1、Designation: D2887 13Designation: 406Standard Test Method forBoiling Range Distribution of Petroleum Fractions by GasChromatography1,2This standard is issued under the fixed designation D2887; the number immediately following the designation indicates the year oforiginal adoption or, in the case of
2、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.This standard has been approved for use by agencies of the Department of Defense.1. Scope*1.1 This test meth
3、od 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 test method islimited to samples havi
4、ng a boiling range greater than 55.5C(100F), and having a vapor pressure sufficiently low to permitsampling at ambient temperature.NOTE 1Since a boiling range is the difference between twotemperatures, only the constant of 1.8F/C is used in the conversion ofthe temperature range from one system of u
5、nits to another.1.1.1 Procedure A (Sections 6-14)Allows a larger selec-tion of columns and analysis conditions such as packed andcapillary columns as well as a Thermal Conductivity Detectorin addition to the Flame Ionization Detector. Analysis timesrange from 14 to 60 min.1.1.2 Procedure B (Sections
6、 15-23)Is restricted to only 3capillary columns and requires no sample dilution. In addition,Procedure B is used not only for the sample types described inProcedure A but also for the analysis of samples containingbiodiesel mixtures B5, B10, and B20. The analysis time, whenusing Procedure B (Acceler
7、ated D2887), is reduced to about 8min.1.2 This test method is not to be used for the analysis ofgasoline samples or gasoline components. These types ofsamples must be analyzed by Test Method D3710.1.3 The values stated in SI units are to be regarded asstandard. The inch-pound units given in parenthe
8、ses 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 this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations
9、prior to use.2. Referenced Documents2.1 ASTM Standards:3D86 Test Method for Distillation of Petroleum Products atAtmospheric PressureD1160 Test Method for Distillation of Petroleum Products atReduced PressureD2892 Test Method for Distillation of Crude Petroleum(15-Theoretical Plate Column)D3710 Test
10、 Method for Boiling Range Distribution of Gaso-line and Gasoline Fractions by Gas ChromatographyD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4626 Practice for Calculation of Gas ChromatographicResponse FactorsD6708 Practice for Statistical Assessment and Improvementof Expect
11、ed Agreement Between Two Test Methods thatPurport to Measure the Same Property of a MaterialE260 Practice for Packed Column Gas ChromatographyE355 Practice for Gas Chromatography Terms and Relation-shipsE516 Practice for Testing Thermal Conductivity DetectorsUsed in Gas ChromatographyE594 Practice f
12、or Testing Flame Ionization Detectors Usedin Gas or Supercritical Fluid Chromatography1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.04.0H on Chromatographic Distribution Methods.Current editio
13、n approved May 1, 2013. Published June 2013. Originallyapproved in 1973. Last previous edition approved in 2012 as D288712. DOI:10.1520/D2887-13.2This standard has been developed through the cooperative effort betweenASTM International and the Energy Institute, London. The EI and ASTMInternational l
14、ogos imply that the ASTM International and EI standards aretechnically equivalent, but does not imply that both standards are editoriallyidentical.3For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandard
15、s volume information, refer to the standards Document Summary page onthe ASTM website.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States13. Terminology3.1 DefinitionsThis t
16、est method makes reference to manycommon gas chromatographic procedures, terms, and relation-ships. Detailed definitions of these can be found in PracticesE260, E355, and E594.3.2 Definitions of Terms Specific to This Standard:3.2.1 area slice, nthe area, resulting from the integrationof the chromat
17、ographic detector signal, within a specifiedretention time interval. In area slice mode (see 6.3.2), peakdetection parameters are bypassed and the detector signalintegral is recorded as area slices of consecutive, fixed durationtime intervals.3.2.2 corrected area slice, nan area slice corrected forb
18、aseline offset, by subtraction of the exactly correspondingarea slice in a previously recorded blank (non-sample) analy-sis.3.2.3 cumulative corrected area, nthe accumulated sum ofcorrected area slices from the beginning of the analysis througha given retention time, ignoring any non-sample area (fo
19、rexample, solvent).3.2.4 final boiling point (FBP), nthe temperature (corre-sponding to the retention time) at which a cumulative correctedarea count equal to 99.5 % of the total sample area under thechromatogram is obtained.3.2.5 initial boiling point (IBP), nthe temperature (corre-sponding to the
20、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 rate, nthe time interval used to integrate thecontinuous (analog) chromatographic detector response duringan analysis. The slice rate is expressed in hertz
21、(for example,integrations or slices per second).3.2.7 slice time, nthe 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 area, nthe cumulative corrected area,from the initial area point to the final area
22、 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 atoms in the compound. Aprefix is used to indicate the carbon chain form, while as
23、ubscripted 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 the use of gas chromatography. A nonpolarpacked or open tubular (capillary) gas
24、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 recorded throughout the analysis. Boilingpoints are assigned to the time axis fro
25、m 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 obtained.4.2 Procedure A and Procedure B yield essentially the sameresults. Se
26、e Sections 14 and 23, and the accompanying researchreports.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 determinati
27、on can be usedto replace conventional distillation 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 o
28、btained by true boilingpoint (TBP) distillation (see Test Method D2892). They are notequivalent to results from low efficiency distillations such asthose obtained with Test Method D86 or D1160.5.3 Procedure B was tested with biodiesel mixtures andreports the Boiling Point Distribution of FAME esters
29、 ofvegetable and animal origin mixed with ultra low sulfur diesel.Procedure A6. Apparatus6.1 ChromatographThe gas chromatograph used musthave the following performance characteristics:6.1.1 DetectorEither a flame ionization or a thermalconductivity detector may be used. The detector must havesuffici
30、ent 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 sensitiv-ity level, detector stability must be such that a baseline drift
31、 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 that no temperature below the column temperature exists.NOTE 2It i
32、s 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 shorten the useful life of the detector.6.1.2 Column Temperature Progra
33、mmerThe 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) before reaching theupper end of the temperature program. The programmi
34、ng 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 will be required if samples with IBPsof less than 93C (200F) are to
35、be analyzed. This is typicallyD2887 132provided 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 the stationary phase remains liquid. Theinitial temperatu
36、re 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 maximum column temperature employed, or providefor on-column i
37、njection with some means of programming theentire column, including the point of sample introduction, up tothe maximum temperature required. Connection of the columnto the sample inlet system must be such that no temperaturebelow the column temperature exists.6.1.5 Flow ControllersThe gas chromatogr
38、aph 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 must be suffi-ciently high to compensate for the increase in column ba
39、ck-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 psig)have been found to be suitable.6.1.6 MicrosyringeA microsyringe i
40、s needed for sampleintroduction.NOTE 3Automatic 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 hydrocarbonswith atmospheric boiling points of 538C (1000F), and the sampli
41、ngsystem 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 meet the column performancerequirements of 9.3.1 and 9.3.3. Successf
42、ully used columnsand conditions are given in Table 1.6.3 Data Acquisition System:6.3.1 RecorderA0 to 1 mV range recording potentiometeror equivalent, with a full-scale response time of2sorless maybe used.6.3.2 IntegratorMeans must be provided for determiningthe accumulated area under the chromatogra
43、m. 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 peaks (peak detectionmode). In addition, the system must be capable of con
44、vertingthe 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/computer (for example, 1 V, 10 V) mustbe within the linear range of the detecto
45、r/electrometer systemused. The system must be capable of subtracting the area sliceof a blank run from the corresponding area slice of a samplerun.NOTE 4Some gas chromatographs have an algorithm built into theiroperating software that allows a mathematical model of the baselineprofile to be stored i
46、n 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 subsequent analytical determinations.7. Reagents and Materials7.1 Purity
47、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 wheresuch specifications are available.4Other grades may be used,4Reagent Ch
48、emicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the testing of reagents notlisted by the American Chemical Society, see Annual Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand Natio
49、nal 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 outside 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 helium
