1、Designation: D2887 15Designation: 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 538 C (1000 F) or lower at atmosphericpressure as measured by this test method. This test method islimited to sampl
4、es having a boiling range greater than 55.5 C(100 F), 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 1.8 F C is used in the conversion ofthe temperature range from one s
5、ystem 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 min to 60 min.1.1.2 Procedure
6、B (Sections 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
7、B (Accelerated 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 i
8、n 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 this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory li
9、mitations 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)
10、D3710 Test 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 Assessme
11、nt and Improvementof 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 Ch
12、romatography1This 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 July 1, 2015. Published July 2015. Originally ap
13、provedin 1973. Last previous edition approved in 2014 as D2887 14. DOI: 10.1520/D2887-15.2This 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
14、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 ASTMStandards volume information, refer to the standards Document Su
15、mmary 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 Pr
16、actice 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
17、E594.3.2 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
18、is recorded 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 accumulat
19、ed sum 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 th
20、e total 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 us
21、ed to 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 slicenumbe
22、r divided 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
23、 compounds 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 distributio
24、n determination 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 li
25、near rate 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. Fro
26、m these 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 com
27、position 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
28、 agreement 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 Tes
29、t Method 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 cha
30、racteristics: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 o
31、fresolution 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 temperature
32、employed. 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 co
33、ntributes 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
34、elute compounds up to aboiling temperature of 538 C (1000 F) 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 1526.
35、1.3 Cryogenic Column CoolingColumn starting tem-peratures below ambient will be required if samples with IBPsof less than 93 C (200 F) are to be analyzed. This is typicallyprovided by adding a source of either liquid carbon dioxide orliquid nitrogen, controlled through the oven temperature cir-cuitr
36、y. Excessively 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
37、 capable of 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
38、 the sample 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 inle
39、t pressure 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 ope
40、n tubularcolumns, inlet pressures from 10 kPa to 70 kPa (1.5 psig to10 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
41、 operatedat a temperature sufficiently high to completely vaporize hydrocarbonswith atmospheric boiling points of 538 C (1000 F), and the samplingsystem is connected to the chromatographic column avoiding any coldtemperature zones.6.2 ColumnAny column and conditions may be used thatprovide separatio
42、n of typical petroleum 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 RecorderA 0 mV to 1 mV range recording potenti-ometer or equivalent,
43、with a full-scale response time of 2 s orless may be 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 norma
44、l chromatographic software for 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 analys
45、is, are stored for later processing. 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
46、.NOTE 4Some gas chromatographs 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. Som
47、e integration systems also store 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 specifica
48、tions of the Committee onAnalytical 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
49、) 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 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
