ASTM D2887-2018 Standard Test Method for Boiling Range Distribution of Petroleum Fractions by Gas Chromatography.pdf

1、Designation: D2887 18Designation: 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 B

6、 (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 B

7、 (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 D7096.1.3 The values stated in SI units are to be regarded asstandard. The values given in parenthes

8、es after SI units areprovided for information only and are not considered standard.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, health, and environmenta

9、l practices and deter-mine the applicability of regulatory limitations prior to use.1.5 This international standard was developed in accor-dance with internationally recognized principles on standard-ization established in the Decision on Principles for theDevelopment of International Standards, Gui

10、des and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.2. Referenced Documents2.1 ASTM Standards:3D86 Test Method for Distillation of Petroleum Products andLiquid Fuels at Atmospheric PressureD1160 Test Method for Distillation of Petroleum Products

11、 atReduced PressureD2892 Test Method for Distillation of Crude Petroleum(15-Theoretical Plate Column)D4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4626 Practice for Calculation of Gas ChromatographicResponse FactorsD6300 Practice for Determination of Precision and BiasData fo

12、r Use in Test Methods for Petroleum Products andLubricantsD6708 Practice for Statistical Assessment and Improvementof Expected Agreement Between Two Test Methods thatPurport to Measure the Same Property of a MaterialD7096 Test Method for Determination of the Boiling Range1This test method is under t

13、he 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 June 1, 2018. Published August 2018. Originallyapproved in 1973. Last previous edition a

14、pproved in 2016 as D2887 16a. DOI:10.1520/D2887-18.2This 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 aretechnically equivalent, but does no

15、t 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 page onthe ASTM website.*A Summa

16、ry 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 StatesThis international standard was developed in accordance with internationally recognized principles on standardization established

17、in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.1Distribution of Gasoline by Wide-Bore Capillary GasChromatographyD7169 Test Method for Boiling Point Distributio

18、n ofSamples with Residues Such as Crude Oils and Atmo-spheric and Vacuum Residues by High Temperature GasChromatographyE260 Practice for Packed Column Gas ChromatographyE355 Practice for Gas Chromatography Terms and Relation-shipsE516 Practice for Testing Thermal Conductivity DetectorsUsed in Gas Ch

19、romatographyE594 Practice 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 Practi

20、cesE260, E355, and 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 detec

21、tor signalintegral 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 a

22、rea, nthe accumulated 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 eq

23、ual 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 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, nt

24、he time interval used 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 equa

25、l 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 point, where thechromatographic signal is considered to have returned tobaseline after complete sample elution.3.3 Abbreviations:3.3.1 Acommon abbrevia

26、tion of hydrocarbon 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 boilin

27、g range distribution determination by distilla-tion is simulated by the use of gas chromatography.Anonpolarpacked 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

28、a reproducible linear 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 i

29、n the sample. From 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 ins

30、ight into the composition 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 testin

31、g 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 (see Test Method D2892). They are notequivalent to results from low efficiency distillations such asthose

32、obtained with Test 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 followin

33、g performance characteristics: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 a

34、nd 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 ofnot more than 1 % of full scale per hour is obtained. Thedetector must be capable of operating continuously at atemperature equivalent to the maximum c

35、olumn temperatureemployed. 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 atD2887 182a temperature higher than the maximum column temperature employed.Operation at highe

36、r temperature generally contributes 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

37、 1 min for the IBP and to 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 de

38、scribed in 7.8.6.1.3 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 temp

39、erature cir-cuitry. 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 in

40、let system mustbe 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. Connectio

41、n of the columnto 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

42、 column. The inlet 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

43、 Table 1. For open 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:

44、the system can be 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 that

45、provide separation 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-omete

46、r or equivalent, 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 syst

47、emmust have normal 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

48、 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 detector/electrometer systemused. The system must be capable of subtracting the area sliceof a blank run from the corresponding area sli

49、ce 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 in memory. This profile is automatically subtractedfrom the detector signal on subsequent sample analyses to compensate forTABLE 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 diam