1、Designation: D2887 08D2887 12Designation: 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 Department of Defense.1. Scope*1.1 This t
3、est 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 538C (1000F) or lower at atmospheric pressureas measured by this test method. This test method is limited to s
4、amples having a boiling range greater than 55.5C (100F), 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 1.8F/C is used in the conversion of the temperaturerange from on
5、e system of units to another.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 D3710.1.3 The values stated in SI units are to be regarded as standard. The inch-pound units given in parentheses are
6、 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 applicability of regulatorylimitations prior to
7、use.2. Referenced Documents2.1 ASTM Standards:3D86 Test Method for Distillation of Petroleum Products at Atmospheric PressureD1160 Test Method for Distillation of Petroleum Products at Reduced PressureD2892 Test Method for Distillation of Crude Petroleum (15-Theoretical Plate Column)D3710 Test Metho
8、d for Boiling Range Distribution of Gasoline and Gasoline Fractions by Gas ChromatographyD4057 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 A
9、greement Between Two Test Methods that Purportto Measure the Same Property of a MaterialE260 Practice for Packed Column Gas ChromatographyE355 Practice for Gas Chromatography Terms and RelationshipsE516 Practice for Testing Thermal Conductivity Detectors Used in Gas ChromatographyE594 Practice for T
10、esting Flame Ionization Detectors Used in Gas or Supercritical Fluid Chromatography1 This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.04.0Hon Chromatographic Distribution Methods.Current edition
11、 approved Dec. 1, 2008Nov. 1, 2012. Published January 2009April 2013. Originally approved in 1973. Last previous edition approved in 20062008 asD288706a.08. DOI: 10.1520/D2887-08.10.1520/D2887-12.2 This standard has been developed through the cooperative effort between ASTM International and the Ins
12、titute of Petroleum, Energy Institute, London. The IPEI andASTM International logos imply that the ASTM International and IPEI standards are technically equivalent, but their use does not imply that both standards are editoriallyidentical.3 For referencedASTM standards, visit theASTM website, www.as
13、tm.org, or contactASTM Customer Service at serviceastm.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 c
14、hanges have been made to the previous version. Becauseit 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 of
15、ficial document.*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 test method makes reference to many common gas chromatographic procedur
16、es, terms, and relationships.Detailed definitions of these can be found in Practices E260, E355, and E594.3.2 Definitions of Terms Specific to This Standard:3.2.1 area sliceslice, nthe area, resulting from the integration of the chromatographic detector signal, within a specifiedretention time inter
17、val. In area slice mode (see 6.3.2), peak detection parameters are bypassed and the detector signal integral isrecorded as area slices of consecutive, fixed duration time intervals.3.2.2 corrected area sliceslice, nan area slice corrected for baseline offset, by subtraction of the exactly correspond
18、ing areaslice in a previously recorded blank (non-sample) analysis.3.2.3 cumulative corrected areaarea, nthe accumulated sum of corrected area slices from the beginning of the analysisthrough a given retention time, ignoring any non-sample area (for example, solvent).3.2.4 final boiling point (FBP)(
19、FBP), nthe temperature (corresponding to the retention time) at which a cumulativecorrected area count equal to 99.5 % of the total sample area under the chromatogram is obtained.3.2.5 initial boiling point (IBP)(IBP), nthe temperature (corresponding to the retention time) at which a cumulativecorre
20、cted area count equal to 0.5 % of the total sample area under the chromatogram is obtained.3.2.6 slice raterate, nthe time interval used to integrate the continuous (analog) chromatographic detector response duringan analysis. The slice rate is expressed in hertz (for example, integrations or slices
21、 per second).3.2.7 slice timetime, nthe time associated with the end of each contiguous area slice. The slice time is equal to the slicenumber divided by the slice rate.3.2.8 total sample areaarea, nthe cumulative corrected area, from the initial area point to the final area point, where thechromato
22、graphic signal is considered to have returned to baseline after complete sample elution.3.3 Abbreviations: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 denote
23、s the number of carbon atoms (for example, normaldecane = n-C10; isotetradecane = i-C14).4. Summary of Test 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
24、 used to elute the hydrocarbon components of the sample in orderof increasing boiling point. The column temperature 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 ob
25、tained under the samechromatographic conditions by analyzing a known mixture of hydrocarbons covering the boiling range expected in the sample.From these data, the boiling range distribution can be obtained.5. Significance and Use5.1 The boiling range distribution of petroleum fractions provides an
26、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 product specification
27、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 efficiency distillations such
28、as thoseobtained with Test Method D86 or D1160.6. Apparatus6.1 ChromatographThe gas 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.
29、0 % dodecane with a peak height of at least 10 % of full scale on the recorder under 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 ful
30、l scale per hour is obtained. The detector must be capable of operatingcontinuously 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 operat
31、e a thermal conductivity detector at a temperature higher than the maximum column 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 m
32、ust be capable of linear programmed temperature operationover a range sufficient to establish a retention time of at least 1 min for the IBPand to elute compounds up to a boiling temperatureD2887 122of 538C (1000F) before reaching the upper end of the temperature program. The programming rate must b
33、e sufficientlyreproducible to obtain retention time repeatability of 0.1 min (6 s) for each 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 93C (200F) are to be analyzed.
34、This is typically provided by adding a source of either liquid carbon dioxide or liquidnitrogen, 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 shou
35、ld be only low enough to obtain a calibrationcurve meeting the specifications of the method.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 m
36、eans of programming the entirecolumn, including the point of sample introduction, up to 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 equipp
37、ed with mass flow controllers capable of maintaining carriergas flow constant to 61 % over 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
38、 columntemperature is raised. An inlet pressure of 550 kPa (80 psig) has been found satisfactory with the packed columns described inTable 1. For open tubular columns, 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 sam
39、ple introduction.NOTE 3Automatic sampling devices or other sampling means, such 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 538C (1000F), and the sampling system isc
40、onnected to the chromatographic column avoiding any cold temperature zones.6.2 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
41、columns andconditions are given in Table 1.6.3 Data Acquisition System:6.3.1 RecorderA 0 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.
42、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 peaks (peak detection mode). In addition,the system must be capable of conv
43、erting the continuously integrated detector signal into area slices of fixed duration. Thesecontiguous area slices, collected for the entire analysis, are stored for later processing. The electronic range of theintegrator/computer (for example, 1 V, 10 V) must be within the linear range of the detec
44、tor/electrometer system used. The systemmust be capable of subtracting the area slice of a blank run from the corresponding area slice of a sample run.NOTE 4Some gas chromatographs have an algorithm built into their operating software that allows a mathematical model of the baseline profile tobe sto
45、red in memory.This profile is automatically subtracted from the detector signal on subsequent sample analyses to compensate for any baseline offset.Some integration systems also store and automatically subtract a blank analysis from subsequent analytical determinations.TABLE 1 Typical Operating Cond
46、itionsPacked 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 ph
47、ase 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 50 Initial column temperat
48、ure, 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 temperature, C 350 380 370Detec
49、tor 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 treated.B Chromosorb G (AW-DMS).C Chromosorb P, acid washed.D2887 1237. Reagents and Materials7.1 Purity of ReagentsReagent grade chemicals shall be used in all tests. Unless otherwise indicated, it is intended that allreagents conform to the specificati
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