1、Designation: D 1319 08Designation: 156/97An American National StandardStandard Test Method forHydrocarbon Types in Liquid Petroleum Products byFluorescent Indicator Adsorption1This standard is issued under the fixed designation D 1319; the number immediately following the designation indicates the y
2、ear 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.This standard has been approved for use by agencies of the Depart
3、ment of Defense.1. Scope*1.1 This test method covers the determination of hydrocar-bon types over the concentration ranges from 5 to 99 volume %aromatics, 0.3 to 55 volume % olefins, and 1 to 95 volume %saturates in petroleum fractions that distill below 315C. Thistest method may apply to concentrat
4、ions outside these ranges,but the precision has not been determined. Samples containingdark-colored components that interfere in reading the chro-matographic bands cannot be analyzed.NOTE 1For the determination of olefins below 0.3 volume %, othertest methods are available, such as Test Method D 271
5、0.1.2 This test method is intended for use with full boilingrange products. Cooperative data have established that theprecision statement does not apply to narrow boiling petroleumfractions near the 315C limit. Such samples are not elutedproperly, and results are erratic.1.3 The applicability of thi
6、s test method to products derivedfrom fossil fuels other than petroleum, such as coal, shale, ortar sands, has not been determined, and the precision statementmay or may not apply to such products.1.4 This test method has two precision statements depictedin tables. The first table is applicable to u
7、nleaded fuels that donot contain oxygenated blending components. It may or maynot apply to automotive gasolines containing lead antiknockmixtures. The second table is applicable to oxygenate blended(for example, MTBE, ethanol) automotive spark ignition fuelsamples with a concentration range of 1340
8、volume percentaromatics, 433 volume percent olefins, and 4568 volumepercent saturates.1.5 The oxygenated blending components, methanol, etha-nol, methyl-tert-butylether (MTBE), tert-amylmethylether(TAME), and ethyl-tert-butylether (ETBE), do not interferewith the determination of hydrocarbon types a
9、t concentrationsnormally found in commercial blends. These oxygenatedcomponents are not detected since they elute with the alcoholdesorbent. Other oxygenated compounds shall be individuallyverified. When samples containing oxygenated blending com-ponents are analyzed, correct the results to a total-
10、sample basis.1.6 The values stated in SI units are to be regarded asstandard. No other units of measurement are included in thisstandard.1.7 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 e
11、stablish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. For specificwarning statements, see Section 7, 8.1, and 10.5.2. Referenced Documents2.1 ASTM Standards:2D86 Test Method for Distillation of Petroleum Products atAtmospheric Pres
12、sureD 1655 Specification for Aviation Turbine FuelsD 2710 Test Method for Bromine Index of Petroleum Hy-drocarbons by Electrometric TitrationD 3663 Test Method for Surface Area of Catalysts andCatalyst CarriersD 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4815 Test Method f
13、or Determination of MTBE, ETBE,TAME, DIPE, tertiary-Amyl Alcohol and C1to C4Alco-hols in Gasoline by Gas ChromatographyD 5599 Test Method for Determination of Oxygenates inGasoline by Gas Chromatography and Oxygen SelectiveFlame Ionization Detection1This test method is under the jurisdiction of ASTM
14、 Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.04.0C on Liquid Chromatography.In the IP, this test method is under the jurisdiction of the StandardizationCommittee. This test method has been approved by the sponsoring committees andaccepted by
15、the cooperating societies in accordance with established procedures.Current edition approved Oct. 15, 2008. Published October 2008. Originallyapproved in 1954. Last previous edition approved in 2003 as D 1319031.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Cus
16、tomer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocke
17、n, PA 19428-2959, United States.E11 Specification for Wire Cloth and Sieves for TestingPurposes2.2 Other Standards:GC/OFID EPA Test MethodOxygen and Oxygenate Con-tent Analysis3BS 4101:2000 Test sieves. Technical requirements andtesting. Test sieves of metal wire cloth43. Terminology3.1 Definitions
18、of Terms Specific to This Standard:3.1.1 aromaticsthe volume % of monocyclic and polycy-clic aromatics, plus aromatic olefins, some dienes, compoundscontaining sulfur and nitrogen, or higher boiling oxygenatedcompounds (excluding those listed in 1.5).3.1.2 olefinsthe volume % of alkenes, plus cycloa
19、lkenes,and some dienes.3.1.3 saturatesthe volume % of alkanes, plus cycloal-kanes.4. Summary of Test Method4.1 Approximately 0.75 mL of sample is introduced into aspecial glass adsorption column packed with activated silicagel. A small layer of the silica gel contains a mixture offluorescent dyes. W
20、hen all the sample has been adsorbed on thegel, alcohol is added to desorb the sample down the column.The hydrocarbons are separated in accordance with theiradsorption affinities into aromatics, olefins, and saturates. Thefluorescent dyes are also separated selectively, with the hydro-carbon types,
21、and make the boundaries of the aromatic, olefin,and saturate zones visible under ultraviolet light. The volumepercentage of each hydrocarbon type is calculated from thelength of each zone in the column.5. Significance and Use5.1 The determination of the total volume % of saturates,olefins, and aroma
22、tics in petroleum fractions is important incharacterizing the quality of petroleum fractions as gasolineblending components and as feeds to catalytic reformingprocesses. This information is also important in characterizingpetroleum fractions and products from catalytic reforming andfrom thermal and
23、catalytic cracking as blending componentsfor motor and aviation fuels. This information is also importantas a measure of the quality of fuels, such as specified inSpecification D 1655.6. Apparatus6.1 Adsorption Columns, with precision bore (“true bore” IPdesignation) tubing, as shown on the right in
24、 Fig. 1, made ofglass and consisting of a charger section with a capillary neck,a separator section, and an analyzer section; or with standardwall tubing, as shown on the left in Fig. 1. Refer to Table 1 forcolumn tolerance limits.6.1.1 The inner diameter of the analyzer section for theprecision bor
25、e tubing shall be 1.60 to 1.65 mm. In addition thelength of an approximately 100-mm thread of mercury shallnot vary by more than 0.3 mm in any part of the analyzersection. In glass-sealing the various sections to each other,long-taper connections shall be made instead of shoulderedconnections. Suppo
26、rt the silica gel with a small piece of glasswool located between the ball and socket of the 12/2 sphericaljoint and covering the analyzer outlet. The column tip attachedto the 12/2 socket shall have a 2-mm internal diameter. Clampthe ball and socket together and ensure that the tip does nottend to
27、slide from a position in a direct line with the analyzersection during the packing and subsequent use of the column.Commercial compression-type connectors may be used tocouple the bottom of the separator section (which has been cutsquare), to the disposable 3-mm analyzer section, provided thatthe in
28、ternal geometry is essentially similar to the aforemen-tioned procedure and provides for a smooth physical transitionfrom the inner diameters of the two glass column sections.Similar commercial compression-type connectors may be em-ployed at the terminal end of the 3-mm analyzer section,having an in
29、tegral porous support to retain the silica gel.6.1.2 For convenience, adsorption columns with standardwall tubing, as shown on the left in Fig. 1, can be used. Whenusing standard wall tubing for the analyzer section, it isnecessary to select tubing of uniform bore and to provide aleakproof connectio
30、n between the separator and the analyzersections. Calibrations of standard wall tubing would be im-practical; however, any variations of 0.5 mm or greater, asmeasured by ordinary calipers, in the outside diameter alongthe tube can be taken as an indication of irregularities in theinner diameter and
31、such tubing should not be used. Prepare theglassware to retain the gel. One way to accomplish this is todraw out one end of the tubing selected for the analyzer sectionto a fine capillary. Connect the other end of the analyzer sectionto the separator section with a suitable length of vinyl tubing,ma
32、king certain that the two glass sections touch. A 30 6 5mmlength of vinyl tubing has been found to be suitable. To ensurea leakproof glass-to-vinyl seal with the analyzer section, it isnecessary to heat the upper end of the analyzer section until itis just hot enough to melt the vinyl, then insert t
33、he upper endof the analyzer section into the vinyl sleeve. Alternatively, thisseal can be made by securing the vinyl sleeve to the analyzersection by wrapping it tightly with soft wire. Commercialcompression-type connectors may be used to couple the bottomof the separator section (which has been cut
34、 square), to the3-mm analyzer section, provided that the internal geometry isessentially similar to the aforementioned procedure and pro-vides for a smooth physical transition from the inner diametersof the two glass column sections. Similar commercialcompression-type connectors may be employed at t
35、he terminalend of the 3-mm analyzer section having an integral poroussupport to retain the silica gel.6.2 Zone-Measuring DeviceThe zones may be markedwith a glass-writing pencil and the distances measured with ameter rule, with the analyzer section lying horizontally. Alter-natively, the meter rule
36、may be fastened adjacent to thecolumn. In this case, it is convenient to have each rule fitted3Code of Federal Regulations, Part 80 of Title 40, 80.46 (g); also published inthe Federal Register, Vol 59, No. 32, Feb. 16, 1994, p. 7828. No longer available.4Available from BSI British Standards, 389 Ch
37、iswick High Road, London, W44AL, United Kingdom (www.bsi-).D1319082with four movable metal index clips (Fig. 1) for marking zoneboundaries and measuring the length of each zone.6.3 Ultraviolet Light Source, with radiation predominantlyat 365 nm is required. A convenient arrangement consists ofone or
38、 two 915 or 1220-mm units mounted vertically along theapparatus. Adjust to give the best fluorescence.6.4 Electric Vibrator, for vibrating individual columns orthe frame supporting multiple columns.6.5 Hypodermic Syringe, 1 mL, graduated to 0.01 or 0.02mL, with needle 102 mm in length. Needles of No
39、. 18, 20, or22 gauge are satisfactory.6.6 Regulator(s), capable of adjusting and maintaining thepressure within the 0 to 103 kPa delivery range.7. Reagents and Materials7.1 Silica Gel,5 ,6manufactured to conform to the specifi-cations shown in Table 2. Determine the pH of the silica gel asfollows: C
40、alibrate a pH meter with standard pH 4 and pH 7buffer solutions. Place5gofthegelsample in a 250-mLbeaker. Add 100 mL of water and a stirring bar. Stir the slurryon a magnetic stirrer for 20 min and then determine the pH5If you are aware of alternative suppliers, please provide this information toAST
41、M International Headquarters. Your comments will receive careful consider-ation at a meeting of the responsible technical committee,1which you may attend.6The sole source of supply of the silica gel known to the committee at this timeis W. R. Grace and Co., Davison Chemical Div., Baltimore, MD 21203
42、; specifyCode 923.FIG. 1 Adsorption Columns with Standard Wall (left) and Precision Bore (right) Tubing in Analyzer SectionD1319083with the calibrated meter. Before use, dry the gel in a shallowvessel at 175C for 3 h. Transfer the dried gel to an air tightcontainer while still hot, and protect it th
43、ereafter from atmo-spheric moisture.NOTE 2Some batches of silica gel that otherwise meet specificationshave been found to produce olefin boundary fading. The exact reason forthis phenomenon is unknown but will affect accuracy and precision.7.2 Fluorescent Indicator Dyed Gel A standard dyedgel,5,7con
44、sisting of a mixture of recrystallized Petrol Red AB4and purified portions of the olefin and aromatic dyes obtainedby chromatographic adsorption, following a definite, uniformprocedure, and deposited on silica gel. The dyed gel shall bestored in a dark place under an atmosphere of nitrogen. Whenstor
45、ed under these conditions, the dyed gel can have a shelf lifeof at least five years. It is recommended that portions of thedyed gel be transferred as required to a smaller working vialfrom which the dyed gel is routinely taken for analyses.7.3 Isoamyl Alcohol, (3-methyl-1-butanol) 99 %.(WarningFlamm
46、able. Health hazard.)7.4 Isopropyl Alcohol, (2-propanol) minimum 99 % purity.(Warning Flammable. Health hazard.)7.5 Pressuring GasAir (or nitrogen) delivered to the topof the column at pressures controllable over the range from 0to 103 kPa gauge. (WarningCompressed gas under highpressure.)7.6 Aceton
47、e, reagent grade, residue free. (WarningFlammable. Health hazard.)7.7 Buffer Solutions, pH 4 and 7.8. Sampling8.1 Obtain a representative sample in accordance withsampling procedures in Practice D 4057. For samples thatwould meet volatility conditions of Group 2 or less of TestMethod D86, ensure tha
48、t the sample is maintained at atemperature of#4C when opening or transferring the sample.(WarningFlammable. Health hazard.)9. Preparation of Apparatus9.1 Mount the apparatus assembly in a darkened room orarea to facilitate observation of zone boundaries. For multipledeterminations, assemble an appar
49、atus that includes the ultra-violet light source, a rack to hold the columns, and a gasmanifold system with spherical joints to connect to the desirednumber of columns.10. Procedure10.1 Ensure that the silica gel is tightly packed in thecolumn and charger section (up to the appropriate level), whichincludes the appropriate amount of dyed gel (3 to 5 mm) addedto an approximately half-full separator section, prior to the startof the sample analysis. See Note 3 for specific guidance.NOTE 3One way to prepare the column for analysis is to freelysuspend th
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