1、Designation: D2892 11Standard 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 AnnexA7Test Method for the Verification of RefluxDividing Valves,1.4.8 Annex A8Practice for Conversion of ObservedVapor 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 Performanc
10、e 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 estab
11、lish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use. For specificwarning statements, see Section 10.2. Referenced Documents2.1 ASTM Standards:2D941 Test Method for Density and Relative Density (Spe-cific Gravity) of Liquids by Lipkin
12、Bicapillary Pycnom-eter3D1217 Test Method for Density and Relative Density (Spe-cific Gravity) of Liquids by Bingham PycnometerD1298 Test Method for Density, Relative Density (SpecificGravity), or API Gravity of Crude Petroleum and LiquidPetroleum Products by Hydrometer MethodD2887 Test Method for B
13、oiling Range Distribution ofPetroleum Fractions by Gas ChromatographyD3710 Test Method for Boiling Range Distribution ofGasoline and Gasoline Fractions by Gas ChromatographyD4006 Test Method for Water in Crude Oil by DistillationD4052 Test Method for Density, Relative Density, and API1This test meth
14、od is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.08 on Volatility.Current edition approved July 1, 2011. Published August 2011. Originallyapproved in 1970. Last previous edition approved in 2010 as D289210. DOI
15、:10.1520/D2892-11.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Withdrawn. The last approved version of th
16、is historical standard is referencedon www.astm.org.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.Gravity of Liquids by Digital Density MeterD4057 Practice for Manua
17、l Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD5134 Test Method for Detailed Analysis of PetroleumNaphthas through n-Nonane by Capillary Gas Chromatog-raphyD6300 Practice for Determination of Precision and BiasData for Use in Tes
18、t Methods for Petroleum Products andLubricantsD6729 Test Method 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 100MetreC
19、apillary (with Precolumn) High-Resolution Gas Chroma-tographyD6733 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 nosignif
20、icant gain or loss of heat throughout the length of thecolumn.3.1.1.1 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-ma
21、lly greater than the reflux in the head. The opposite is truewhen 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 an
22、d including n-butane, andretention of the heavier hydrocarbons.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 prese
23、nt in the sample.3.1.4 distillation pressure, nthe pressure measured 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 co
24、lumn.3.1.5.1 DiscussionIt is also known as the head tempera-ture 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, nin distillation, when the column isfilled with liquid once the
25、boilup rate obstructs the internalreflux.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
26、in kilopascals (mm Hg)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 ra
27、tio of thecondensate 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
28、design of the plates, and depends on the composition of thematerial in the column at the final cut point and on the finaltemperature.3.1.12 takeoff rate, nin distillation, the volume of productwithdrawn from the reflux divider over a specified period.3.1.13 theoretical plate, nthe section of a colum
29、n requiredto achieve 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 p
30、late that isachieved 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 400CAET in a fractionating column having an efficiency at totalreflux of at least 14, but not greater than 18, theoretical plates.4.
31、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 ratios, and the temperatu
32、resof 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 fraction areobtained. Dis
33、tillation 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 %,or both, versus AET are
34、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.5.2 This test method corr
35、esponds to the standard laboratorydistillation efficiency referred to as 15/5. The fractions pro-duced can be analyzed as produced or combined to produceD2892 112samples for analytical studies, engineering, and product qualityevaluations. The preparation and evaluation of such blends isnot part of t
36、his 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 conform to the re
37、quirements 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 size of the charge
38、, 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 bottom of the flask t
39、o ensure itsimmersion at the end of the distillation.When a second sidearmFIG. 1 ApparatusD2892 113is 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 sligh
40、tly flattened 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 th
41、e advantage 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
42、full boilup 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 propo
43、rtioning 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
44、by direct 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. Thi
45、s requires 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 immer
46、sed at the 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
47、.1.3 Fractionating 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 p
48、ackings.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 comprised of aintegral glass column and reflux divide
49、r totally enclosed in ahighly reflective vacuum jacket having a permanent vacuum ofTABLE 1 Data for n-Heptane-Methylcyclohexane Test Mixture at 75 % of Maximum Boilup and 101.3 kPa (760 mm Hg)PropakA,B,C,D,EHelipakF,G,HPerforated PlatesE,I,JWire MeshE,KColumn diameter, mm 25 50 70 25 50 25 50 25 50Packing size, mm 4 6 6 No. 2917 No. 2918 NALNALNALNALBoilup, mL/h 3 cm2650 670 675 300 350 640 660 810 1050Dynamic holdup% of packed volume 17 15.3 17.0 15 14.3 NALNAL8.0 10.0mL/theoretical plate 3.2 16 39 1.6 8.7 2.8 12.3 2.0 12.9Pressure dropkPa/
