1、Designation: D1319 10D1319 13Standard Test Method forHydrocarbon Types in Liquid Petroleum Products byFluorescent Indicator Adsorption1This standard is issued under the fixed designation D1319; the number immediately following the designation indicates the year oforiginal adoption or, in the case of
2、 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 test met
3、hod covers the determination of hydrocarbon 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. This testmethod may apply to concentrations outside these ranges, but the precisi
4、on has not been determined. Samples containingdark-colored components that interfere in reading the chromatographic bands cannot be analyzed.NOTE 1For the determination of olefins below 0.3 volume %, other test methods are available, such as Test Method D2710.1.2 This test method is intended for use
5、 with full boiling range products. Cooperative data have established that the precisionstatement does not apply to narrow boiling petroleum fractions near the 315C limit. Such samples are not eluted properly, andresults are erratic.1.3 The applicability of this test method to products derived from f
6、ossil fuels other than petroleum, such as coal, shale, or tarsands, has not been determined, and the precision statement may or may not apply to such products.1.4 This test method has two precision statements depicted in tables. The first table is applicable to unleaded fuels that do notcontain oxyg
7、enated blending components. It may or may not apply to automotive gasolines containing lead antiknock mixtures.The second table is applicable to oxygenate blended (for example, MTBE, ethanol) automotive spark ignition fuel samples witha concentration range of 1340 volume percent aromatics, 433 volum
8、e percent olefins, and 4568 volume percent saturates.1.5 The oxygenated blending components, methanol, ethanol, methyl-tert-butylether (MTBE), tert-amylmethylether (TAME),and ethyl-tert-butylether (ETBE), do not interfere with the determination of hydrocarbon types at concentrations normally foundin
9、 commercial blends. These oxygenated components are not detected since they elute with the alcohol desorbent. Otheroxygenated compounds shall be individually verified. When samples containing oxygenated blending components are analyzed,correct the results to a total-sample basis.1.6 WARNINGMercury h
10、as been designated by many regulatory agencies as a hazardous material that can cause centralnervous system, kidney and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Cautionshould be taken when handling mercury and mercury containing products. See the ap
11、plicable product Material Safety Data Sheet(MSDS) for details and EPAs websitehttp:/www.epa.gov/mercury/faq.htmfor additional information. Users should be awarethat selling mercury and/or mercury containing products into your state or country may be prohibited by law.1.7 The values stated in SI unit
12、s are to be regarded as standard. No other units of measurement are included in this standard.1.8 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 pra
13、ctices and determine the applicability of regulatorylimitations prior to use. For specific warning statements, see Section 7, 8.1, and 10.5.1 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.
14、0Con Liquid Chromatography.In the IP, this test method is under the jurisdiction of the Standardization Committee. This test method has been approved by the sponsoring committees and accepted bythe cooperating societies in accordance with established procedures.Current edition approved May 1, 2010Ma
15、y 1, 2013. Published June 2010June 2013. Originally approved in 1954. Last previous edition approved in 20082010 asD1319D1319 10.08. DOI: 10.1520/D1319-10.10.1520/D1319-13.This document is not an ASTM standard and is intended only to provide the user of an ASTM standard an indication of what changes
16、 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 official
17、 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 States12. Referenced Documents2.1 ASTM Standards:2D86 Test Method for Distillation of Petroleum Products at Atmospheri
18、c PressureD1655 Specification for Aviation Turbine FuelsD2710 Test Method for Bromine Index of Petroleum Hydrocarbons by Electrometric TitrationD3663 Test Method for Surface Area of Catalysts and Catalyst CarriersD4057 Practice for Manual Sampling of Petroleum and Petroleum ProductsD4815 Test Method
19、 for Determination of MTBE, ETBE, TAME, DIPE, tertiary-Amyl Alcohol and C1 to C4 Alcohols inGasoline by Gas ChromatographyD5599 Test Method for Determination of Oxygenates in Gasoline by Gas Chromatography and Oxygen Selective FlameIonization DetectionE11 Specification for Woven Wire Test Sieve Clot
20、h and Test Sieves2.2 Other Standards:GC/OFID EPA Test MethodOxygen and Oxygenate Content Analysis3BS 4101:2000 Test sieves. Technical requirements and testing. Test sieves of metal wire cloth43. Terminology3.1 Definitions of Terms Specific to This Standard:3.1.1 aromaticsthe volume % of monocyclic a
21、nd polycyclic aromatics, plus aromatic olefins, some dienes, compoundscontaining sulfur and nitrogen, or higher boiling oxygenated compounds (excluding those listed in 1.5).3.1.2 olefinsthe volume % of alkenes, plus cycloalkenes, and some dienes.3.1.3 saturatesthe volume % of alkanes, plus cycloalka
22、nes.4. Summary of Test Method4.1 Approximately 0.75 mL of sample is introduced into a special glass adsorption column packed with activated silica gel. Asmall layer of the silica gel contains a mixture of fluorescent dyes. When all the sample has been adsorbed on the gel, alcohol isadded to desorb t
23、he sample down the column. The hydrocarbons are separated in accordance with their adsorption affinities intoaromatics, olefins, and saturates. The fluorescent dyes are also separated selectively, with the hydrocarbon types, and make theboundaries of the aromatic, olefin, and saturate zones visible
24、under ultraviolet light. The volume percentage of each hydrocarbontype is calculated from the length of each zone in the column.5. Significance and Use5.1 The determination of the total volume % of saturates, olefins, and aromatics in petroleum fractions is important incharacterizing the quality of
25、petroleum fractions as gasoline blending components and as feeds to catalytic reforming processes.This information is also important in characterizing petroleum fractions and products from catalytic reforming and from thermaland catalytic cracking as blending components for motor and aviation fuels.
26、 This information is also important as a measure ofthe quality of fuels, such as specified in Specification D1655.6. Apparatus6.1 Adsorption Columns, with precision bore (“true bore” IP designation) tubing, as shown on the right in Fig. 1, made of glassand consisting of a charger section with a capi
27、llary neck, a separator section, and an analyzer section; or with standard wall tubing,as shown on the left in Fig. 1. Refer to Table 1 for column tolerance limits.6.1.1 The inner diameter of the analyzer section for the precision bore tubing shall be 1.60 to 1.65 mm. In addition the lengthof an app
28、roximately 100-mm thread of mercury shall not vary by more than 0.3 mm in any part of the analyzer section. Inglass-sealing the various sections to each other, long-taper connections shall be made instead of shouldered connections. Supportthe silica gel with a small piece of glass wool located betwe
29、en the ball and socket of the 12/2 spherical joint and covering theanalyzer outlet. The column tip attached to the 12/2 socket shall have a 2-mm internal diameter. Clamp the ball and socket togetherand ensure that the tip does not tend to slide from a position in a direct line with the analyzer sect
30、ion during the packing andsubsequent use of the column. Commercial compression-type connectors may be used to couple the bottom of the separator section(which has been cut square), to the disposable 3-mm analyzer section, provided that the internal geometry is essentially similarto the aforementione
31、d procedure and provides for a smooth physical transition from the inner diameters of the two glass columnsections. Similar commercial compression-type connectors may be employed at the terminal end of the 3-mm analyzer section,having an integral porous support to retain the silica gel.2 For referen
32、cedASTM 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 on the ASTM website.3 Code of Federal Regulations, Part 80 of Title 40, 80.46 (g); also publis
33、hed in the Federal Register, Vol 59, No. 32, Feb. 16, 1994, p. 7828. No longer available.4 Available from BSI British Standards, 389 Chiswick High Road, London, W4 4AL, United Kingdom (www.bsi-).D1319 1326.1.2 For convenience, adsorption columns with standard wall tubing, as shown on the left in Fig
34、. 1, can be used. When usingstandard wall tubing for the analyzer section, it is necessary to select tubing of uniform bore and to provide a leakproof connectionbetween the separator and the analyzer sections. Calibrations of standard wall tubing would be impractical; however, any variationsof 0.5 m
35、m or greater, as measured by ordinary calipers, in the outside diameter along the tube can be taken as an indication ofirregularities in the inner diameter and such tubing should not be used. Prepare the glassware to retain the gel. One way toaccomplish this is to draw out one end of the tubing sele
36、cted for the analyzer section to a fine capillary. Connect the other end ofthe analyzer section to the separator section with a suitable length of vinyl tubing, making certain that the two glass sections touch.A 30 6 5 mm length of vinyl tubing has been found to be suitable. To ensure a leakproof gl
37、ass-to-vinyl seal with the analyzersection, it is necessary to heat the upper end of the analyzer section until it is just hot enough to melt the vinyl, then insert the upperend of the analyzer section into the vinyl sleeve. Alternatively, this seal can be made by securing the vinyl sleeve to the an
38、alyzersection by wrapping it tightly with soft wire. Commercial compression-type connectors may be used to couple the bottom of theseparator section (which has been cut square), to the 3-mm analyzer section, provided that the internal geometry is essentiallysimilar to the aforementioned procedure an
39、d provides for a smooth physical transition from the inner diameters of the two glasscolumn sections. Similar commercial compression-type connectors may be employed at the terminal end of the 3-mm analyzersection having an integral porous support to retain the silica gel.FIG. 1 Adsorption Columns wi
40、th Standard Wall (left) and Precision Bore (right) Tubing in Analyzer SectionD1319 1336.2 Zone-Measuring DeviceThe zones may be marked with a glass-writing pencil and the distances measured with a meterrule, with the analyzer section lying horizontally.Alternatively, the meter rule may be fastened a
41、djacent to the column. In this case,it is convenient to have each rule fitted with four movable metal index clips (Fig. 1) for marking zone boundaries and measuringthe length of each zone.6.3 Ultraviolet Light Source, with radiation predominantly at 365 nm is required. A convenient arrangement consi
42、sts of one ortwo 915 or 1220-mm units mounted vertically along the apparatus. Adjust to give the best fluorescence.6.4 Electric Vibrator, for vibrating individual columns or the frame supporting multiple columns.6.5 Hypodermic Syringe, 1 mL, graduated to 0.01 or 0.02 mL, with needle 102 mm in length
43、. Needles of No. 18, 20, or 22 gaugeare satisfactory.6.6 Regulator(s), capable of adjusting and maintaining the pressure within the 0 to 103 kPa delivery range.7. Reagents and Materials7.1 Silica Gel,5,manufactured to conform to the specifications shown in Table 2. Determine the pH of the silica gel
44、 as follows:Calibrate a pH meter with standard pH 4 and pH 7 buffer solutions. Place 5 g of the gel sample in a 250-mL beaker. Add 100 mLof water and a stirring bar. Stir the slurry on a magnetic stirrer for 20 min and then determine the pH with the calibrated meter.Before use, dry the gel in a shal
45、low vessel at 175C for 3 h.Transfer the dried gel to an air tight container while still hot, and protectit thereafter from atmospheric moisture.NOTE 2Some batches of silica gel that otherwise meet specifications have been found to produce olefin boundary fading. The exact reason for thisphenomenon i
46、s unknown but will affect accuracy and precision.7.2 Fluorescent Indicator Dyed GelA standard dyed gel,5,6 consisting of a mixture of recrystallized Petrol Red AB4 andpurified portions of the olefin and aromatic dyes obtained by chromatographic adsorption, following a definite, uniform procedure,5 I
47、f you are aware of alternative suppliers, please provide this information to ASTM International Headquarters. Your comments will receive careful consideration at ameeting of the responsible technical committee,1 which you may attend.6 The sole source of supply of the silica gel known to the committe
48、e at this time is W. R. Grace and Co., Davison Chemical Div., Baltimore, MD 21203; specify Code923.6 The sole source of supply of the standard dyed gel known to the committee at this time is produced by UOP LLC, and distributed byAdvanced Specialty Gas EquipmentInc, 241 Lackland Drive, Middlesex, Ne
49、w Jersey 08846. Request “FIA Standard Dyed Gel,” UOP LLC Product No. 80675.TABLE 1 Tolerance Limits to Column DimensionsStandard Column DimensionsCharger SectionInside diameter = 12 2 mmPack gel to this level = approximately 75 mmOverall length = 150 5 mmNeck SectionInside diameter = 2 0.5 mmOverall length = 50 5 mmSeparator SectionInside diameter = 5 0.5 mmOverall length = 190 5 mmLong taper section below separatorTip outside diameter = 3.5 0.5 mmTip inside diameter = 2 0.5 mmOverall length = 25 2 mmAnalyzer SectionInside diamete
