ASTM D2887-2016a Standard Test Method for Boiling Range Distribution of Petroleum Fractions by Gas Chromatography《使用气相色谱法测定石油馏分沸腾区域分布的标准试验方法》.pdf

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1、Designation: D2887 16D2887 16aDesignation: 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

2、 case of 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

3、This test method covers the determination of the boiling range distribution of petroleum products. The test method isapplicable to petroleum products and fractions having a final boiling point of 538 C (1000 F) or lower at atmospheric pressureas measured by this test method. This test method is limi

4、ted to samples having a boiling range greater than 55.5 C (100 F), andhaving a vapor pressure sufficiently low to permit sampling at ambient temperature.NOTE 1Since a boiling range is the difference between two temperatures, only the constant of 1.8 F C is used in the conversion of the temperaturera

5、nge from one system of units to another.1.1.1 Procedure A (Sections 6 14)Allows a larger selection of columns and analysis conditions such as packed and capillarycolumns as well as a Thermal Conductivity Detector in addition to the Flame Ionization Detector. Analysis times range from14 min to 60 min

6、.1.1.2 Procedure B (Sections 15 23)Is restricted to only 3 capillary columns and requires no sample dilution. In addition,Procedure B is used not only for the sample types described in ProcedureAbut also for the analysis of samples containing biodieselmixtures B5, B10, and B20. The analysis time, wh

7、en using Procedure B (Accelerated D2887), is reduced to about 8 min.1.2 This test method is not to be used for the analysis of gasoline samples or gasoline components. These types of samples mustbe analyzed by Test Method D7096.1.3 The values stated in SI units are to be regarded as standard. The in

8、ch-pound units given in parentheses are for informationonly.1.4 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilityof the user of this standard to establish appropriate safety and health practices and determine the applicabi

9、lity of regulatorylimitations prior to use.2. Referenced Documents2.1 ASTM Standards:3D86 Test Method for Distillation of Petroleum Products and Liquid Fuels at Atmospheric PressureD1160 Test Method for Distillation of Petroleum Products at Reduced PressureD2892 Test Method for Distillation of Crude

10、 Petroleum (15-Theoretical Plate Column)D4057 Practice for Manual Sampling of Petroleum and Petroleum ProductsD4626 Practice for Calculation of Gas Chromatographic Response FactorsD6708 Practice for Statistical Assessment and Improvement of Expected Agreement Between Two Test Methods that Purportto

11、Measure the Same Property of a Material1 This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of SubcommitteeD02.04.0H on Chromatographic Distribution Methods.Current edition approved April 1, 2016Oct. 1,

12、 2016. Published May 2016November 2016. Originally approved in 1973. Last previous edition approved in 20152016 asD2887 15D28871. DOI: 10.1520/D2887-16. 16. DOI: 10.1520/D2887-16A.2 This standard has been developed through the cooperative effort between ASTM International and the Energy Institute, L

13、ondon. The EI and ASTM International logosimply that the ASTM International and EI standards are technically equivalent, but does not imply that both standards are editorially identical.3 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceast

14、m.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes have been made to the previous version. Becaus

15、eit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM is to be considered the official document.*A Summary of Changes section appears

16、 at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1D7096 Test Method for Determination of the Boiling Range Distribution of Gasoline by Wide-Bore Capillary GasChromatographyD7169 Test Method for Boiling Point

17、Distribution of Samples with Residues Such as Crude Oils and Atmospheric and VacuumResidues by High Temperature Gas ChromatographyE260 Practice for Packed Column Gas ChromatographyE355 Practice for Gas Chromatography Terms and RelationshipsE516 Practice for Testing Thermal Conductivity Detectors Use

18、d in Gas ChromatographyE594 Practice for Testing Flame Ionization Detectors Used in Gas or Supercritical Fluid Chromatography3. Terminology3.1 DefinitionsThis test method makes reference to many common gas chromatographic procedures, terms, and relationships.Detailed definitions of these can be foun

19、d in Practices E260, E355, and E594.3.2 Definitions of Terms Specific to This Standard:3.2.1 area slice, nthe area, resulting from the integration of the chromatographic detector signal, within a specified retentiontime interval. In area slice mode (see 6.3.2), peak detection parameters are bypassed

20、 and the detector signal integral is recordedas area slices of consecutive, fixed duration time intervals.3.2.2 corrected area slice, nan area slice corrected for baseline offset, by subtraction of the exactly corresponding area slicein a previously recorded blank (non-sample) analysis.3.2.3 cumulat

21、ive corrected area, nthe accumulated sum of corrected area slices from the beginning of the analysis througha given retention time, ignoring any non-sample area (for example, solvent).3.2.4 final boiling point (FBP), nthe temperature (corresponding to the retention time) at which a cumulative correc

22、ted areacount equal to 99.5 % of the total sample area under the chromatogram is obtained.3.2.5 initial boiling point (IBP), nthe temperature (corresponding to the retention time) at which a cumulative corrected areacount equal to 0.5 % of the total sample area under the chromatogram is obtained.3.2

23、.6 slice rate, nthe time interval used to integrate the continuous (analog) chromatographic detector response during ananalysis. 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 each contiguous area slice. Th

24、e slice time is equal to the slice numberdivided 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 to baseline after complete sample elution.3.3 Abbreviations:

25、3.3.1 Acommon abbreviation of hydrocarbon compounds is to designate the number of carbon atoms in the compound.Aprefixis used to indicate the carbon chain form, while a subscripted suffix denotes the number of carbon atoms (for example, normaldecane = n-C10; isotetradecane = i-C14).4. Summary of Tes

26、t Method4.1 The boiling range distribution determination by distillation is simulated by the use of gas chromatography. A nonpolarpacked or open tubular (capillary) gas chromatographic column is used to elute the hydrocarbon components of the sample in orderof increasing boiling point. The column te

27、mperature is raised at a reproducible linear rate and the area under the chromatogramis recorded throughout the analysis. Boiling points are assigned to the time axis from a calibration curve obtained under the samechromatographic conditions by analyzing a known mixture of hydrocarbons covering the

28、boiling range expected in the sample.From these data, the boiling range distribution can be obtained.4.2 Procedure A and Procedure B yield essentially the same results. See Sections 14 and 23, and the accompanying researchreports.5. Significance and Use5.1 The boiling range distribution of petroleum

29、 fractions provides an insight into the composition of feedstocks and productsrelated to petroleum refining processes. The gas chromatographic simulation of this determination can be used to replaceconventional distillation methods for control of refining operations. This test method can be used for

30、 product specification testingwith the mutual agreement of interested parties.5.2 Boiling range distributions obtained by this test method are essentially equivalent to those obtained by true boiling point(TBP) distillation (see Test Method D2892). They are not equivalent to results from low efficie

31、ncy distillations such as thoseobtained with Test Method D86 or D1160.5.3 Procedure B was tested with biodiesel mixtures and reports the Boiling Point Distribution of FAME esters of vegetable andanimal origin mixed with ultra low sulfur diesel.D2887 16a2Procedure A6. Apparatus6.1 ChromatographThe ga

32、s chromatograph used must have the following performance characteristics:6.1.1 DetectorEither a flame ionization or a thermal conductivity detector may be used. The detector must have sufficientsensitivity to detect 1.0 % dodecane with a peak height of at least 10 % of full scale on the recorder und

33、er conditions prescribedin this test method and without loss of resolution as defined in 9.3.1. When operating at this sensitivity level, detector stability mustbe such that a baseline drift of not more than 1 % of full scale per hour is obtained. The detector must be capable of operatingcontinuousl

34、y at a temperature equivalent to the maximum column temperature employed. Connection of the column to the detectormust be such that no temperature below the column temperature exists.NOTE 2It is not desirable to operate a thermal conductivity detector at a temperature higher than the maximum column

35、temperature employed.Operation at higher temperature generally contributes to higher noise levels and greater drift and can shorten the useful life of the detector.6.1.2 Column Temperature ProgrammerThe chromatograph must be capable of linear programmed temperature operationover a range sufficient t

36、o establish a retention time of at least 1 min for the IBPand to elute compounds up to a boiling temperatureof 538 C (1000 F) before reaching the upper end of the temperature program. The programming rate must be sufficientlyreproducible to obtain retention time repeatability of 0.1 min (6 s) for ea

37、ch component in the calibration mixture described in 7.8.6.1.3 Cryogenic Column CoolingColumn starting temperatures below ambient will be required if samples with IBPs of lessthan 93 C (200 F) are to be analyzed. This is typically provided by adding a source of either liquid carbon dioxide or liquid

38、nitrogen, controlled through the oven temperature circuitry. Excessively low initial column temperature must be avoided to ensurethat the stationary phase remains liquid. The initial temperature of the column should be only low enough to obtain a calibrationcurve meeting the specifications of the me

39、thod.6.1.4 Sample Inlet SystemThe sample inlet system must be capable of operating continuously at a temperature equivalent tothe maximum column temperature employed, or provide for on-column injection with some means of programming the entirecolumn, including the point of sample introduction, up to

40、 the maximum temperature required. Connection of the column to thesample inlet system must be such that no temperature below the column temperature exists.6.1.5 Flow ControllersThe gas chromatograph must be equipped with mass flow controllers capable of maintaining carriergas flow constant to 61 % o

41、ver the full operating temperature range of the column. The inlet pressure of the carrier gas suppliedto the gas chromatograph must be sufficiently high to compensate for the increase in column backpressure as the columntemperature is raised. An inlet pressure of 550 kPa (80 psig) has been found sat

42、isfactory with the packed columns described inTable 1. For open tubular columns, inlet pressures from 10 kPa to 70 kPa (1.5 psig to 10 psig) have been found to be suitable.6.1.6 MicrosyringeA microsyringe is needed for sample introduction.NOTE 3Automatic sampling devices or other sampling means, suc

43、h as indium encapsulation, can be used provided: the system can be operated ata temperature sufficiently high to completely vaporize hydrocarbons with atmospheric boiling points of 538 C (1000 F), and the sampling system isconnected to the chromatographic column avoiding any cold temperature zones.6

44、.2 ColumnAny column and conditions may be used that provide separation of typical petroleum hydrocarbons in order ofincreasing boiling point and meet the column performance requirements of 9.3.1 and 9.3.3. Successfully used columns andconditions are given in Table 1.6.3 Data Acquisition System:TABLE

45、 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 U

46、C-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 SA GB PC PC Carrier 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 5

47、0 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 N2 helium Detector FID FID FIDCarrier gas flow, mL/min 40 30 25 60 Detector temper

48、ature, C 350 380 370Detector TC FID FID TC Injector temperature, C 340 cool on-column cool on-columnDetector temperature, C 360 370 360 390 Sample size, L 0.5 1 0.10.2Injection port temperature, C 360 370 350 390 Sample concentration mass % 25 2 neatSample size, 4 0.3 1 5A Diatoport S; silane treate

49、d.B Chromosorb G (AW-DMS).C Chromosorb P, acid washed.D2887 16a36.3.1 RecorderA0 mV to 1 mV range recording potentiometer or equivalent, with a full-scale response time of 2 s or less maybe used.6.3.2 IntegratorMeans must be provided for determining the accumulated area under the chromatogram. This can be done bymeans of an electronic integrator or computer-based chromatography data system. The integrator/computer system must havenormal chromatographic software for measuring the retention time and areas of eluting pea