1、Designation: D7500 10D7500 12Standard Test Method forDetermination of Boiling Range Distribution of Distillatesand Lubricating Base Oilsin Boiling Range from 100 to735C by Gas Chromatography1This standard is issued under the fixed designation D7500; the number immediately following the designation i
2、ndicates the year oforiginal adoption or, in the 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.1. Scope*1.1 This test method covers the determinat
3、ion of the boiling range distribution of petroleum products by capillary gaschromatography using flame ionization detection. This standard test method has been developed through the harmonization of twotest methods, Test Method D6352 and IP 480. As both of these methods cover the same scope and incl
4、ude very similar operatingconditions, it was agreed that a single standard method would benefit the global simulated distillation community.1.2 This test method is not applicable for the analysis of petroleum or petroleum products containing low molecular weightcomponents (for example naphthas, refo
5、rmates, gasolines, diesel). Components containing hetero atoms (for example alcohols,ethers, acids, or esters) or residue are not to be analyzed by this test method. See Test Methods D7096, D2887, or D7213 forpossible applicability to analysis of these types of materials. This method is also not sui
6、table for samples that will not elutecompletely from the gas chromatographic column, leaving residues. For such samples as crude oils and residues, see Test MethodsD5307 and D7169.1.3 This test method is applicable to distillates with initial boiling points above 100C and final boiling points below
7、735C(carbon 110); for example, distillates (IBP 100C), base oils and lubricating base stocks.1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.1.5 This standard does not purport to address all of the safety concerns, if any,
8、 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 use.2. Referenced Documents2.1 ASTM Standards:2D86 Test Method for Distillation of Petroleum Products
9、at Atmospheric PressureD1160 Test Method for Distillation of Petroleum Products at Reduced PressureD2887 Test Method for Boiling Range Distribution of Petroleum Fractions by Gas ChromatographyD5307 Test Method for Determination of Boiling Range Distribution of Crude Petroleum by Gas Chromatography (
10、Withdrawn2011)3D6352 Test Method for Boiling Range Distribution of Petroleum Distillates in Boiling Range from 174 to 700C by GasChromatographyD7096 Test Method for Determination of the Boiling Range Distribution of Gasoline by Wide-Bore Capillary GasChromatographyD7169 Test Method for Boiling Point
11、 Distribution of Samples with Residues Such as Crude Oils and Atmospheric and VacuumResidues by High Temperature Gas ChromatographyD7213 Test Method for Boiling Range Distribution of Petroleum Distillates in the Boiling Range from 100 to 615C by GasChromatography1 This test method is under the juris
12、diction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.04.0Hon Chromatographic Distribution Methods.Current edition approved May 1, 2010Nov. 1, 2012. Published August 2010April 2013. Originally approved in 2008. Last previous edition a
13、pproved in 20082010 asD7500D7500-08.-10. DOI: 10.1520/D7500-10.10.1520/D7500-12.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page o
14、n the ASTM website.3 The last approved version of this historical standard is referenced on www.astm.org.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. Becauseit may not be techn
15、ically 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 at the end of this
16、standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1E355 Practice for Gas Chromatography Terms and RelationshipsE594 Practice for Testing Flame Ionization Detectors Used in Gas or Supercritical Fluid ChromatographyE1510 Practice f
17、or Installing Fused Silica Open Tubular Capillary Columns in Gas ChromatographsD7500 1222.2 ISO Standard:4ISO 3170 Petroleum Liquids Manual Sampling3. Terminology3.1 DefinitionsThis test method makes reference to many common gas chromatographic procedures, terms, and relationships.For definitions of
18、 these terms used in this test method, refer to Practices E355, E594, and E1510.3.2 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 6.4.
19、1), peak detection parameters are bypassed 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
20、blank (non-sample) analysis.3.2.3 cumulative 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 ret
21、ention time) at which a cumulative corrected 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 ar
22、ea under the chromatogram is obtained.3.2.6 slice rate, nthe frequency used in sampling (analog) the chromatographic detector signal during an analysis. The slicerate is expressed in Hz (for example integrations or slices per second).3.2.7 slice time, nthe inverse function of the acquisition rate. I
23、t is the time duration of each sampling pulse usually expressedin seconds. The slice time is the time at the end of each contiguous area slice.3.2.8 total sample area, nthe cumulative corrected area, from the initial area point to the final area point, where thechromatographic signal has returned to
24、 baseline after complete sample elution.3.3 AbbreviationsA common abbreviation of hydrocarbon compounds is to designate the number of carbon atoms in thecompound. A prefix is used to indicate the carbon chain form, while a subscripted suffix denotes the number of carbon atoms (forexample n-C10 for n
25、ormal-decane, i-C14 for iso-tetradecane).4. Summary of Test Method4.1 The boiling range distribution determination by distillation is simulated by the use of gas chromatography.Anon-polar opentubular (capillary) gas chromatographic column is used to elute the hydrocarbon components of the sample in
26、order of increasingboiling point.4.2 A sample aliquot is diluted with a viscosity reducing solvent and introduced into the chromatographic system. Samplevaporization is provided by separate heating of the point of injection or in conjunction with column oven heating.4.3 The column oven temperature i
27、s raised at a specified linear rate to affect separation of the hydrocarbon components in orderof increasing boiling point. The elution of sample components is quantitatively determined using a flame ionization detector. Thedetector signal is recorded as area slices for consecutive retention time in
28、tervals during the analysis.4.4 Retention times of known normal paraffin hydrocarbons, spanning the scope of the test method, are determined andcorrelated to their boiling point temperatures. The normalized cumulative corrected sample areas for each consecutive recordedtime interval are used to calc
29、ulate the boiling range distribution. The boiling point temperature at each reported percent offincrement is calculated from the retention time calibration.5. Significance and Use5.1 The boiling range distribution of medium and heavy petroleum distillate fractions provides an insight into the compos
30、itionof feed stocks and products related to petroleum refining processes (for example, hydrocracking, hydrotreating, visbreaking, ordeasphalting). The gas chromatographic simulation of this determination can be used to replace conventional distillation methodsfor control of refining operations. This
31、 test method can be used for product specification testing with the mutual agreement ofinterested parties.5.2 This test method extends the scope of boiling range determination by gas chromatography to include distillates(IBP 100C) and heavy petroleum distillate fractions beyond the scope of Test Met
32、hod D2887 (538C).5.3 Boiling range distributions obtained by this test method have not been analyzed for correlation to those obtained by lowefficiency distillation, such as with Test Method D86 or D1160. This test method does not claim agreement between these physical4 Available from American Natio
33、nal Standards Institute (ANSI), 25 W. 43rd St., 4th Floor, New York, NY 10036, http:/www.ansi.org.D7500 123distillations and simulated distillation. Efforts to resolve this question will continue. When successful resolutions of the questionsare determined, this test method will be revised accordingl
34、y.6. Apparatus6.1 ChromatographThe gas chromatographic system used shall have the following performance characteristics:6.1.1 Carrier Gas Flow ControlThe chromatograph shall be equipped with carrier gas pressure or flow control capable ofmaintaining constant carrier gas flow to 61 % throughout the c
35、olumn temperature program cycle.6.1.2 Column OvenCapable of sustained and linear programmed temperature operation from near ambient (for example, 30to 35C) up to 430C.6.1.3 Column Temperature ProgrammerThe chromatograph shall be capable of linear programmed temperature operation upto 430C at selecta
36、ble linear rates up to 10C/min. The programming rate shall be sufficiently reproducible to obtain the retentiontime repeatability of 0.1 min (6 s) for each component in the calibration mixture described in 7.5.6.1.4 DetectorThis test method requires the use of a flame ionization detector (FID). The
37、detector shall meet or exceed thefollowing specifications in accordance with Practice E594. Check the detector according the instrument manufacturers instructions.6.1.4.1 Operating Temperature100 to 430C.6.1.4.2 Connection of the column to the detector shall be such that no temperature below the col
38、umn temperature exists betweenthe column and the detector. Refer to Practice E1510 for proper installation and conditioning of the capillary column.6.1.5 Sample Inlet SystemAny sample inlet system capable of meeting the performance specification in AnnexA3 and executethe conditions of Table 2. Progr
39、ammable temperature vaporization (PTV) and cool on-column (COC) injection systems have beenused successfully.6.2 MicrosyringeAmicrosyringe with a 23-gauge or smaller stainless steel needle is used for on-column sample introduction.Syringes of 0.1 to 10-L capacity are available.6.2.1 Automatic syring
40、e injection is recommended to achieve best precision.6.3 ColumnThis test method is limited to the use of non-polar wall coated open tubular (WCOT) columns of high thermalstability. Fused silica (aluminum coated) and stainless steel columns with 0.53 to 0.75-mm internal diameter have been successfull
41、yused. Cross-linked or bonded 100 % dimethyl-polysiloxane stationary phases with film thickness of 0.09 to 0.17 m have beenused. The column length and liquid phase film thickness shall allow the elution of C110 n-paraffin (BP = 735C). The column andconditions shall provide separation of typical petr
42、oleum hydrocarbons in order of increasing boiling point and meet the columnperformance requirements of A3.2.1. The column shall provide a resolution not less than 2 and not higher than 4 using the testmethod operating conditions in Table 2.6.4 Data Acquisition System:6.4.1 Integrator/Computer System
43、Means shall be provided for determining the accumulated area under the chromatogram.This can be done by means of an electronic integrator or computer-based chromatography data system. The integrator/computersystem shall have normal chromatographic software for measuring the retention time and areas
44、of eluting peaks (peak processingmode). In addition, the system shall be capable of converting the continuously integrated detector signal into area slices of fixedduration (slice mode). These contiguous area slices, collected for the entire analysis, are stored for later processing. A similarcollec
45、tion of contiguous slices is also collected for the blank run. It is necessary that the number of slices collected for sample andblank analysis are the same. The electronic range of the integrator/computer (for example 1 V, 10 V) shall be operated within thelinear range of the detector/electrometer
46、system used.NOTE 1Some gas chromatographs have an algorithm built into their operating software that allows a mathematical model of the baseline profile tobe stored in memory. This profile is automatically subtracted from the detector signal on subsequent sample runs to compensate for the column ble
47、ed.Some integration systems also store and automatically subtract a blank analysis from subsequent analytical determinations.TABLE 1 Reference Material 5010A% Dist.m/m C F r, C R, C r, F R, FIBP 421 789 3 9 5 165 476 888 2 4 4 810 491 916 2 4 3 720 510 950 2 5 3 930 524 975 2 5 3 940 536 998 2 5 3 9
48、50 548 1018 2 5 3 960 559 1039 2 5 3 970 572 1061 2 5 3 980 585 1085 2 5 3 990 602 1116 2 5 3 995 617 1142 2 5 3 9FBP 661 1223 9 17 16 31A Values obtained from including Reference Oil 5010 in the ILS sample set.D7500 1247. Reagents and Materials7.1 Liquid Stationary PhaseA methyl silicone stationary
49、 phase for the column.7.2 Carrier GasesHelium, of at least 99.999 % (v/v) purity. Any oxygen present is removed by a chemical resin filter.(WarningFollow the safety instructions from the filter supplier.) Total impurities not to exceed 10 mL/m3. Helium or Nitrogen(99.999 %) can also be used as detector makeup gas.7.3 Hydrogen99.999 % Grade suitable for flame ionization detectors. Total impurities not to exceed 10 mL/m3.7.4 Compressed AirRegulated for flame ionization detectors. Total impurities not to exceed 10 mL/m3.7.5 Alkanes
