ASTM D7213-2015 red 3692 Standard Test Method for Boiling Range Distribution of Petroleum Distillates in the Boiling Range from 100&x2009 &xb0 C to 615&x2009 &xb0 C by Gas Chromato.pdf

1、Designation: D7213 14D7213 15Standard Test Method forBoiling Range Distribution of Petroleum Distillates in theBoiling Range from 100 C to 615 C by GasChromatography1This standard is issued under the fixed designation D7213; the number immediately following the designation indicates the year oforigi

2、nal 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 determination of the boiling range

3、distribution of petroleum products. This test method isapplicable to petroleum distillates having an initial boiling point greater than 100 C and a final boiling point less than 615 C atatmospheric pressure as measured by this test method.1.2 The test method is not applicable for analysis of petrole

4、um distillates containing low molecular weight components (forexample, naphthas, reformates, gasolines, crude oils). Materials containing heterogeneous components (for example, alcohols,ethers, acids or esters) or residue are not to be analyzed by this test method. See Test Methods D7096, D2887, D63

5、52, or D7169.1.3 This test method uses the principles of simulated distillation methodology.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,

6、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 a

7、t Atmospheric PressureD1160 Test Method for Distillation of Petroleum Products at Reduced PressureD2887 Test Method for Boiling Range Distribution of Petroleum Fractions by Gas ChromatographyD2892 Test Method for Distillation of Crude Petroleum (15-Theoretical Plate Column)D4626 Practice for Calcula

8、tion of Gas Chromatographic Response FactorsD6352 Test Method for Boiling Range Distribution of Petroleum Distillates in Boiling Range from 174 C to 700 C by GasChromatographyD7096 Test Method for Determination of the Boiling Range Distribution of Gasoline by Wide-Bore Capillary GasChromatographyD71

9、69 Test Method for Boiling Point Distribution of Samples with Residues Such as Crude Oils and Atmospheric and VacuumResidues by High Temperature Gas ChromatographyE355 Practice for Gas Chromatography Terms and RelationshipsE594 Practice for Testing Flame Ionization Detectors Used in Gas or Supercrit

10、ical Fluid ChromatographyE1510 Practice for Installing Fused Silica Open Tubular Capillary Columns in Gas Chromatographs3. Terminology3.1 DefinitionsThis test method makes reference to many common gas chromatographic procedures, terms, and relationships.Detailed definitions of these can be found in

11、Practices E355, E594, and E1510.3.2 Definitions of Terms Specific to This Standard:1 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.C

12、urrent edition approved Oct. 1, 2014July 1, 2015. Published December 2014Ju;y 2015. Originally approved in 2005. Last previous edition approved in 20122014 asD7213 12D7213 14.1. DOI: 10.1520/D7213-14.10.1520/D7213-15.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM

13、 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 changes have been made

14、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 official document.*A Sum

15、mary 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 States13.2.1 area slice, nthe area, resulting from the integration of the chromatographic detector signal, within a specified retentio

16、ntime interval. In area slice mode (see 6.4.2), 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 corr

17、esponding area slicein a previously recorded 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

18、), nthe temperature (corresponding to the retention 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 ar

19、eacount equal to 0.5 % of the total sample area under the chromatogram is obtained.3.2.6 slice rate, nthe time interval used to integrate the continuous (analog) chromatographic detector response during ananalysis. The slice rate is expressed in Hz (for example, integrations or slices per second).3.

20、2.7 slice time, nthe cumulative slice rate (analysis time) associated with each area slice throughout the chromatographicanalysis. 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 point to the final area poi

21、nt.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, normal decane n-Cl0; iso-tetradecane = i-Cl4).4

22、. Summary of Test Method4.1 The boiling range distribution by distillation is simulated by the use of gas chromatography. The solvent should not interferewith measurement of the sample in the 100 C to 615 C range, and it should be apolar. A non-polar open tubular (capillary) gaschromatographic colum

23、n is used to elute the hydrocarbon components of the sample in order of increasing boiling 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 conjun

24、ction with column oven heating.4.3 The column oven temperature is raised at a reproducible linear rate to effect separation of the hydrocarbon components inorder of increasing boiling point. The elution of sample components is quantitatively determined using a flame ionization detector.The detector

25、signal integral is recorded as area slices for consecutive retention time intervals during the analysis.4.4 Retention times of known normal paraffin hydrocarbons spanning the scope of this test method (C5-C60) are determined andcorrelated to their boiling point temperatures. The normalized cumulativ

26、e corrected sample areas for each consecutive recordedtime interval are used to calculate 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

27、 light and medium petroleum distillate fractions provides an insight into the compositionof feed stocks and products related to petroleum refining process, This gas chromatographic determination of boiling range canbe used to replace conventional distillation methods for control of refining operatio

28、ns. This test method can be used for productspecification testing with the mutual agreement of interested parties.5.2 This test method extends the scope of boiling range determination by gas chromatography to include light and mediumpetroleum distillate fractions beyond the scope of Test Method D288

29、7 (538 C) and below Test Method D6352 (700 C).5.3 Boiling range distributions obtained by this test method are theoretically equivalent to those obtained by true boiling point(TBP) distillation (see Test Method D2892). They are not equivalent to results from low efficiency distillation such as those

30、obtained with Test Method D86 or D1160.6. Apparatus6.1 ChromatographThe gas chromatographic system used shall have the following performance characteristics:6.1.1 Column OvenCapable of sustained and linear programmed temperature operation from near ambient (for example,35 C to 50 C) up to 400 C.6.1.

31、2 Column Temperature ProgrammerThe chromatograph shall be capable of linear programmed temperature operation upto 400 C at selectable linear rates up to 20 Cmin. The programming rate shall be sufficiently reproducible to obtain the retentiontime repeatability of 0.1 min (6 s) for each component in t

32、he calibration mixture described in 7.5.6.1.3 DetectorThis test method requires a flame ionization detector (FID). The detector shall meet or exceed the followingspecifications as detailed in Practice E594. The flame jet should have an orifice of approximately 0.45 mm to 0.50 mm.D7213 1526.1.3.1 Ope

33、rating Temperature, 400 C.6.1.3.2 Sensitivity, 0.005 coulombs/g carbon.6.1.3.3 Minimum Detectability, 1 10-11 g carbon/s.6.1.3.4 Linear Range, 106.6.1.3.5 Connection of the column to the detector shall be such that no temperature below the column temperature exists. Referto Practice E1510 for proper

34、 installation and conditioning of the capillary column.6.1.4 Sample Inlet SystemAny sample inlet system capable of meeting the performance specification in 7.6 may be used.Programmed temperature vaporization (PTV) and programmable cool on-column injection systems have been used successfully.6.1.5 Ca

35、rrier Gas Flow ControlThe chromatograph shall be equipped with carrier gas pressure or flow control capable ofmaintaining constant carrier gas flow control through the column throughout the column temperature program cycle.6.2 MicrosyringeAmicrosyringe with a 23 gauge or smaller stainless steel need

36、le is used for on-column sample introduction.Syringes of 0.1 L to 10 L capacity are available.6.2.1 Automatic syringe 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. Gla

37、ss, fused silica, and stainless steel columns, with a 0.53 mm diameter have been successfully used. Cross-linked orbonded 100 % dimethyl-polysiloxane stationary phases with film thickness of 0.5 m to 1.0 m have been used. The column lengthand liquid phase film thickness shall allow the elution of at

38、 least C60 n-paraffin (BP = 615 C). The column and conditions shallprovide separation of typical petroleum hydrocarbons in order of increasing boiling point and meet the column resolutionrequirements of 8.2.1. The column shall provide a resolution between one and ten using this test methods operatin

39、g conditions.6.4 Data Acquisition System:6.4.1 RecorderA0 mV to 1 mV range recording potentiometer or equivalent, with a full-scale response time of 2 s or less maybe used to provide a graphical display.6.4.2 IntegratorMeans shall be provided for determining the accumulated area under the chromatogr

40、am. This can be done bymeans of an electronic integrator or computer-based chromatography data system. The integrator/computer system shall havenormal chromatographic software for measuring the retention time and areas of eluting peaks (peak detection mode). In addition,the system shall be capable o

41、f converting the continuously integrated detector signal into area slices of fixed duration (area slicemode). These contiguous area slices, collected for the entire analysis, are stored for later processing. The electronic range of theintegrator/computer (for example, 1 V, 10 V) shall be operated wi

42、thin the linear range of the detector/electrometer 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 subs

43、equent sample runs to compensate for the column bleed.Some integration systems also store and automatically subtract a blank analysis from subsequent analytical determinations.7. Reagents and Materials37.1 Carrier GasHelium or hydrogen of high purity. (WarningHelium and hydrogen are compressed gases

44、 under highpressure; hydrogen is an extremely flammable gas under high pressure.) These gases may be used as the carrier gas and shouldnot contain more than 5 mL/m3 of oxygen. The total amount of impurities should not exceed 10 mL/m3. Additional purificationis recommended by the use of molecular sie

45、ves or other suitable agents to remove water, oxygen, and hydrocarbons. Availablepressure shall be sufficient to ensure a constant carrier gas flow rate.7.2 HydrogenHydrogen of high purity (for example, hydrocarbon-free) is used as fuel for the flame ionization detector (FID).(WarningHydrogen is an

46、extremely flammable gas under high pressure.)7.3 AirHigh purity (for example, hydrocarbon-free) compressed air is used as the oxidant for the flame ionization detector(FID). (WarningCompressed air is a gas under high pressure and supports combustion.)7.4 SolventsUnless otherwise indicated, it is int

47、ended that all solvents conform to the specifications of the committee onanalytical Reagents of theAmerican Chemical Society where such specifications are available.3 Other grades may be used providedit is first ascertained that the solvent is of sufficiently high purity to permit its use without le

48、ssening the accuracy of thedetermination.7.4.1 Carbon Disulfide (CS2)(99+ % pure) may be used as a viscosity reducing solvent and as a means of reducing mass ofsample introduced onto the column to ensure linear detector response and reduced peak skewness. It is miscible with asphaltichydrocarbons an

49、d provides a relatively small response with the FID. The quality (hydrocarbon content) should be determined bythis test method prior to use as a sample diluent. (Warning Carbon disulfide is extremely flammable and toxic.)3 Reagent Chemicals, American Chemical Society Specifications, American Chemical Society, Washington, DC. For Suggestions on the testing of reagents not listed bythe American Chemical Society, see Annual Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia an