1、Designation: D2892 16D2892 17Standard 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 o
2、f 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) to a final cu
3、t temperatureof 400 C 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 acceptable appa
4、ratus 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 procedures for
5、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 % distilled can be
6、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 naphthas, andfrac
7、tions having initial boiling points above 400 C.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 Distillation Column
8、,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 for the Cal
9、ibration 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 Appendix X
10、2Practice for Performance Check.1.5 The values stated in SI units are to be regarded as the standard.1.5.1 ExceptionThe 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 responsibi
11、lityof 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 10.1.7 WARNINGMercury has been designated by many regulatory agencies as a hazardous material that
12、 can cause centralnervous system, kidney, and liver damage. Mercury, or its vapor, may be hazardous to health and corrosive to materials. Cautionshould be taken when handling mercury and mercury containing products. See the applicable product Material Safety Data Sheet(MSDS) for details and EPAs web
13、sitehttp:/www.epa.gov/mercury/faq.htmfor additional information. Users should be awarethat selling mercury and/or mercury containing products into your state or country may be prohibited by law.1.8 This international standard was developed in accordance with internationally recognized principles on
14、standardizationestablished in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued1 This test method is under the jurisdiction ofASTM Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of Subcommi
15、tteeD02.08 on Volatility.Current edition approved Dec. 1, 2016May 1, 2017. Published January 2017May 2017. Originally approved in 1970. Last previous edition approved in 20152016 asD2892 15.D2892 16. DOI: 10.1520/D2892-16.10.1520/D2892-17.This document is not an ASTM standard and is intended only to
16、 provide the user of an ASTM standard 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
17、 the standard as published by ASTM is to be considered the official document.*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 States1by the World Trade Organization Technical Ba
18、rriers to Trade (TBT) Committee.D2892 1722. Referenced Documents2.1 ASTM Standards:2D941 Test Method for Density and Relative Density (Specific Gravity) of Liquids by Lipkin Bicapillary Pycnometer3D1217 Test Method for Density and Relative Density (Specific Gravity) of Liquids by Bingham PycnometerD
19、1298 Test Method for Density, Relative Density, or API Gravity of Crude Petroleum and Liquid Petroleum Products byHydrometer MethodD2887 Test Method for Boiling Range Distribution of Petroleum Fractions by Gas ChromatographyD3710 Test Method for Boiling Range Distribution of Gasoline and Gasoline Fr
20、actions by Gas Chromatography (Withdrawn2014)4D4006 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
21、 Sampling of Petroleum 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 De
22、termination of Individual 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 M
23、ethod for Determination 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 Di
24、scussionWhen distilling a mixture of compounds as is the case of crude petroleum, there will be a normal increase in reflux ratio downthe column. In the case where heat losses occur in the column, the internal reflux is abnormally greater than the reflux in the head.The opposite is true when the col
25、umn gains heat, as with an overheated mantle.3.1.2 boilup rate, nin 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
26、DiscussionIn practice, a crude petroleum is regarded as debutanized if the light hydrocarbon cut collected in the cold trap contains more than95 % of the C2 to C4 hydrocarbons and less than 5 % of the C5 hydrocarbons initially present in the sample.3.1.4 distillation pressure, nthe pressure measured
27、 as close as possible 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 t
28、he vapor temperature.3.1.6 dynamic hold-up, nin column distillation, the quantity of liquid held up in the column under normal operatingconditions.3.1.7 flood point, nin distillation, the point at which the velocity of the upflowing vapors obstructs the down-coming refluxand the column suddenly fill
29、s with liquid.2 For referencedASTM standards, visit theASTM website, www.astm.org, or contactASTM Customer Service at serviceastm.org. For Annual Book of ASTM Standardsvolume information, refer to the standards Document Summary page on the ASTM website.3 Withdrawn. The last approved version of this
30、historical standard is referenced on www.astm.org.4 The last approved version of this historical standard is referenced on www.astm.org.D2892 1733.1.8 internal reflux, nin distillation, the liquid normally running down inside the column.3.1.9 pressure drop, nthe difference between the pressure measu
31、red 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 realplate columns. It is higher for aromatics than for paraffins, and for higher molecula
32、r weights than for lighter molecules, at a givenboilup rate.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 co
33、lumn after draining at the end of a distillation.3.1.11.1 DiscussionIt is characteristic of the packing or the design of the plates, and depends on the composition of the material in the column at thefinal cut point and on the final temperature.3.1.12 takeoff rate, n in distillation, the volume of p
34、roduct withdrawn from the reflux divider over a specified period.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
35、millimetres. In the case of real platecolumns, the efficiency is expressed as the percentage of one theoretical plate that is achieved on one real plate.4. Summary of Test Method4.1 A weighed sample of 1 L to 30 L of stabilized crude petroleum is distilled to a maximum temperature of 400 C AET in af
36、ractionating column having an efficiency at total reflux of at least 14, but not greater than 18, theoretical plates.4.2 Areflux ratio of 5:1 is maintained at all operating pressures, except that at the lowest operating pressures between 0.674 kPaand 0.27 kPa (5 mm and 2 mm Hg), a reflux ratio of 2:
37、1 is optional. In cooperative testing or in cases of dispute, the stages of lowpressure, the reflux ratios, and the temperatures of cut points must be mutually agreed upon by the interested parties prior tobeginning the distillation.4.3 Observations of temperature, pressure, and other variables are
38、recorded at intervals and at the end of each cut or fraction.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 re
39、sidue at 15 C arecalculated from mass and density.4.5 From these data the TBP curves in mass or volume percent, 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
40、of fractions of various boiling ranges and is therefore valuable in 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 f
41、or analytical studies, engineering, and product quality evaluations.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 mixt
42、ures with initial boiling points above 400 C.6. Apparatus6.1 Distillation 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 Distill
43、ation FlaskThe distillation flask shall be of a size that is at least 50 % larger than the volume of the charge. Thesize of the charge, between 1.0 L and 30 L, is determined by the holdup characteristics of the fractionating column, as shown inTable 1 and described in Annex A2. The distillation flas
44、k shall have at least one sidearm.D2892 1746.1.1.1 The sidearm is used as a thermowell. 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 bleed
45、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 the bottomon which the magnetic stirrer can rotate without grinding the glass. In this case, termination of the thermowell shall be off cente
46、r40 mm 6 5 mm to avoid the magnetic stirring bar. Boiling chips can be used as an 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 flask
47、s of a volume greater than 10 L are not recommended.)6.1.2 Heating SystemHeating 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
48、an elementlocated in the bottom central area and the remaining two thirds in the rest of the hemisphere is recommended. While proportioningFIG. 1 ApparatusD2892 175controllers are preferred, heat input can be manually adjusted by use of a variable auto transformer on each circuit, the smallerheater
49、being automatically controlled by an instrument sensing the pressure drop of the column as registered in a 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 WmL of charge. Twicethis amount is recommended for quick heat-up.6.1.2.2 The heat density in the flask heaters is approximately equal to 0.5 Wcm2 to 0.6 Wcm2. This requires the use of nickelreinforced nickel-reinforced quartz fabric
