1、Designation: D1319 14D1319 15Standard 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 U.S. Department of Defense.1. Scope*1.1 This tes
3、t method 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.315 C. Thistest method may apply to concentrations outside these ranges, but
4、the precision 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 inten
5、ded for use with full boiling range products. Cooperative data have established that the precisionstatement does not apply to narrow boiling petroleum fractions near the 315C315 C limit. Such samples are not eluted properly,and results are erratic.1.3 This test method includes a relative bias sectio
6、n based on Practice D6708 accuracy assessment between Test Method D1319and Test Method D5769 for total aromatics in spark-ignition engine fuels as a possible Test Method D1319 alternative to TestMethod D5769 for U.S. EPA spark-ignition engine fuel regulations reporting. The Practice D6708 derived co
7、rrelation equation isonly applicable for fuels in the total aromatic concentration range from 3.3 % to 34.4 % by volume as measured by Test MethodD1319 and the distillation temperature T95, at which 95 % of the sample has evaporated, ranges from 149.1 C to 196.6 C(300.3 F to 385.8 F) when tested acc
8、ording to Test Method D86.1.3.1 The applicable Test Method D5769 range for total aromatics is 3.7 % to 29.4 % by volume as reported by Test MethodD5769 and the distillation temperature T95 values, at which 95 % of the sample has evaporated, when tested according to TestMethod D86 is from 149.1 C to
9、196.6 C (300.3 F to 385.8 F).1.4 The applicability of this test method to products derived from fossil 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.1.5 This test method has two precision state
10、ments depicted in tables. The first table is applicable to unleaded fuels that do notcontain oxygenated 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
11、spark ignition fuel samples witha concentration range of 1340 13 to 40 volume percent aromatics, 433 4 to 33 volume percent olefins, and 4568 45 to 68volume percent saturates.1.6 The oxygenated blending components, methanol, ethanol, methyl-tert-butylether (MTBE), tert-amylmethylether (TAME),and eth
12、yl-tert-butylether (ETBE), do not interfere with the determination of hydrocarbon types at concentrations normally foundin commercial blends. These oxygenated components are not detected since they elute with the alcohol desorbent. Otheroxygenated compounds shall be individually verified. When sampl
13、es containing oxygenated blending components are analyzed,correct the results to a total-sample basis.1.7 WARNINGMercury has 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 h
14、ealth and corrosive to materials. Cautionshould be taken when handling mercury and mercury containing products. See the applicable product Material Safety Data Sheet(MSDS) for details and EPAs websitehttp:/www.epa.gov/mercury/faq.htmfor additional information. Users should be awarethat selling mercu
15、ry and/or mercury containing products into your state or country may be prohibited by law.1 This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of SubcommitteeD02.04.0C on Liquid Chromatography.Current e
16、dition approved Oct. 1, 2014Dec. 1, 2015. Published October 2014December 2015. Originally approved in 1954. Last previous edition approved in 20132014as D1319 13.D1319 14. DOI: 10.1520/D1319-14.10.1520/D1319-15.This document is not an ASTM standard and is intended only to provide the user of an ASTM
17、 standard an indication of what changes 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 b
18、y ASTM is to be considered the official 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 States11.8 The values stated in SI units are to be regarded as standard. No oth
19、er units of measurement are included in this standard.1.8.1 ExceptionInch-pound units in parentheses are provided for information only.1.9 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 es
20、tablish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. For specific warning statements, see Section 7, 8.1, and 10.5.2. Referenced Documents2.1 ASTM Standards:2D86 Test Method for Distillation of Petroleum Products and Liquid Fuels at A
21、tmospheric 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 Te
22、st Method 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 DetectionD5769 Test Method for Determination of
23、Benzene, Toluene, and Total Aromatics in Finished Gasolines by GasChromatography/Mass SpectrometryD6708 Practice for Statistical Assessment and Improvement of Expected Agreement Between Two Test Methods that Purportto Measure the Same Property of a MaterialE11 Specification for Woven Wire Test Sieve
24、 Cloth 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 %volume perc
25、ent of monocyclic and polycyclic aromatics, plus aromatic olefins, some dienes,compounds containing sulfur and nitrogen, or higher boiling oxygenated compounds (excluding those listed in 1.51.6).3.1.2 olefinsthe volume %volume percent of alkenes, plus cycloalkenes, and some dienes.3.1.3 saturatesthe
26、 volume %volume percent of alkanes, plus cycloalkanes.4. Summary of Test Method4.1 Approximately 0.75 mL0.75 mLof sample is introduced into a special glass adsorption column packed with activated silicagel.Asmall layer of the silica gel contains a mixture of fluorescent dyes. When all the sample has
27、 been adsorbed on the gel, alcoholis added to desorb the 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 theboundarie
28、s of the aromatic, olefin, and saturate zones visible 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 %volume percent of saturates, olefins, and aromatics
29、in petroleum fractions isimportant in characterizing the quality of petroleum fractions as gasoline blending components and as feeds to catalytic reformingprocesses. This information is also important in characterizing petroleum fractions and products from catalytic reforming and fromthermal and cat
30、alytic cracking as blending components for motor and aviation fuels. This information is also important as ameasure of the 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
31、Fig. 1, made of glassand consisting of a charger section with a capillary 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.2 For referencedASTM standards, visit theASTM website, www.astm.org,
32、 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 published in the Federal Register, Vol 59, No. 32, Feb. 16, 1
33、994, p. 7828. No longer available.4 Available from BSI British Standards, 389 Chiswick High Road, London, W4 4AL, United Kingdom (www.bsi-).D1319 1526.1.1 The inner diameter of the analyzer section for the precision bore tubing shall be 1.601.60 mm to 1.65 mm. In addition thelength of an approximate
34、ly 100-mm100 mm thread of mercury shall not vary by more than 0.3 mm 0.3 mm in any part of theanalyzer section. In glass-sealing the various sections to each other, long-taper connections shall be made instead of shoulderedconnections. Support the silica gel with a small piece of glass wool located
35、between the ball and socket of the 12/2 spherical jointand covering the analyzer outlet. The column tip attached to the 12/2 socket shall have a 2-mm2 mm internal diameter. Clamp theball and socket together and ensure that the tip does not tend to slide from a position in a direct line with the anal
36、yzer section duringthe packing and subsequent use of the column. Commercial compression-type connectors may be used to couple the bottom of theseparator section (which has been cut square), to the disposable 3-mm3 mm analyzer section, provided that the internal geometryis essentially similar to the
37、aforementioned procedure and provides for a smooth physical transition from the inner diameters ofthe two glass column sections. Similar commercial compression-type connectors may be employed at the terminal end of the3-mm3 mm analyzer section, having an integral porous support to retain the silica
38、gel.6.1.2 For convenience, adsorption columns with standard wall tubing, as shown on the left in Fig. 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
39、sections. Calibrations of standard wall tubing would be impractical; however, any variationsFIG. 1 Adsorption Columns with Standard Wall (left) and Precision Bore (right) Tubing in Analyzer SectionD1319 153of 0.5 mm 0.5 mm or greater, as measured by ordinary calipers, in the outside diameter along t
40、he tube can be taken as an indicationof irregularities 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 selected for the analyzer section to a fine capillary. Connect the other end ofthe
41、analyzer section to the separator section with a suitable length of vinyl tubing, making certain that the two glass sections touch.A 3030 mm 6 5 mm 5 mm length of vinyl tubing has been found to be suitable. To ensure a leakproof glass-to-vinyl seal withthe analyzer section, it is necessary to heat t
42、he upper end of the analyzer section until it is just hot enough to melt the vinyl, theninsert the upper end of the analyzer section into the vinyl sleeve. Alternatively, this seal can be made by securing the vinyl sleeveto the analyzer section by wrapping it tightly with soft wire. Commercial compr
43、ession-type connectors may be used to couple thebottom of the separator section (which has been cut square), to the 3-mm3 mm analyzer section, provided that the internalgeometry is essentially similar to the aforementioned procedure and provides for a smooth physical transition from the innerdiamete
44、rs of the two glass column sections. Similar commercial compression-type connectors may be employed at the terminalend of the 3-mm3 mm analyzer section having an integral porous support to retain the silica gel.6.1.3 An alternative pressuring gas connection is shown in Fig. 2. Otherwise, all adsorpt
45、ion column dimensions andrequirements are unchanged.TABLE 1 Tolerance Limits to Column DimensionsStandard Column DimensionsCharger SectionInside diameter = 12 2 mmInside diameter = 12 mm 2 mmPack gel to this level = approximately 75 mmOverall length = 150 5 mmOverall length = 150 mm 5 mmNeck Section
46、Inside diameter = 2 0.5 mmInside diameter = 2 mm 0.5 mmOverall length = 50 5 mmOverall length = 50 mm 5 mmSeparator SectionInside diameter = 5 0.5 mmInside diameter = 5 mm 0.5 mmOverall length = 190 5 mmOverall length = 190 mm 5 mmLong taper section below separatorTip outside diameter = 3.5 0.5 mmTi
47、p outside diameter = 3.5 mm 0.5 mmTip inside diameter = 2 0.5 mmTip inside diameter = 2 mm 0.5 mmOverall length = 25 2 mmOverall length = 25 mm 2 mmAnalyzer SectionInside diameter = 1.5 0.5 mmInside diameter = 1. mm5 0.5 mmStandard wall tubingOverall length = 1200 30 mmOverall length = 1200 mm 30 mm
48、Precision Bore Column DimensionsCharger sectionInside diameter = 12 2 mmInside diameter = 12 mm 2 mmPack gel to this level = approximately 75 mmOverall length = 150 5 mmOverall length = 150 mm 5 mmNeck SectionInside diameter = 2 0.5 mmInside diameter = 2 mm 0.5 mmOverall length = 50 5 mmOverall leng
49、th = 50 mm 5 mmSeparator SectionInside diameter = 5 0.5 mmInside diameter = 5 mm 0.5 mmOverall length = 190 5 mmOverall length = 190 mm 5 mmAnalyzer SectionInside diameter = 1.60-1.65 mmInside diameter = 1.60 mm -1.65 mmOverall length = 1200 30 mmOverall length = 1200 mm 30 mmTipOverall length = 30 5 mmOverall length = 30 mm 5 mmD1319 1546.2 Zone-Measuring DeviceThe zones may be marked with a glass-writing pencil and the distances measured with a meterrule, with
