1、Designation:D289211 Designation: D2892 11aStandard 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 revisio
2、n, the year of last 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 distillation of stabilized crude petroleum (see Note 1)
3、to a final cut temperatureof 400C Atmospheric Equivalent Temperature (AET). This test method employs a fractionating column having an efficiency of14 to 18 theoretical plates operated at a reflux ratio of 5:1. Performance criteria for the necessary equipment is specified. Sometypical examples of acc
4、eptable apparatus are presented in schematic form.This test method offers a compromise between efficiencyand time in order to facilitate the comparison of distillation data between laboratories.NOTE 1Defined as having a Reid vapor pressure less than 82.7 kPa (12 psi).1.2 This test method details pro
5、cedures for the production of a liquefied gas, distillate fractions, and residuum of standardizedquality on which analytical data can be obtained, and the determination of yields of the above fractions by both mass and volume.From the preceding information, a graph of temperature versus mass % disti
6、lled can be produced. This distillation curvecorresponds to a laboratory technique, which is defined at 15/5 (15 theoretical plate column, 5:1 reflux ratio) or TBP (true boilingpoint).1.3 This test method can also be applied to any petroleum mixture except liquefied petroleum gases, very light napht
7、has, andfractions having initial boiling points above 400C.1.4 This test method contains the following annexes and appendixes:1.4.1 Annex A1Test Method for the Determination of the Efficiency of a Distillation Column,1.4.2 Annex A2Test Method for the Determination of the Dynamic Holdup of a Distilla
8、tion Column,1.4.3 Annex A3Test Method for the Determination of the Heat Loss in a Distillation Column (Static Conditions),1.4.4 Annex A4Test Method for the Verification of Temperature Sensor Location,1.4.5 Annex A5Test Method for Determination of the Temperature Response Time,1.4.6 Annex A6Practice
9、for the Calibration of Sensors,1.4.7 Annex A7Test Method for the Verification of Reflux Dividing Valves,1.4.8 Annex A8Practice for Conversion of Observed Vapor Temperature to Atmospheric Equivalent Temperature (AET),1.4.9 Appendix X1Test Method for Dehydration of a Sample of Wet Crude Oil, and1.4.10
10、 Appendix X2Practice for Performance Check.1.5 The values stated in SI units are to be regarded as the standard. The values given in parentheses are for information only.1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilit
11、yof the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatorylimitations prior to use. For specific warning statements, see Section 10.2. Referenced Documents2.1 ASTM Standards:2D941 Test Method for Density and Relative Density (Spec
12、ific Gravity) of Liquids by Lipkin Bicapillary Pycnometer3D1217 Test Method for Density and Relative Density (Specific Gravity) of Liquids by Bingham PycnometerD1298 Test Method for Density, Relative Density (Specific Gravity), orAPI Gravity of Crude Petroleum and Liquid PetroleumProducts by Hydrome
13、ter MethodD2887 Test Method for Boiling Range Distribution of Petroleum Fractions by Gas Chromatography1This test method is under the jurisdiction of ASTM Committee D02 on Petroleum Products and Lubricants and is the direct responsibility of Subcommittee D02.08 onVolatility.Current edition approved
14、JulyDec. 1, 2011. Published August 2011.January 2012. Originally approved in 1970. Last previous edition approved in 20102011 asD289210.D289211. DOI: 10.1520/D2892-11A.2For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual B
15、ook of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3Withdrawn. The last approved version of this historical standard is referenced on www.astm.org.1This document is not an ASTM standard and is intended only to provide the user of an ASTM standar
16、d an indication of what changes have been made to the previous version. Becauseit may not be technically possible to adequately depict all changes accurately, ASTM recommends that users consult prior editions as appropriate. In all cases only the current versionof the standard as published by ASTM i
17、s to be considered the official document.*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.D3710 Test Method for Boiling Range Distribution of Gasoline and Gasoline Fract
18、ions by Gas ChromatographyD4006 Test Method for Water in Crude Oil by DistillationD4052 Test Method for Density, Relative Density, and API Gravity of Liquids by Digital Density MeterD4057 Practice for Manual Sampling of Petroleum and Petroleum ProductsD4177 Practice for Automatic Sampling of Petrole
19、um and Petroleum ProductsD5134 Test Method for Detailed Analysis of Petroleum Naphthas through n-Nonane by Capillary Gas ChromatographyD6300 Practice for Determination of Precision and Bias Data for Use in Test Methods for Petroleum Products and LubricantsD6729 Test Method for Determination of Indiv
20、idual Components in Spark Ignition Engine Fuels by 100 Metre Capillary HighResolution Gas ChromatographyD6730 Test Method for Determination of Individual Components in Spark Ignition Engine Fuels by 100Metre Capillary (withPrecolumn) High-Resolution Gas ChromatographyD6733 Test Method for Determinat
21、ion of Individual Components in Spark Ignition Engine Fuels by 50-Metre Capillary HighResolution Gas Chromatography3. Terminology3.1 Definitions:3.1.1 adiabaticity, nthe condition in which there is no significant gain or loss of heat throughout the length of the column.3.1.1.1 DiscussionWhen distill
22、ing a mixture of compounds as is the case of crude petroleum, there will be a normal increasein reflux ratio down the column. In the case where heat losses occur in the column, the internal reflux is abnormally greater thanthe reflux in the head. The opposite is true when the column gains heat, as w
23、ith an overheated mantle.3.1.2 boilup rate, n in distillation, the quantity of vapor entering the column per unit of time.3.1.3 debutanization of crude petroleum, nthe removal of the light hydrocarbons up to and including n-butane, and retentionof the heavier hydrocarbons.3.1.3.1 DiscussionIn practi
24、ce, a crude petroleum is regarded as debutanized if the light hydrocarbon cut collected in the coldtrap contains more than 95 % of the C2to C4hydrocarbons and less than 5 % of the C5hydrocarbons initially present in the sample.3.1.4 distillation pressure, nthe pressure measured as close as possible
25、to the point where the vapor temperature is taken,normally at the top of the condenser.3.1.5 distillation temperature, nthe temperature of the saturated vapor measured in the head just above the fractionatingcolumn.3.1.5.1 DiscussionIt is also known as the head temperature or the vapor temperature.3
26、.1.6 dynamic hold-up, nin column distillation, the quantity of liquid held up in the column under normal operatingconditions.3.1.7 flood point, n in distillation, when the column is filled with liquid once the boilup rate obstructs the internal reflux. ,the point at which the velocity of the upflowi
27、ng vapors obstructs the down-coming reflux and the column suddenly fills with liquid.3.1.8 internal reflux, nin distillation, the liquid normally running down inside the column.3.1.9 pressure drop, nthe difference between the pressure measured in the condenser and the pressure measured in thedistill
28、ation flask.3.1.9.1 DiscussionIt is expressed in kilopascals (mm Hg) per metre of packed height for packed columns, or kilopascals (mmHg) overall for real plate columns. It is higher for aromatics than for paraffins, and for higher molecular weights than for lightermolecules, at a given boilup rate.
29、3.1.10 reflux ratio, R, nin distillation, the ratio of the condensate at the head of the column that is returned to the column (reflux) to that withdrawn as product.3.1.11 static hold-up or wettage, nthe quantity of liquid retained in the column after draining at the end of a distillation.3.1.11.1 D
30、iscussionIt is characteristic of the packing or the design of the plates, and depends on the composition of thematerial in the column at the final cut point and on the final temperature.3.1.12 takeoff rate, n in distillation, the volume of product withdrawn from the reflux divider over a specified p
31、eriod.3.1.13 theoretical plate, nthe section of a column required to achieve thermodynamic equilibrium between a liquid and itsvapor.3.1.13.1 DiscussionThe height equivalent to one theoretical plate (HETP) for packed columns is expressed in millimetres. Inthe case of real plate columns, the efficien
32、cy is expressed as the percentage of one theoretical plate that is achieved on one realplate.4. Summary of Test Method4.1 A weighed sample of 1 to 30 L of stabilized crude petroleum is distilled to a maximum temperature of 400C AET in afractionating column having an efficiency at total reflux of at
33、least 14, but not greater than 18, theoretical plates.4.2 A reflux ratio of 5:1 is maintained at all operating pressures, except that at the lowest operating pressures between 0.674and 0.27 kPa (5 and 2 mm Hg), a reflux ratio of 2:1 is optional. In cooperative testing or in cases of dispute, the sta
34、ges of lowpressure, the reflux ratios, and the temperatures of cut points must be mutually agreed upon by the interested parties prior tobeginning the distillation.D2892 11a24.3 Observations of temperature, pressure, and other variables are recorded at intervals and at the end of each cut or fractio
35、n.4.4 The mass and density of each cut or fraction are obtained. Distillation yields by mass are calculated from the mass of allfractions, including liquefied gas cut and the residue. Distillation yields by volume of all fractions and the residue at 15C arecalculated from mass and density.4.5 From t
36、hese 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 conducted on a crude oil to determine its value. It provides an estimate of theyields of fractions of various boiling ranges and is therefore valuable i
37、n technical discussions of a commercial nature.5.2 This test method corresponds to the standard laboratory distillation efficiency referred to as 15/5. The fractions producedcan be analyzed as produced or combined to produce samples for analytical studies, engineering, and product quality evaluation
38、s.The preparation and evaluation of such blends is not part of this test method.5.3 This test method can be used as an analytical tool for examination of other petroleum mixtures with the exception of LPG,very light naphthas, and mixtures with initial boiling points above 400C.6. Apparatus6.1 Distil
39、lation at Atmospheric PressureAll components must conform to the requirements specified as follows. Automaticdevices can be employed provided they meet the same requirements. A typical apparatus is illustrated in Fig. 1.6.1.1 Distillation FlaskThe distillation flask shall be of a size that is at lea
40、st 50 % larger than the volume of the charge. Thesize of the charge, between 1.0 and 30 L, is determined by the holdup characteristics of the fractionating column, as shown in Table1 and described in Annex A2. The distillation flask shall have at least one sidearm.6.1.1.1 The sidearm is used as a th
41、ermowell. It shall terminate about 5 mm from the bottom of the flask to ensure its immersionat the end of the distillation. When a second sidearm is present, it can be used for pressure drop detection with a nitrogen bleedor for mechanical stirring, or both.6.1.1.2 If a magnetic stirrer is used with
42、 a spherical flask, the flask shall have a slightly flattened or concave area at the bottomon which the magnetic stirrer can rotate without grinding the glass. In this case, termination of the thermowell shall be off center40 6 5 mm to avoid the magnetic stirring bar. Boiling chips can be used as an
43、 alternative to a stirrer.6.1.1.3 (WarningWhile the advantage of visibility in glass 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 recommended.)6.1.2 Heating SystemHeating
44、of the flask shall be provided in such a way that full boilup can be maintained at a steady rateat all pressure levels.An electric heating mantle covering the lower half of the flask and having one third of the heat in an elementlocated in the bottom central area and the remaining two thirds in the
45、rest of the hemisphere is recommended. While proportioningcontrollers are preferred, heat input can be manually adjusted by use of a variable auto transformer on each circuit, the smallerheater being automatically controlled by an instrument sensing the pressure drop of the column as registered in a
46、 differentialpressure instrument or alternatively by direct measurement of distillation rate.6.1.2.1 Minimum wattage required to provide full boilup of crude petroleum is approximately 0.125 W/mL of charge. Twicethis amount is recommended for quick heat-up.6.1.2.2 The heat density in the flask heate
47、rs is approximately equal to 0.5 to 0.6 W/cm2. This requires the use of nickelreinforced quartz fabric to ensure a reasonable service life.6.1.2.3 Immersion heaters can be employed in a similar way and have the advantage of faster response, but they are more fragileand require a specially designed f
48、lask to ensure that the heating elements remain immersed at the end of the run. When used, theirheat density should be approximately equal to 4 W/cm2.6.1.2.4 The upper half of the flask shall be covered with a mantle to avoid unnecessary heat losses from the upper surface andshall have an electric h
49、eater supplying about 0.25 W/cm2at full-rated voltage.6.1.3 Fractionating ColumnThe fractionating column must contain either particulate packing or real plates similar to thosewhose performance characteristics are summarized in Table 1 and meet the specifications stated in 6.1.3.1 through 6.1.3.4. Table2 lists current North American suppliers of suitable packings.6.1.3.1 The internal diameter shall be between 25 and 70 mm.6.1.3.2 The efficiency shall be between 14 and 18 theoretical plates at total reflux when measured by the procedure descri
