1、Designation: D 2892 05An American National StandardStandard Test Method forDistillation of Crude Petroleum (15-Theoretical PlateColumn)1This standard is issued under the fixed designation D 2892; the number immediately following the designation indicates the year oforiginal adoption or, in the case
2、of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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 (se
3、e Note 1) to a final cuttemperature 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 example
4、s of acceptableapparatus are presented 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 deta
5、ils procedures for the production 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
6、 % distilled can be produced. 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
7、 naphthas,and fractions having initial 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 Disti
8、llation Column,1.4.3 Annex A3Test 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 A6Practic
9、e for the Calibration of Sensors,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 Ap
10、pendix X2Practice for Performance 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 th
11、e user of this standard to establish 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:2D 941 Test Method for Density and Relative Density (Spe-cif
12、ic Gravity) of Liquids by Lipkin Bicapillary Pycnom-eter3D 1217 Test Method for Density and Relative Density(Specific Gravity) of Liquids by Bingham PycnometerD 1298 Test Method for Density, Relative Density (SpecificGravity), or API Gravity of Crude Petroleum and LiquidPetroleum Products by Hydrome
13、ter MethodD 2887 Test Method for Boiling Range Distribution ofPetroleum Fractions by Gas ChromatographyD 3710 Test Method for Boiling Range Distribution ofGasoline and Gasoline Fractions by Gas ChromatographyD 4006 Test Method for Water in Crude Oil by DistillationD 4052 Test Method for Density and
14、Relative Density of1This test method 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 Nov. 1, 2005. Published November 2005. Originallyapproved in 1970. Last previous edit
15、ion approved in 2003 as D 289203a.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.1*A Summary of C
16、hanges 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.Liquids by Digital Density MeterD 4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4177 Practice for Automatic Sam
17、pling of Petroleum andPetroleum ProductsD 5134 Test Method for Detailed Analysis of PetroleumNaphthas through n-Nonane by Capillary Gas Chromatog-raphyD 6729 Test Method for Determination of Individual Com-ponents in Spark Ignition Engine Fuels by 100 MeterCapillary High Resolution Gas Chromatograph
18、yD 6730 Test Method for Determination of Individual Com-ponents in Spark Ignition Engine Fuels by 100-MetreCapillary (with Precolumn) High-Resolution Gas Chroma-tographyD 6733 Test Method for Determination of Individual Com-ponents in Spark Ignition Engine Fuels by 50-MeterCapillary High Resolution
19、Gas Chromatography3. Terminology3.1 Definitions:3.1.1 adiabaticitythe condition in which there is no sig-nificant 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 ref
20、lux 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 truewhen the column gains heat, as with an overheated mantle.3.1.2 boilup ratethe quantity of vapor entering the col-umn per unit of ti
21、me.3.1.2.1 DiscussionIt is expressed in millilitres of liquidper hour for a given column or in millilitres per hour per squarecentimetre of cross-sectional area for comparative purposes. Inthe latter case, it refers to the test mixture of n-heptane andmethylcyclohexane in the efficiency evaluation (
22、seeAnnexA1)and is measured at the bottom of the column. The maximumboilup of the n-heptane-methylcyclohexane test mixture is thatwhich the column can handle under stable conditions withoutflooding. In routine adiabatic operation, the boilup rate can beestimated roughly from the takeoff rate multipli
23、ed by the refluxratio plus one.3.1.3 debutanization of crude petroleumthe 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
24、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 pressurethe pressure measured as closeas possible to the point where the vapor temperature is taken,normally at the top of the condenser.3.1.5 distil
25、lation temperaturethe temperature of the satu-rated vapor measured in the head just above the fractionatingcolumn.3.1.5.1 DiscussionIt is also known as the head tempera-ture or the vapor temperature.3.1.6 dynamic hold-upthe quantity of liquid held up in thecolumn under normal operating conditions.3.
26、1.6.1 DiscussionIt is expressed as a percentage of thepacked volume for packed columns so that the data can becompared. For real plate columns, it is expressed in millilitresper plate. The data can only be compared with others of thesame diameter because of different tray spacing. Data forpacked col
27、umns cannot be compared with those of real platecolumns except in absolute units of millilitres per theoreticalplate (see Table 1). Dynamic hold-up increases with increasingdistillation rate up to the flood point and varies from one kindof fractionator to another.3.1.7 flood pointthe point at which
28、the velocity of theupflowing vapors obstructs the downcoming reflux and thecolumn suddenly loads with liquid.3.1.7.1 DiscussionUnder these conditions no vapor canreach the head and the heat to the distillation flask must bereduced to establish normal operations again.The flood point isnormally deter
29、mined during the efficiency evaluation of acolumn using the n-heptane-methylcyclohexane test mixture(see Annex A1).3.1.8 internal refluxthe liquid normally running downinside the column.3.1.8.1 DiscussionIn the case of an adiabatic columnwhen distilling a pure compound, the internal reflux is consta
30、ntfrom top to bottom and is equal to the reflux at the refluxdivider. When distilling crude petroleum, the fractionationoccurring in the dynamic holdup will cause a temperaturegradient to be established with attendant greater amount ofinternal reflux at the bottom of the column.3.1.9 pressure dropth
31、e difference between 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 fo
32、r paraffins, and for higher molecular weightsthan for lighter molecules, at a given boilup rate.3.1.10 reflux ratio, Rthe ratio of reflux to distillate.3.1.10.1 DiscussionThe vapor reaching the top of thecolumn is totally condensed and the resulting liquid is dividedinto two parts. One part L (reflu
33、x), is returned to the columnand the other part, D (distillate), is withdrawn as product. Thereflux ratio ( R = L/D), can vary from zero at total takeoff(L=0) to infinity at total reflux (D=0).3.1.11 static hold-up or wettagethe quantity of liquidretained in the column after draining at the end of a
34、 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 ratethe rate of product takeoff from thereflux divider expressed in millilitr
35、es per hour.3.1.13 theoretical platethe section of a column requiredto achieve thermodynamic equilibrium between a liquid and itsvapor.D28920523.1.13.1 DiscussionThe height equivalent to one theoreti-cal plate (HETP) for packed columns is expressed in millime-tres. In the case of real plate columns,
36、 the efficiency isexpressed as the percentage of one theoretical plate 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 totalref
37、lux 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 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 disput
38、e, thestages of low pressure, the reflux 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
39、.4.4 The mass and density of each cut or 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 thes
40、e data the TBP curves in mass or volume %,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 tech
41、nical discussions of a commercial nature.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
42、preparation and evaluation of such blends 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
43、 Atmospheric PressureAll componentsmust conform 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 % la
44、rger than the volume of the charge.The size 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.TABLE 1 Data for n-Heptane-Methylcyclohexane Te
45、st 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 packe
46、d 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/m 1.2 1.05 0.94 1.53 1.41 NALNAL0.97 0.75mm Hg/m 9.0 7.9 7.1 11.5 10.6 NALNAL7.3 5.6kPa/theoretical plate 0.045 0.056 0.06 0.03 0.045 0.15 0.16 0.05 0.05mm Hg/theoretical plate 0.34 0
47、.42 0.43 0.24 0.34 1.1 1.2 0.35 0.37HETP, mm (% of real plates) 38 53 61 21 32 (60 %) (65 %) 48 66For 15-plate TowersPacked height, cm (plates) 57 80 91 31.5 48 (25) (23) 72 99Packed volume, mL 280 1570 3460 155 917 NALNAL353 1940Dynamic holdup, mL 47 240 590 23 131 42 184 28 194Pressure dropkPa 0.6
48、8 0.84 0.86 0.48 0.68 2.2 2.4 0.70 0.73mm Hg 5.1 6.3 6.5 3.6 5.1 16.5 18.0 5.3 5.5Charge volume, LMin (4 % Holdup) 1.2 6.0 15 0.575 3.3 1.0 4.6 0.7 4.9Max (1 % Holdup) 4.8 24.0 60 2.3 13.0 4.2 10.4 2.8 19.4ACooke, G. M. and Jameson, B. G. Analytical Chemistry, Vol 27, 1955, p. 1798.BStruck, R. T. an
49、d Kinner, C. R. Industrial and Engineering Chemistry, Vol 42, 1950, p. 77.CCannon, M. R. Industrial and Engineering Chemistry, Vol 41, No. 9, 1949, p. 1953.DBulletin 23, Scientific Development Co. P.O. Box 795, State College, PA 16801.ECooke, G. M. Analytical Chemistry, Vol 39, 1967, p. 286.FBulletin of Podbielniak Div. of Reliance Glass Works, P.O. Box 825, Bensenville, IL 60106.GFeldman, J., et al, Industrial and Engineering Chemistry, Vol 45, January 1953, p. 214.HHelipak Performance Characteristics, Begemean, C. R. and Turkal, P. J. (Labora
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