromatographicResponse FactorsD 6708 Practice for Statistical Assessment and Improve-ment of Expected Agreement Between Two Test Methodsthat Purport to Measure the Same Property of a MaterialE 260 Practice for Packed Column Gas ChromatographyE 355 Practice for Gas Ch
9、romatography Terms and Rela-tionshipsE 516 Practice for Testing Thermal Conductivity DetectorsUsed in Gas ChromatographyE 594 Practice for Testing Flame Ionization Detectors Usedin Gas or Supercritical Fluid Chromatography1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum
10、Products and Lubricants and is the direct responsibility of SubcommitteeD02.04.0H on Chromatographic Distribution Methods.Current edition approved Dec. 1, 2006. Published January 2007. Originallyapproved in 1973. Last previous edition approved in 2006 as D 288706.2This standard has been developed th
11、rough the cooperative effort betweenASTM and the Institute of Petroleum, London. The IP and ASTM logos imply thatthe ASTM and IP standards are technically equivalent, but their use does not implythat both standards are editorially identical.3For referenced ASTM standards, visit the ASTM website, www
12、.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*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive,
13、PO Box C700, West Conshohocken, PA 19428-2959, United States.3. Terminology3.1 DefinitionsThis test method makes reference to manycommon gas chromatographic procedures, terms, and relation-ships. Detailed definitions of these can be found in PracticesE 260, E 355, and E 594.3.2 Definitions of Terms
14、Specific to This Standard:3.2.1 area slicethe area, resulting from the integration ofthe chromatographic detector signal, within a specified reten-tion time interval. In area slice mode (see 6.3.2), peak detectionparameters are bypassed and the detector signal integral isrecorded as area slices of c
15、onsecutive, fixed duration timeintervals.3.2.2 corrected area slicean area slice corrected for base-line offset, by subtraction of the exactly corresponding areaslice in a previously recorded blank (non-sample) analysis.3.2.3 cumulative corrected areathe accumulated sum ofcorrected area slices from
16、the beginning of the analysis througha given retention time, ignoring any non-sample area (forexample, solvent).3.2.4 final boiling point (FBP)the temperature (corre-sponding to the retention time) at which a cumulative correctedarea count equal to 99.5 % of the total sample area under thechromatogr
17、am is obtained.3.2.5 initial boiling point (IBP)the temperature (corre-sponding to the retention time) at which a cumulative correctedarea count equal to 0.5 % of the total sample area under thechromatogram is obtained.3.2.6 slice ratethe time interval used to integrate thecontinuous (analog) chroma
18、tographic detector response duringan analysis. The slice rate is expressed in hertz (for example,integrations or slices per second).3.2.7 slice timethe time associated with the end of eachcontiguous area slice. The slice time is equal to the slicenumber divided by the slice rate.3.2.8 total sample a
19、reathe cumulative corrected area,from the initial area point to the final area point, where thechromatographic signal is considered to have returned tobaseline after complete sample elution.3.3 Abbreviations:3.3.1 Acommon abbreviation of hydrocarbon compounds isto designate the number of carbon atom
20、s in the compound. Aprefix is used to indicate the carbon chain form, while asubscripted suffix denotes the number of carbon atoms (forexample, normal decane = n-C10; isotetradecane = i-C14).4. Summary of Test Method4.1 The boiling range distribution determination by distilla-tion is simulated by th
21、e use of gas chromatography. A nonpolarpacked or open tubular (capillary) gas chromatographic col-umn is used to elute the hydrocarbon components of the samplein order of increasing boiling point. The column temperature israised at a reproducible linear rate and the area under thechromatogram is rec
22、orded throughout the analysis. Boilingpoints are assigned to the time axis from a calibration curveobtained under the same chromatographic conditions by ana-lyzing a known mixture of hydrocarbons covering the boilingrange expected in the sample. From these data, the boilingrange distribution can be
23、obtained.5. Significance and Use5.1 The boiling range distribution of petroleum fractionsprovides an insight into the composition of feedstocks andproducts related to petroleum refining processes. The gaschromatographic simulation of this determination can be usedto replace conventional distillation
24、 methods for control ofrefining operations. This test method can be used for productspecification testing with the mutual agreement of interestedparties.5.2 Boiling range distributions obtained by this test methodare essentially equivalent to those obtained by true boilingpoint (TBP) distillation (s
25、ee Test Method D 2892). They arenot equivalent to results from low efficiency distillations suchas those obtained with Test Method D86or D 1160.6. Apparatus6.1 ChromatographThe gas chromatograph used musthave the following performance characteristics:6.1.1 DetectorEither a flame ionization or a ther
26、malconductivity detector may be used. The detector must havesufficient sensitivity to detect 1.0 % dodecane with a peakheight of at least 10 % of full scale on the recorder underconditions prescribed in this test method and without loss ofresolution as defined in 9.3.1. When operating at this sensit
27、iv-ity level, detector stability must be such that a baseline drift ofnot more than 1 % of full scale per hour is obtained. Thedetector must be capable of operating continuously at atemperature equivalent to the maximum column temperatureemployed. Connection of the column to the detector must besuch
28、 that no temperature below the column temperature exists.NOTE 1It is not desirable to operate a thermal conductivity detector ata temperature higher than the maximum column temperature employed.Operation at higher temperature generally contributes to higher noiselevels and greater drift and can shor
29、ten the useful life of the detector.6.1.2 Column Temperature ProgrammerThe chromato-graph must be capable of linear programmed temperatureoperation over a range sufficient to establish a retention time ofat least 1 min for the IBP and to elute compounds up to aboiling temperature of 538C (1000F) bef
30、ore reaching theupper end of the temperature program. The programming ratemust be sufficiently reproducible to obtain retention timerepeatability of 0.1 min (6 s) for each component in thecalibration mixture described in 7.8.6.1.3 Cryogenic Column CoolingColumn starting tem-peratures below ambient w
31、ill be required if samples with IBPsof less than 93C (200F) are to be analyzed. This is typicallyprovided by adding a source of either liquid carbon dioxide orliquid nitrogen, controlled through the oven temperature cir-cuitry. Excessively low initial column temperature must beavoided to ensure that
32、 the stationary phase remains liquid. Theinitial temperature of the column should be only low enough toobtain a calibration curve meeting the specifications of themethod.6.1.4 Sample Inlet SystemThe sample inlet system mustbe capable of operating continuously at a temperature equiva-lent to the maxi
33、mum column temperature employed, or providefor on-column injection with some means of programming theentire column, including the point of sample introduction, up toD 2887 06a2the maximum temperature required. Connection of the columnto the sample inlet system must be such that no temperaturebelow t
34、he column temperature exists.6.1.5 Flow ControllersThe gas chromatograph must beequipped with mass flow controllers capable of maintainingcarrier gas flow constant to 61 % over the full operatingtemperature range of the column. The inlet pressure of thecarrier gas supplied to the gas chromatograph m
35、ust be suffi-ciently high to compensate for the increase in column back-pressure as the column temperature is raised. An inlet pressureof 550 kPa (80 psig) has been found satisfactory with thepacked columns described in Table 1. For open tubularcolumns, inlet pressures from 10 to 70 kPa (1.5 to 10 p
36、sig)have been found to be suitable.6.1.6 MicrosyringeA microsyringe is needed for sampleintroduction.NOTE 2Automatic sampling devices or other sampling means, such asindium encapsulation, can be used provided: the system can be operatedat a temperature sufficiently high to completely vaporize hydroc
37、arbonswith atmospheric boiling points of 538C (1000F), and the samplingsystem is connected to the chromatographic column avoiding any coldtemperature zones.6.2 ColumnAny column and conditions may be used thatprovide separation of typical petroleum hydrocarbons in orderof increasing boiling point and
38、 meet the column performancerequirements of 9.3.1 and 9.3.3. Successfully used columnsand conditions are given in Table 1.6.3 Data Acquisition System:6.3.1 RecorderA 0 to 1 mV range recording potentiom-eter or equivalent, with a full-scale response time of2sorlessmay be used.6.3.2 IntegratorMeans mu
39、st be provided for determiningthe accumulated area under the chromatogram. This can bedone by means of an electronic integrator or computer-basedchromatography data system. The integrator/computer systemmust have normal chromatographic software for measuring theretention time and areas of eluting pe
40、aks (peak detectionmode). In addition, the system must be capable of convertingthe continuously integrated detector signal into area slices offixed duration. These contiguous area slices, collected for theentire analysis, are stored for later processing. The electronicrange of the integrator/compute
41、r (for example, 1 V, 10 V) mustbe within the linear range of the detector/electrometer systemused. The system must be capable of subtracting the area sliceof a blank run from the corresponding area slice of a samplerun.NOTE 3Some gas chromatographs have an algorithm built into theiroperating softwar
42、e that allows a mathematical model of the baselineprofile to be stored in memory. This profile is automatically subtractedfrom the detector signal on subsequent sample analyses to compensate forany baseline offset. Some integration systems also store and automaticallysubtract a blank analysis from s
43、ubsequent analytical determinations.7. Reagents and Materials7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents conform to the specifications of the Committee onAnalytical Reagents of the American Chemical Society wher
44、esuch specifications are available.4Other grades may be used,provided it is first ascertained that the reagent is of sufficientlyhigh purity to permit its use without lessening the accuracy ofthe determination.7.2 Liquid Phase for ColumnsMethyl silicone gums andliquids provide the proper chromatogra
45、phic hydrocarbon elu-tion characteristics for this test method.7.3 Solid Support for Packed ColumnsChromatographicgrade diatomateous earth solid support material within aparticle size range from 60 to 100 sieve mesh size is recom-mended.7.4 Carrier GasHelium or nitrogen of high purity.(WarningHelium
46、 and nitrogen are compressed gases under4Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset
47、, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.TABLE 1 Typical Operating ConditionsPacked Columns 1 2 3 4 Open Tubular Columns 5 6 7Column length, m (ft) 1.2 (4) 1.5 (5) 0.5 (1.5) 0.6 (2) Column length (m) 7.5 5 10Column out
48、side diameter, mm(in.)6.4 (1/4) 3.2 (1/8) 3.2 (1/8) 6.4 (1/8) Column inner diameter (mm) 0.53 0.53 0.53Liquid phase OV-1 SE-30 UC-W98 SE-30 Stationary phase DB-1 HP-1 HP-1Percent liquid phase 3 5 10 10 Stationary phase thickness(m)1.5 0.88 2.65Support material SAGBPCPCCarrier gas nitrogen helium hel
49、iumSupport mesh size 60/80 60/80 80/100 60/80 Carrier gas flow rate, mL/min 30 12 12Initial column temperature, C 20 40 30 50 Initial column temperature, C 40 35 35Final column temperature, C 360 350 360 390 Final column temperature, C 340 350 350Programming rate,C/min 10 6.5 10 7.5 Programming rate, C/min 10 10 20Carrier gas helium helium N2helium Detector FID FID FIDCarrier gas flow, mL/min 40 30 25 60 Detector temperature, C 350 380 370Detector TC FID FID TC Injector temperature, C 340 cool on-column cool on-columnDetector temperatur
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