1、Designation: D2887 14Designation: 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 U.S. Department of Defense.1. Scope*1.1 This test
3、 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 test method islimited to samples
4、 having 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
5、 of units to another.1.1.1 Procedure A (Sections 614)Allows a largerselection of columns and analysis conditions such as packedand capillary columns as well as a Thermal ConductivityDetector in addition to the Flame Ionization Detector. Analysistimes range from 14 to 60 min.1.1.2 Procedure B (Sectio
6、ns 1523)Is restricted to only3 capillary columns and requires no sample dilution. Inaddition, Procedure B is used not only for the sample typesdescribed in Procedure A but also for the analysis of samplescontaining biodiesel mixtures B5, B10, and B20. The analysistime, when using Procedure B (Accele
7、rated D2887), is reducedto about 8 min.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 parenth
8、eses 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 Tes
10、t Method for Boiling Range Distribution of Gaso-line and Gasoline Fractions by Gas Chromatography(Withdrawn 2014)4D4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4626 Practice for Calculation of Gas ChromatographicResponse FactorsD6708 Practice for Statistical Assessment and Im
11、provementof Expected 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 Chromatogra
12、phy1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.04.0H on Chromatographic Distribution Methods.Current edition approved Oct. 1, 2014. Published December 2014. Originallyapproved
13、 in 1973. Last previous edition approved in 2013 as D2887 12. DOI:10.1520/D2887-14.2This standard has been developed through the cooperative effort betweenASTM International and the Energy Institute, London. The EI and ASTMInternational logos imply that the ASTM International and EI standards aretec
14、hnically 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 ASTMStandards volume information, refer to the standards Document Summary
15、page onthe ASTM website.4The last approved version of this historical standard is referenced onwww.astm.org.*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 States1E594 Practice
16、 for Testing Flame Ionization Detectors Usedin Gas or Supercritical Fluid Chromatography3. Terminology3.1 DefinitionsThis test 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
17、.2 Definitions of Terms Specific to This Standard:3.2.1 area slice, nthe area, resulting from the integrationof the chromatographic detector signal, within a specifiedretention time interval. In area slice mode (see 6.3.2), peakdetection parameters are bypassed and the detector signalintegral is rec
18、orded as area slices of consecutive, fixed durationtime intervals.3.2.2 corrected area slice, nan area slice corrected forbaseline 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
19、 ofcorrected area slices from the beginning of the analysis througha given retention time, ignoring any non-sample area (forexample, 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 tota
20、l sample area under thechromatogram is obtained.3.2.5 initial boiling point (IBP), nthe 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 rate, nthe time interval used to
21、integrate thecontinuous (analog) chromatographic detector response duringan analysis. The slice rate is expressed in hertz (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 divi
22、ded by the slice rate.3.2.8 total sample area, nthe 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 compo
23、unds isto designate the number of carbon atoms 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 dete
24、rmination by distilla-tion is simulated by the 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 r
25、ate and the area under thechromatogram is recorded 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 thes
26、e data, the boilingrange distribution can be obtained.4.2 Procedure A and Procedure B yield essentially the sameresults. See Sections 14 and 23, and the accompanying researchreports.5. Significance and Use5.1 The boiling range distribution of petroleum fractionsprovides an insight into the compositi
27、on of feedstocks andproducts related to petroleum refining processes. The gaschromatographic simulation of this determination can be usedto replace conventional distillation methods for control ofrefining operations. This test method can be used for productspecification testing with the mutual agree
28、ment of interestedparties.5.2 Boiling range distributions obtained by this test methodare essentially equivalent to those obtained by true boilingpoint (TBP) distillation (see Test Method D2892). They are notequivalent to results from low efficiency distillations such asthose obtained with Test Meth
29、od D86 or D1160.5.3 Procedure B was tested with biodiesel mixtures andreports the Boiling Point Distribution of FAME esters ofvegetable and animal origin mixed with ultra low sulfur diesel.Procedure A6. Apparatus6.1 ChromatographThe gas chromatograph used musthave the following performance character
30、istics:6.1.1 DetectorEither a flame ionization or a thermalconductivity 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 ofresol
31、ution as defined in 9.3.1. When operating at this sensitiv-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 temperatureemploy
32、ed. Connection of the column to the detector must besuch that no temperature below the column temperature exists.NOTE 2It is not desirable to operate a thermal conductivity detector ata temperature higher than the maximum column temperature employed.Operation at higher temperature generally contribu
33、tes to higher noiselevels and greater drift and can shorten 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
34、compounds up to aboiling temperature of 538C (1000F) before 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.D2887 1426.1.3 Cryo
35、genic Column CoolingColumn starting tem-peratures below ambient will 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. Excessi
36、vely low initial column temperature must beavoided to ensure that 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 o
37、f operating continuously at a temperature equiva-lent to the maximum column temperature employed, or providefor on-column injection with some means of programming theentire column, including the point of sample introduction, up tothe maximum temperature required. Connection of the columnto the sampl
38、e inlet system must be such that no temperaturebelow the 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
39、 of thecarrier gas supplied to the gas chromatograph must 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 tubularc
40、olumns, inlet pressures from 10 to 70 kPa (1.5 to 10 psig)have been found to be suitable.6.1.6 MicrosyringeA microsyringe is needed for sampleintroduction.NOTE 3Automatic sampling devices or other sampling means, such asindium encapsulation, can be used provided: the system can be operatedat a tempe
41、rature sufficiently high to completely vaporize hydrocarbonswith 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 petroleu
42、m hydrocarbons in orderof increasing boiling point and 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 RecorderA0 to 1 mV range recording potentiometeror equivalent, with a full-scale response
43、time of2sorless maybe used.6.3.2 IntegratorMeans must 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
44、measuring theretention time and areas of eluting peaks (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 proces
45、sing. The electronicrange of the integrator/computer (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 4Some gas chromatographs
46、have an algorithm built into theiroperating software 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 stor
47、e and automaticallysubtract a blank analysis from subsequent 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 onAnalyt
48、ical Reagents of the American Chemical Society whereTABLE 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 in
49、ner 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 heliumSupport 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
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