1、Designation: D2892 18Standard 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 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 pr
4、esented 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 producti
5、on 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. T
6、his 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 A3T
8、est 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 Senso
9、rs,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 Perfo
10、rmance 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 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It i
11、s theresponsibility of the user of this standard to 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 10.1.7 WARNINGMercury has been designated by manyregulatory agen
12、cies as a hazardous material that can causecentral nervous system, kidney, 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 Shee
13、t (MSDS) for details and EPAswebsitehttp:/www.epa.gov/mercury/faq.htmfor addi-tional information. Users should be aware that selling mercuryand/or mercury containing products into your state or countrymay be prohibited by law.1.8 This international standard was developed in accor-dance with internat
14、ionally recognized principles on standard-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
15、 Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.08 on Volatility.Current edition approved April 1, 2018. Published April 2018. Originallyapproved in 1970. Last previous edition approved in 2017 as D2892 17a. DOI:10.1520/D2892-18.*
16、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 StatesThis international standard was developed in accordance with internationally recognized principles on standardization estab
17、lished in the Decision on Principles 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 G
18、ravity) of Liquids by Lipkin Bicapillary 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
19、Method for Boiling Range Distribution 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, Relativ
20、e Density, and APIGravity of Liquids 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 Chr
21、oma-tographyD6300 Practice for Determination 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 fo
22、r Determination of Individual Com-ponents 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. Ter
23、minology3.1 Definitions:3.1.1 adiabaticity, 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 colu
24、mn. 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 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.
25、1.3 debutanization of crude petroleum, 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 9
26、5 % of the C2to C4hydrocarbons and 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 te
27、mperature 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-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 operatingcondition
28、s.3.1.7 flood point, nin distillation, 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 betw
29、een the pressuremeasured in the condenser 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
30、for higher molecular weightsthan for 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 liquidr
31、etained 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 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,
32、the volume of productwithdrawn from 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
33、 expressed in millime-tres. In the 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
34、Book of ASTMStandards 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.4The last approved version of this historical standard is referenced onwww.astm.org.D2892 1824. Sum
35、mary of Test Method4.1 A weighed sample 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 a
36、ll operatingpressures, except that 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 a
37、greed upon by theinterested parties 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 calcul
38、ated from themass of all fractions, 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 Us
39、e5.1 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 corresponds to the standard labo
40、ratorydistillation 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 isnot part of this test method.5.3 This test method
41、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 400 C.6. Apparatus6.1 Distillation at Atmospheric PressureAll componentsmust conform to the requirements specified as follows. Aut
42、o-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, between 1.0 L and 30 L, is determi
43、nedby the 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 to ensure itsimmersion at the end o
44、f 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 flattened or concave area at thebottom on which the mag
45、netic stirrer can rotate withoutgrinding 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
46、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 boilup can be maintained at asteady rate at all pres
47、sure 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 controllers are preferred, heatinput can be manu
48、ally 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 measurement of distillation rate.6.1.2.1 Minimu
49、m wattage required to provide full 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 i
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