1、Designation: D2892 18aStandard 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
2、revision. 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 cuttempera
3、ture of 400 C 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 p
4、resented 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 product
5、ion 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.
6、This 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
7、 initial boiling points above 400 C.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 A3
8、Test 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 Sens
9、ors,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 Perf
10、ormance Check.1.5 The values stated in SI units are to be regarded asstandard. The values given in parentheses after SI units areprovided for information only and are not considered standard.1.6 WARNINGMercury has been designated by manyregulatory agencies as a hazardous substance that can causeseri
11、ous medical issues. Mercury, or its vapor, has been dem-onstrated to be hazardous to health and corrosive to materials.Use Caution when handling mercury and mercury-containingproducts. See the applicable product Safety Data Sheet (SDS)for additional information. The potential exists that sellingmerc
12、ury or mercury-containing products, or both, is prohibitedby local or national law. Users must determine legality of salesin their location.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 t
13、o establish appro-priate safety, health, and environmental practices and deter-mine the applicability of regulatory limitations prior to use.For specific warning statements, see Section 10.1.8 This international standard was developed in accor-dance with internationally recognized principles on stan
14、dard-ization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recom-mendations issued by the World Trade Organization TechnicalBarriers to Trade (TBT) Committee.1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products,
15、Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.08 on Volatility.Current edition approved Dec. 1, 2018. Published December 2018. Originallyapproved in 1970. Last previous edition approved in 2018 as D2892 18. DOI:10.1520/D2892-18A.*A Summary of Changes section appear
16、s at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principle
17、s for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.12. Referenced Documents2.1 ASTM Standards:2D941 Test Method for Density and Relative Density (Spe-cific Gravity) of Liquids by Lipkin Bicapi
18、llary Pycnom-eter3D1217 Test Method for Density and Relative Density (Spe-cific Gravity) of Liquids 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 Distributi
19、on of Pe-troleum Fractions by Gas ChromatographyD3710 Test Method for Boiling Range Distribution of Gaso-line and Gasoline Fractions by Gas Chromatography(Withdrawn 2014)4D4006 Test Method for Water in Crude Oil by DistillationD4052 Test Method for Density, Relative Density, and APIGravity of Liquid
20、s by Digital Density MeterD4057 Practice for Manual 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 Chroma-tographyD6300 Practice for Dete
21、rmination of Precision and BiasData for Use in Test 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-p
22、onents in Spark Ignition Engine Fuels by 100MetreCapillary (with Precolumn) High-Resolution Gas Chro-matographyD6733 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 adiab
23、aticity, nthe condition in which there is nosignificant 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 oc
24、cur in the column, the internal reflux is abnor-mally 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 petrole
25、um, nthe removal ofthe light hydrocarbons up to and 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
26、less than 5 % of the C5hydrocarbonsinitially present 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 mea
27、sured in the head just above the fraction-ating column.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 distillati
28、on, the point at which thevelocity of the upflowing vapors obstructs the down-comingreflux and the column suddenly 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 con
29、denser and the pressure measured in thedistillation flask.3.1.9.1 DiscussionIt is expressed 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 fo
30、r lighter molecules, at a given boilup rate.3.1.10 reflux ratio, R, nin distillation, the ratio 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 drainin
31、g at the end of a distillation.3.1.11.1 DiscussionIt is characteristic of the packing orthe 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, n in distillation, the volume of productwithdrawn from
32、 the reflux divider over a specified period.3.1.13 theoretical plate, nthe section of a column 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
33、case of real plate columns, the efficiency isexpressed as the percentage of one theoretical plate that isachieved on one real plate.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume inform
34、ation, refer to the standards Document Summary page onthe ASTM website.3Withdrawn. The last approved version of this historical standard is referencedon www.astm.org.4The last approved version of this historical standard is referenced onwww.astm.org.D2892 18a24. Summary of Test Method4.1 A weighed s
35、ample of 1 L to 30 L of stabilized crudepetroleum is distilled to a maximum temperature of 400 CAET in a fractionating column having an efficiency at totalreflux of at least 14, but not greater than 18, theoretical plates.4.2 A reflux ratio of 5:1 is maintained at all operatingpressures, except that
36、 at the lowest operating pressures be-tween 0.674 kPa and 0.27 kPa (5 mm and 2 mm Hg), a refluxratio of 2:1 is optional. In cooperative testing or in cases ofdispute, the stages of low pressure, the reflux ratios, and thetemperatures of cut points must be mutually agreed upon by theinterested partie
37、s 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. Distillation yields by mass are calculated from themass of all fractions
38、, including liquefied gas cut and theresidue. Distillation yields by volume of all fractions and theresidue at 15 C are calculated from mass and density.4.5 From these data the TBP curves in mass or volumepercent, or both, versus AET are drawn.5. Significance and Use5.1 This test method is one of a
39、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 corresponds to the standard laboratorydistillation efficiency refe
40、rred 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 isnot part of this test method.5.3 This test method can be used as an analytical tool
41、forexamination of other petroleum mixtures with the exception ofLPG, very light naphthas, and mixtures with initial boilingpoints above 400 C.6. Apparatus6.1 Distillation at Atmospheric PressureAll componentsmust conform to the requirements specified as follows. Auto-matic devices can be employed pr
42、ovided 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, between 1.0 L and 30 L, is determinedby the holdup characteristics o
43、f 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 to ensure itsimmersion at the end of the distillation.When a second s
44、idearmis 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 flattened or concave area at thebottom on which the magnetic stirrer can rotate withoutgr
45、inding the glass. In this case, termination of the thermowellshall be off center 40 mm 6 5 mm to avoid the magneticstirring bar. Boiling chips can be used as an alternative to astirrer.6.1.1.3 (WarningWhile the advantage of visibility inglass distillation flasks is desirable, flasks of glass may bec
46、omehazardous 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 boilup can be maintained at asteady rate at all pressure levels. An electric heating m
47、antlecovering 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 controllers are preferred, heatinput can be manually adjusted by use of a variable
48、 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 measurement of distillation rate.6.1.2.1 Minimum wattage required to provide full
49、 boilup ofcrude petroleum is approximately 0.125 WmL 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 Wcm2to 0.6 Wcm2. This requires the useof nickel-reinforced quartz fabric to ensure a reasonableservice life.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 the end of the run. Whenuse
