1、Designation: D2892 13Standard Test Method forDistillation of Crude Petroleum (15-Theoretical PlateColumn)1This standard is issued under the fixed designation D2892; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of last r
2、evision. 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 procedure for the distillationof stabilized crude petroleum (see Note 1) to a final cuttemperat
3、ure of 400C Atmospheric Equivalent Temperature(AET). This test method employs a fractionating columnhaving an efficiency of 14 to 18 theoretical plates operated at areflux ratio of 5:1. Performance criteria for the necessaryequipment is specified. Some typical examples of acceptableapparatus are pre
4、sented in schematic form. This test methodoffers a compromise between efficiency and time in order tofacilitate the comparison of distillation data between laborato-ries.NOTE 1Defined as having a Reid vapor pressure less than 82.7 kPa(12 psi).1.2 This test method details procedures for the productio
5、n ofa liquefied gas, distillate fractions, and residuum of standard-ized quality on which analytical data can be obtained, and thedetermination of yields of the above fractions by both mass andvolume. From the preceding information, a graph of tempera-ture versus mass % distilled can be produced. Th
6、is distillationcurve corresponds to a laboratory technique, which is definedat 15/5 (15 theoretical plate column, 5:1 reflux ratio) or TBP(true boiling point).1.3 This test method can also be applied to any petroleummixture except liquefied petroleum gases, very light naphthas,and fractions having i
7、nitial boiling points above 400C.1.4 This test method contains the following annexes andappendixes:1.4.1 Annex A1Test Method for the Determination of theEfficiency of a Distillation Column,1.4.2 Annex A2Test Method for the Determination of theDynamic Holdup of a Distillation Column,1.4.3 Annex A3Tes
8、t Method for the Determination of theHeat Loss in a Distillation Column (Static Conditions),1.4.4 Annex A4Test Method for the Verification of Tem-perature Sensor Location,1.4.5 Annex A5Test Method for Determination of theTemperature Response Time,1.4.6 Annex A6Practice for the Calibration of Sensors
9、,1.4.7 Annex A7Test Method for the Verification of RefluxDividing Valves,1.4.8 Annex A8Practice for Conversion of Observed Va-por Temperature to Atmospheric Equivalent Temperature(AET),1.4.9 Appendix X1Test Method for Dehydration of aSample of Wet Crude Oil, and1.4.10 Appendix X2Practice for Perform
10、ance Check.1.5 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are for informationonly.1.6 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 es
11、tablish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. For specificwarning statements, see Section 10.1.7 WARNINGMercury has been designated by manyregulatory agencies as a hazardous material that can causecentral nervous system, kid
12、ney and liver damage. Mercury, orits vapor, may be hazardous to health and corrosive tomaterials. Caution should be taken when handling mercury andmercury containing products. See the applicable product Ma-terial Safety Data Sheet (MSDS) for details and EPAswebsitehttp:/www.epa.gov/mercury/faq.htmfo
13、r addi-tional information. Users should be aware that selling mercuryand/or mercury containing products into your state or countrymay be prohibited by law.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of Subcomm
14、itteeD02.08 on Volatility.Current edition approved May 1, 2013. Published May 2013. Originallyapproved in 1970. Last previous edition approved in 2011 as D289211a. DOI:10.1520/D2892-13.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Driv
15、e, PO Box C700, West Conshohocken, PA 19428-2959. United States12. Referenced Documents2.1 ASTM Standards:2D941 Test Method for Density and Relative Density (Spe-cific Gravity) of Liquids by Lipkin Bicapillary Pycnom-eter3D1217 Test Method for Density and Relative Density (Spe-cific Gravity) of Liqu
16、ids by Bingham PycnometerD1298 Test Method for Density, Relative Density, or APIGravity of Crude Petroleum and Liquid Petroleum Prod-ucts by Hydrometer MethodD2887 Test Method for Boiling Range Distribution of Pe-troleum Fractions by Gas ChromatographyD3710 Test Method for Boiling Range Distribution
17、 of Gaso-line and Gasoline Fractions by Gas ChromatographyD4006 Test Method for Water in Crude Oil by DistillationD4052 Test Method for Density, Relative Density, and APIGravity of Liquids by Digital Density MeterD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for
18、 Automatic Sampling of Petroleum andPetroleum ProductsD5134 Test Method for Detailed Analysis of PetroleumNaphthas through n-Nonane by Capillary Gas Chroma-tographyD6300 Practice for Determination of Precision and BiasData for Use in Test Methods for Petroleum Products andLubricantsD6729 Test Method
19、 for Determination of Individual Com-ponents in Spark Ignition Engine Fuels by 100 MetreCapillary High Resolution Gas ChromatographyD6730 Test Method for Determination of Individual Com-ponents in Spark Ignition Engine Fuels by 100MetreCapillary (with Precolumn) High-Resolution Gas Chro-matographyD6
20、733 Test Method for Determination of Individual Com-ponents in Spark Ignition Engine Fuels by 50-MetreCapillary High Resolution Gas Chromatography3. Terminology3.1 Definitions:3.1.1 adiabaticity, nthe condition in which there is nosignificant gain or loss of heat throughout the length of thecolumn.3
21、.1.1.1 DiscussionWhen distilling a mixture of com-pounds as is the case of crude petroleum, there will be a normalincrease in reflux ratio down the column. In the case whereheat losses occur in the column, the internal reflux is abnor-mally greater than the reflux in the head. The opposite is truewh
22、en the column gains heat, as with an overheated mantle.3.1.2 boilup rate, nin distillation, the quantity of vaporentering the column per unit of time.3.1.3 debutanization of crude petroleum, nthe removal ofthe light hydrocarbons up to and including n-butane, andretention of the heavier hydrocarbons.
23、3.1.3.1 DiscussionIn practice, a crude petroleum is re-garded as debutanized if the light hydrocarbon cut collected inthe cold trap contains more than 95 % of the C2to C4hydrocarbons and less than 5 % of the C5hydrocarbonsinitially present in the sample.3.1.4 distillation pressure, nthe pressure mea
24、sured asclose as possible to the point where the vapor temperature istaken, normally at the top of the condenser.3.1.5 distillation temperature, nthe temperature of thesaturated vapor measured in the head just above the fraction-ating column.3.1.5.1 DiscussionIt is also known as the head tempera-tur
25、e or the vapor temperature.3.1.6 dynamic hold-up, nin column distillation, the quan-tity of liquid held up in the column under normal operatingconditions.3.1.7 flood point, n in distillation, the point at which thevelocity of the upflowing vapors obstructs the down-comingreflux and the column sudden
26、ly fills with liquid.3.1.8 internal reflux, nin distillation, the liquid normallyrunning down inside the column.3.1.9 pressure drop, nthe difference between the pressuremeasured in the condenser and the pressure measured in thedistillation flask.3.1.9.1 DiscussionIt is expressed in kilopascals (mm H
27、g)per metre of packed height for packed columns, or kilopascals(mm Hg) overall for real plate columns. It is higher foraromatics than for paraffins, and for higher molecular weightsthan for lighter molecules, at a given boilup rate.3.1.10 reflux ratio, R, nin distillation, the ratio of thecondensate
28、 at the head of the column that is returned to thecolumn ( reflux) to that withdrawn as product.3.1.11 static hold-up or wettage, nthe quantity of liquidretained in the column after draining at the end of a distillation.3.1.11.1 DiscussionIt is characteristic of the packing orthe design of the plate
29、s, and depends on the composition of thematerial in the column at the final cut point and on the finaltemperature.3.1.12 takeoff rate, n in distillation, the volume of productwithdrawn from the reflux divider over a specified period.3.1.13 theoretical plate, nthe section of a column requiredto achie
30、ve thermodynamic equilibrium between a liquid and itsvapor.3.1.13.1 DiscussionThe height equivalent to one theoreti-cal plate (HETP) for packed columns is expressed in millime-tres. In the case of real plate columns, the efficiency isexpressed as the percentage of one theoretical plate that isachiev
31、ed on one real plate.4. Summary of Test Method4.1 A weighed sample of 1 to 30 L of stabilized crudepetroleum is distilled to a maximum temperature of 400C2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMS
32、tandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn. The last approved version of this historical standard is referencedon www.astm.org.D2892 132AET in a fractionating column having an efficiency at totalreflux of at least 14, but not greater than
33、18, theoretical plates.4.2 A reflux ratio of 5:1 is maintained at all operatingpressures, except that at the lowest operating pressures be-tween 0.674 and 0.27 kPa (5 and 2 mm Hg), a reflux ratio of2:1 is optional. In cooperative testing or in cases of dispute, thestages of low pressure, the reflux
34、ratios, and the temperaturesof cut points must be mutually agreed upon by the interestedparties prior to beginning the distillation.4.3 Observations of temperature, pressure, and other vari-ables are recorded at intervals and at the end of each cut orfraction.4.4 The mass and density of each cut or
35、fraction areobtained. Distillation yields by mass are calculated from themass of all fractions, including liquefied gas cut and theresidue. Distillation yields by volume of all fractions and theresidue at 15C are calculated from mass and density.4.5 From these data the TBP curves in mass or volume %
36、,or both, versus AET are drawn.5. Significance and Use5.1 This test method is one of a number of tests conductedon a crude oil to determine its value. It provides an estimate ofthe yields of fractions of various boiling ranges and is thereforevaluable in technical discussions of a commercial nature.
37、5.2 This test method corresponds to the standard laboratorydistillation efficiency referred to as 15/5. The fractions pro-duced can be analyzed as produced or combined to producesamples for analytical studies, engineering, and product qualityevaluations. The preparation and evaluation of such blends
38、 isnot part of this test method.5.3 This test method can be used as an analytical tool forexamination of other petroleum mixtures with the exception ofLPG, very light naphthas, and mixtures with initial boilingpoints above 400C.6. Apparatus6.1 Distillation at Atmospheric PressureAll componentsmust c
39、onform to the requirements specified as follows. Auto-matic devices can be employed provided they meet the samerequirements. A typical apparatus is illustrated in Fig. 1.6.1.1 Distillation FlaskThe distillation flask shall be of asize that is at least 50 % larger than the volume of the charge.The si
40、ze of the charge, between 1.0 and 30 L, is determined bythe holdup characteristics of the fractionating column, asshown in Table 1 and described in Annex A2. The distillationflask shall have at least one sidearm.6.1.1.1 The sidearm is used as a thermowell. It shallterminate about 5 mm from the botto
41、m of the flask to ensure itsimmersion at the end of the distillation.When a second sidearmis present, it can be used for pressure drop detection with anitrogen bleed or for mechanical stirring, or both.6.1.1.2 If a magnetic stirrer is used with a spherical flask,the flask shall have a slightly flatt
42、ened or concave area at thebottom on which the magnetic stirrer can rotate withoutgrinding the glass. In this case, termination of the thermowellshall be off center 40 6 5 mm to avoid the magnetic stirringbar. Boiling chips can be used as an alternative to a stirrer.6.1.1.3 (WarningWhile the advanta
43、ge of visibility inglass distillation flasks is desirable, flasks of glass may becomehazardous the larger the charge they contain. For this reason,glass flasks of a volume greater than 10 L are not recom-mended.)6.1.2 Heating SystemHeating of the flask shall be pro-vided in such a way that full boil
44、up can be maintained at asteady rate at all pressure levels. An electric heating mantlecovering the lower half of the flask and having one third of theheat in an element located in the bottom central area and theremaining two thirds in the rest of the hemisphere is recom-mended. While proportioning
45、controllers are preferred, heatinput can be manually adjusted by use of a variable autotransformer on each circuit, the smaller heater being automati-cally controlled by an instrument sensing the pressure drop ofthe column as registered in a differential pressure instrument oralternatively by direct
46、 measurement of distillation rate.6.1.2.1 Minimum wattage required to provide full boilup ofcrude petroleum is approximately 0.125 W/mL of charge.Twice this amount is recommended for quick heat-up.6.1.2.2 The heat density in the flask heaters is approxi-mately equal to 0.5 to 0.6 W/cm2. This require
47、s the use ofnickel reinforced quartz fabric to ensure a reasonable servicelife.6.1.2.3 Immersion heaters can be employed in a similar wayand have the advantage of faster response, but they are morefragile and require a specially designed flask to ensure that theheating elements remain immersed at th
48、e end of the run. Whenused, their heat density should be approximately equal to 4W/cm2.6.1.2.4 The upper half of the flask shall be covered with amantle to avoid unnecessary heat losses from the upper surfaceand shall have an electric heater supplying about 0.25 W/cm2at full-rated voltage.6.1.3 Frac
49、tionating ColumnThe fractionating columnmust contain either particulate packing or real plates similar tothose whose performance characteristics are summarized inTable 1 and meet the specifications stated in 6.1.3.1 through6.1.3.4. Table 2 lists current North American suppliers ofsuitable packings.6.1.3.1 The internal diameter shall be between 25 and 70mm.6.1.3.2 The efficiency shall be between 14 and 18 theoreti-cal plates at total reflux when measured by the proceduredescribed in Annex A1.6.1.3.3 The fractionating column shall be compri
