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An American National Standard


Designation: D 2892 – 01

Standard Test Method for


Distillation of Crude Petroleum (15-Theoretical Plate
Column)1
This standard is issued under the fixed designation D 2892; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.

1. Scope 1.4.8 Annex A8—Practice for Conversion of Observed


1.1 This test method covers the procedure for the distillation Vapor Temperature to Atmospheric Equivalent Temperature
2
of stabilized crude petroleum to a final cut temperature of (AET),
400°C Atmospheric Equivalent Temperature (AET). This test 1.4.9 Appendix X1—Test Method for Dehydration of a
method employs a fractionating column having an efficiency of Sample of Wet Crude Oil, and
14 to 18 theoretical plates operated at a reflux ratio of 5:1. 1.4.10 Appendix X2—Practice for Performance Check.
Performance criteria for the necessary equipment is specified. 1.5 The values stated in SI units are to be regarded as
Some typical examples of acceptable apparatus are presented standard. The values given in parentheses are provided for
in schematic form. This test method offers a compromise information only.
between efficiency and time in order to facilitate the compari- 1.6 This standard does not purport to address all of the
son of distillation data between laboratories. safety concerns, if any, associated with its use. It is the
1.2 This test method details procedures for the production of responsibility of the user of this standard to establish appro-

iTeh Standards
a liquified gas, distillate fractions, and residuum of standard-
ized quality on which analytical data can be obtained, and the
priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. For specific

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determination of yields of the above fractions by both mass and precautionary notes, see Section 10.
volume. From the preceding information, a graph of tempera- 2. Referenced Documents
ture versus mass % distilled can be produced. This distillation
Document Preview
curve corresponds to a laboratory technique, which is defined
at 15/5 (15 theoretical plate column, 5:1 reflux ratio) or TBP
2.1 ASTM Standards:
D 941 Test Method for Density and Relative Density (Spe-
(true boiling point). cific Gravity) of Liquids by Lipkin Bicapillary Pycnom-
eter3
ASTM D2892-01
1.3 This test method can also be applied to any petroleum
D 1217 Test Method for Density and Relative Density
mixture except liquified petroleum gases, very light naphthas,
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and fractions having initial boiling points above 400°C. (Specific Gravity) of Liquids by Bingham Pycnometer4
1.4 This test method contains the following Annexes: D 1298 Test Method for Density, Relative Density (Specific
1.4.1 Annex A1—Test Method for the Determination of the Gravity), or API Gravity of Crude Petroleum and Liquid
Efficiency of a Distillation Column, Petroleum Products by Hydrometer Method4
1.4.2 Annex A2—Test Method for the Determination of the D 2427 Test Method for Determination of C2 through C5
Dynamic Holdup of a Distillation Column, Hydrocarbons in Gasolines by Gas Chromatography4
1.4.3 Annex A3—Test Method for the Determination of the D 2887 Test Method for Boiling Range Distribution of
Heat Loss in a Distillation Column (Static Conditions), Petroleum Fractions by Gas Chromatography5
1.4.4 Annex A4—Test Method for the Verification of Tem- D 3710 Test Method for Boiling Range Distributions of
perature Sensor Location, Gasoline and Gasoline Fractions by Gas Chromatography5
1.4.5 Annex A5—Test Method for Determination of the D 4006 Test Method for Water in Crude Oil by Distillation5
Temperature Response Time, D 4052 Test Method for Density and Relative Density of
1.4.6 Annex A6—Practice for the Calibration of Sensors, Liquids by Digital Density Meter5
1.4.7 Annex A7—Test Method for the Verification of Reflux D 4057 Practice for Manual Sampling of Petroleum and
Dividing Valves, Petroleum Products5
D 4177 Practice for Automatic Sampling of Petroleum and
Petroleum Products5
1
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.08 on Volatility.
3
Current edition approved Dec. 10, 2001. Published April 2002. Originally Discontinued; see 1993 Annual Book of ASTM Standards, Vol 05.01.
4
published as D 2892 – 70 T. Last previous edition D 2892 – 99a. Annual Book of ASTM Standards, Vol 05.01.
2 5
Defined as having a Reid vapor pressure less than 82.7 kPa (12 psi). Annual Book of ASTM Standards, Vol 05.02.

Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.

1
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.

D 2892
D 5134 Test Method for Detailed Analysis of Petroleum flooding. In routine adiabatic operation, the boilup rate can be
Naphthas through n-Nonane by Capillary Gas Chromatog- estimated roughly from the takeoff rate multiplied by the reflux
raphy6 ratio plus one.
3.1.3 debutanization of crude petroleum—the removal of
3. Terminology the light hydrocarbons up to and including n-butane, and
3.1 Definitions: retention of the heavier hydrocarbons.
3.1.1 adiabaticity—the condition in which there is no sig- 3.1.3.1 Discussion—In practice, a crude petroleum is re-
nificant gain or loss of heat throughout the length of the garded as debutanized if the light hydrocarbon cut collected in
column. the cold trap contains more than 95 % of the C2 to C4
3.1.1.1 Discussion—When distilling a mixture of com- hydrocarbons and less than 5 % of the C5 hydrocarbons
pounds as is the case of crude petroleum, there will be a normal initially present in the sample.
increase in reflux ratio down the column. In the case where 3.1.4 distillation pressure—the pressure measured as close
heat losses occur in the column, the internal reflux is abnor- as possible to the point where the vapor temperature is taken,
mally greater than the reflux in the head. The opposite is true normally at the top of the condenser.
when the column gains heat, as with an overheated mantle. 3.1.5 distillation temperature—the temperature of the satu-
3.1.2 boilup rate—the quantity of vapor entering the col- rated vapor measured in the head just above the fractionating
umn per unit of time. column.
3.1.2.1 Discussion—It is expressed in millilitres of liquid 3.1.5.1 Discussion—It is also known as the head tempera-
per hour for a given column or in millilitres per hour per square ture or the vapor temperature.
centimetre of cross-sectional area for comparative purposes. In 3.1.6 dynamic hold-up—the quantity of liquid held up in the
the latter case, it refers to the test mixture of n-heptane and column under normal operating conditions.
methylcyclohexane in the efficiency evaluation (see Annex A1) 3.1.6.1 Discussion—It is expressed as a percentage of the
and is measured at the bottom of the column. The maximum packed volume for packed columns so that the data can be
boilup of the n-heptane-methylcyclohexane test mixture is that compared. For real plate columns, it is expressed in millilitres

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which the column can handle under stable conditions without per plate. The data can only be compared with others of the
same diameter because of different tray spacing. Data for

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packed columns cannot be compared with those of real plate
6
Annual Book of ASTM Standards, Vol 05.03.
columns except in absolute units of milliliters per theoretical

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TABLE 1 Data for n-Heptane-Methylcyclohexane Test Mixture at 75 % of Maximum Boilup and 101.3 kPa (760 mm Hg)
PropakA,B,C,D,E HelipakF,G,H Perforated PlatesE,I,J Wire MeshE,K
Column diameter, mm 25 50 70 25 50 25 50 25 50
Packing size, mm 4 ASTM
66 D2892-01
No. 2917 No. 2918 NA NA NA NA L L L L

Boilup, mL/h 3 cm2 650 670


675 300 350 640 660 810 1050
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% of packed volume 17 15.3 17.0 15 14.3 NAL NAL 8.0 10.0
mL/theoretical plate 3.2 16 39 1.6 8.7 2.8 12.3 2.0 12.9
Pressure drop
kPa/m 1.2 1.05 0.94 1.53 1.41 NAL NAL 0.97 0.75
mm Hg/m 9.0 7.9 7.1 11.5 10.6 NAL NAL 7.3 5.6
kPa/theoretical plate 0.045 0.056 0.06 0.03 0.045 0.15 0.16 0.05 0.05
mm Hg/theoretical plate 0.34 0.42 0.43 0.24 0.34 1.1 1.2 0.35 0.37
HETP, mm (% of real plates) 38 53 61 21 32 (60 %) (65 %) 48 66
For 15-plate Towers
Packed height, cm (plates) 57 80 91 31.5 48 (25) (23) 72 99
Packed volume, mL 280 1570 3460 155 917 NAL NAL 353 1940
Dynamic holdup, mL 47 240 590 23 131 42 184 28 194
Pressure drop
kPa 0.68 0.84 0.86 0.48 0.68 2.2 2.4 0.70 0.73
mm Hg 5.1 6.3 6.5 3.6 5.1 16.5 18.0 5.3 5.5
Charge volume, L
Min (4 % Holdup) 1.2 6.0 15 0.575 3.3 1.0 4.6 0.7 4.9
Max (1 % Holdup) 4.8 24.0 60 2.3 13.0 4.2 10.4 2.8 19.4
A
Cooke, G. M. and Jameson, B. G. Analytical Chemistry, Vol 27, 1955, p. 1798.
B
Struck, R. T. and Kinner, C. R. Industrial and Engineering Chemistry, Vol 42, 1950, p. 77.
C
Cannon, M. R. Industrial and Engineering Chemistry, Vol 41, No. 9, 1949, p. 1953.
D
Bulletin 23, Scientific Development Co. P.O. Box 795, State College, PA 16801.
E
Cooke, G. M. Analytical Chemistry, Vol 39, 1967, p. 286.
F
Bulletin of Podbielniak Div. of Reliance Glass Works, P.O. Box 825, Bensenville, IL 60106.
G
Feldman, J., et al, Industrial and Engineering Chemistry, Vol 45, January 1953, p. 214.
H
Helipak Performance Characteristics, Begemean, C. R. and Turkal, P. J. (Laboratory Report of Podbielniak Inc.), 1950.
I
Umholtz, C. L. and Van Winkle, M. Petroleum Refiner, Vol 34, 1955, p. 114 for NH:MCH.
Pressure Drop Calculated from data obtained on o- and m-xylene binary.
J
Oldershaw, C. F. Industrial and Engineering Chemistry, Vol 13, 1941, p. 265.
K
Bragg, L. B. Industrial and Engineering Chemistry, Vol 49, 1957, p. 1062.
L
NA = not applicable.

2
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D 2892
plate (see Table 1). Dynamic hold-up increases with increasing pressures, except that at the lowest operating pressures be-
distillation rate up to the flood point and varies from one kind tween 0.674 and 0.27 kPa (5 and 2 mm Hg), a reflux ratio of
of fractionator to another. 2:1 is optional. In cooperative testing or in cases of dispute, the
3.1.7 flood point—the point at which the velocity of the stages of low pressure, the reflux ratios, and the temperatures
upflowing vapors obstructs the downcoming reflux and the of cut points must be mutually agreed upon by the interested
column suddenly loads with liquid. parties prior to beginning the distillation.
3.1.7.1 Discussion—Under these conditions no vapor can 4.3 Observations of temperature, pressure, and other vari-
reach the head and the heat to the distillation flask must be ables are recorded at intervals and at the end of each cut or
reduced to establish normal operations again. The flood point is fraction.
normally determined during the efficiency evaluation of a 4.4 The mass and density of each cut or fraction are
column using the n-heptane-methylcyclohexane test mixture obtained. Distillation yields by mass are calculated from the
(see Annex A1). mass of all fractions, including liquified gas cut and the
3.1.8 internal reflux—the liquid normally running down residue. Distillation yields by volume of all fractions and the
inside the column. residue at 15°C are calculated from mass and density.
3.1.8.1 Discussion—In the case of an adiabatic column 4.5 From these data the TBP curves in mass or volume %,
when distilling a pure compound, the internal reflux is constant or both, versus AET are drawn.
from top to bottom and is equal to the reflux at the reflux
divider. When distilling crude petroleum, the fractionation 5. Significance and Use
occurring in the dynamic holdup will cause a temperature 5.1 This test method is one of a number of tests conducted
gradient to be established with attendant greater amount of on a crude oil to determine its value. It provides an estimate of
internal reflux at the bottom of the column. the yields of fractions of various boiling ranges and is therefore
3.1.9 pressure drop—the difference between the pressure valuable in technical discussions of a commercial nature.
measured in the condenser and the pressure measured in the 5.2 This test method corresponds to the standard laboratory
distillation flask. distillation efficiency referred to as 15/5. The fractions pro-
iTeh Standards
3.1.9.1 Discussion—It is expressed in kilopascals (mm Hg)
per metre of packed height for packed columns, or kilopascals
duced can be analyzed as produced or combined to produce
samples for analytical studies, engineering, and product quality
(mm Hg) overall for real plate columns. It is higher for
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aromatics than for paraffins, and for higher molecular weights
than for lighter molecules, at a given boilup rate.
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
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3.1.10 reflux ratio, R—the ratio of reflux to distillate.
3.1.10.1 Discussion—The vapor reaching the top of the
examination of other petroleum mixtures with the exception of
LPG, very light naphthas, and mixtures with initial boiling
column is totally condensed and the resulting liquid is divided points above 400°C.
into two parts. One part L (reflux), is returned to the column
ASTM
and the other part, D (distillate), is withdrawn as product. The D2892-01
6. Apparatus
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reflux ratio ( R = L/D), can vary from zero at total takeoff
(L = 0) to infinity at total reflux (D = 0). 6.1 Distillation at Atmospheric Pressure—All components
3.1.11 static hold-up or wettage—the quantity of liquid must conform to the requirements specified as follows. Auto-
retained in the column after draining at the end of a distillation. matic devices can be employed provided they meet the same
3.1.11.1 Discussion—It is characteristic of the packing or requirements. A typical apparatus is illustrated in Fig. 1.
the design of the plates, and depends on the composition of the 6.1.1 Distillation Flask—The distillation flask shall be of a
material in the column at the final cut point and on the final size that is at least 50 % larger than the volume of the charge.
temperature. The size of the charge, between 1.0 and 30 L, is determined by
3.1.12 takeoff rate—the rate of product takeoff from the the holdup characteristics of the fractionating column, as
reflux divider expressed in millilitres per hour. shown in Table 1 and described in Annex A2. The distillation
3.1.13 theoretical plate—the section of a column required flask shall have at least one sidearm.
to achieve thermodynamic equilibrium between a liquid and its 6.1.1.1 The sidearm is used as a thermowell. It shall
vapor. terminate about 5 mm from the bottom of the flask to ensure its
3.1.13.1 Discussion—The height equivalent to one theoreti- immersion at the end of the distillation. When a second sidearm
cal plate (HETP) for packed columns is expressed in millime- is present, it can be used for pressure drop detection with a
tres. In the case of real plate columns, the efficiency is nitrogen bleed or for mechanical stirring, or both.
expressed as the percentage of one theoretical plate that is 6.1.1.2 If a magnetic stirrer is used with a spherical flask,
achieved on one real plate. the flask shall have a slightly flattened or concave area at the
bottom on which the magnetic stirrer can rotate without
4. Summary of Test Method grinding the glass. In this case, termination of the thermowell
4.1 A weighed sample of 1 to 30 L of stabilized crude shall be off center 40 6 5 mm to avoid the magnetic stirring
petroleum is distilled to a maximum temperature of 400°C bar. Boiling chips can be used as an alternative to a stirrer.
AET in a fractionating column having an efficiency at total 6.1.1.3 Warning—While the advantage of visibility in glass
reflux of at least 14, but not greater than 18, theoretical plates. distillation flasks is desirable, flasks of glass may become
4.2 A reflux ratio of 5:1 is maintained at all operating hazardous the larger the charge they contain. For this reason,

3
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D 2892

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ASTM D2892-01
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FIG. 1 Apparatus

glass flasks of a volume greater than 10 L are not recom- the column as registered in a differential pressure instrument or
mended. alternatively by direct measurement of distillation rate.
6.1.2 Heating System—Heating of the flask shall be pro- 6.1.2.1 Minimum wattage required to provide full boilup of
vided in such a way that full boilup can be maintained at a crude petroleum is approximately 0.125 W/mL of charge.
steady rate at all pressure levels. An electric heating mantle Twice this amount is recommended for quick heat-up.
covering the lower half of the flask and having one third of the 6.1.2.2 The heat density in the flask heaters is approxi-
heat in an element located in the bottom central area and the mately equal to 0.5 to 0.6 W/cm2. This requires the use of
remaining two thirds in the rest of the hemisphere is recom- nickel reinforced quartz fabric to ensure a reasonable service
mended. While proportioning controllers are preferred, heat life.
input can be manually adjusted by use of a variable auto 6.1.2.3 Immersion heaters can be employed in a similar way
transformer on each circuit, the smaller heater being automati- and have the advantage of faster response, but they are more
cally controlled by an instrument sensing the pressure drop of fragile and require a specially designed flask to ensure that the

4
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Contact ASTM International (www.astm.org) for the latest information.

D 2892
heating elements remain immersed at the end of the run. When takeoff line over a range of rates from 25 to 95 % of the
used, their heat density should be approximately equal to 4 maximum boilup rate of the column when determined in
W/cm2. accordance with Annex A7.
6.1.2.4 The upper half of the flask shall be covered with a 6.1.4 Condenser—The condenser shall have sufficient ca-
mantle to avoid unnecessary heat losses from the upper surface pacity to condense essentially all the C4 and C5 vapors from the
and shall have an electric heater supplying about 0.25 W/cm2 crude at the specified rate, using a coolant temperature
at full-rated voltage. of −20°C.
6.1.3 Fractionating Column—The fractionating column 6.1.5 Cold Traps—Two efficient traps of adequate capacity
must contain either particulate packing or real plates similar to cooled by dry ice and alcohol mixture shall be connected in
those whose performance characteristics are summarized in series to the vent line of the condenser when light hydrocar-
Table 1 and meet the specifications stated in 6.1.3.1 through bons are present, as at the beginning of the distillation. For
6.1.3.4. Table 2 lists current North American suppliers of vacuum distillation, a Dewar-style trap also cooled by dry ice
suitable packings. is used to protect the vacuum gage from vapors.
6.1.3.1 The internal diameter shall be between 25 and 70 6.1.6 Gas Collector—If uncondensed gas is to be measured,
mm. a gas meter can be connected to the outlet of the cold trap but
6.1.3.2 The efficiency shall be between 14 and 18 theoreti- with a calcium chloride drying tube between them to keep
cal plates at total reflux when measured by the procedure moisture from collecting in the traps. When analysis of the gas
described in Annex A1. sample is required, the gas can be collected in an empty plastic
6.1.3.3 The fractionating column shall be comprised of a balloon of suitable size either in place of the meter or following
integral glass column and reflux divider totally enclosed in a it. The volume of its contents can be determined by calculation
highly reflective vacuum jacket having a permanent vacuum of from the rise in pressure after expanding the sample into an
less than 0.1 mPa (;10−6 mm Hg). It shall be essentially evacuated vessel of known volume.
adiabatic when tested in accordance with Annex A3. 6.1.7 Fraction Collector—This part of the apparatus per-
6.1.3.4 The column shall be enclosed in a heat insulating mits the collection of the distillate without interruption during
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system, such as a glass-fabric mantle, capable of maintaining
the temperature of the outer wall of the glass vacuum jacket
withdrawal of product from the receiver under atmospheric or
reduced pressure. It also permits removal of product from the
equal to that of the internal vapor temperature. To verify this,
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the vacuum jacket shall have a temperature sensor, such as a
thermocouple, soldered to about 6 cm2 of thin copper or brass
vacuum system, without disturbing conditions in the column.
6.1.8 Product Receivers—The receivers shall be of suitable
size for the quantity of crude petroleum being distilled. The
just below the reflux divider. Document Preview
sheet and fastened to the outer wall of the glass jacket at a level recommended capacity is from 100 to 500 mL. They shall be
calibrated and graduated to permit reading to the nearest 1 %.
NOTE 1—For certain types of columns there is no significant difference 6.2 Distillation Under Reduced Pressure—In addition to the
in yields and fraction qualities between an uncompensated and aASTM heat- D2892-01
apparatus listed in 6.1, the apparatus for distillation under
compensated column. In such a case, by mutual agreement between reduced pressure shall include the following:
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parties concerned, the application of a heated insulating system can be
omitted. 6.2.1 Vacuum Pump—The vacuum system shall be capable
of maintaining smooth pressure operation at all pressure levels.
6.1.3.5 The adjustable reflux divider shall be located about It shall have the capacity to draw down the pressure in the
one column diameter above the top of the packing or topmost receiver(s) from atmospheric to 0.25 kPa (2 mm Hg) in less
plate. It must be capable of dividing the condensate with an than 30 s so as to avoid disturbance of the system during
accuracy of better than 90 % between the column and the emptying of receivers under vacuum. Alternatively, a separate
pump can be employed for this purpose.
TABLE 2 North American Sources of Commercially Available 6.2.2 Vacuum Gage—The point of connection of the
Packing Materials
vacuum gage to the system shall be as close as practical to the
Name Size Source
reflux dividing head. The connecting tubing shall be of
Propak 6 by 6 mm Scientific Development Co. sufficient diameter to ensure that no measurable pressure drop
P.O. Box 795
State College, PA 16801 occurs in the line. In no case shall the vacuum gage connection
Helipak 2.5 by 4 mm Reliance Glass Works Inc. be near the vacuum pump.
P.O. Box 825
Bensenville, IL 60106
6.2.2.1 All gages shall be carefully protected from conden-
Perforated plates 25 and 50 mm Reliance Glass Works Inc. sible vapors, especially water vapor, by a cold trap maintained
P.O. Box 825 at the temperature of dry ice.
Bensenville, IL 60106
W.A. Sales Inc. 6.2.3 Pressure Regulator—The regulator shall maintain the
419 Harvester Ct. pressure in the system essentially constant at all operating
Wheeling, IL 60090 pressures. Automatic regulation can be achieved by a device
Knitted wire mesh- Pegasus Industrial Specialties Ltd.
Goodloe multiknit P.O. Box 319 that regulates the demand on the vacuum source. A satisfactory
Agincourt, Ontario MIS 3B9 Canada device is a solenoid valve positioned between the vacuum
Packed Column Co. source and a surge tank of at least 10-L capacity. Alternatively,
970 New Durham Rd.
Edison, NJ 08817 a manual bleed valve can be maintained by a trained operator
with a minimum of attention.

5
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D 2892

FIG. 2 Approximate Pressure Drop-Fractionators Using Propak

6.3 Sensing and Recording Apparatus: manometer, however, will only be of satisfactory accuracy
6.3.1 Temperature Sensors—Only temperature measure- down to a pressure of about 1 kPa and then only when read
ment systems meeting the requirements of 6.3.1.1 and 6.3.1.2 with a good cathetometer (an instrument based on a telescope
shall be used. mounted on a vernier scale to determine levels very accu-
6.3.1.1 The vapor temperature sensor can be a platinum rately). Alternatively, a tensimeter or certified electronic sen-

iTeh Standards
resistance thermometer, a Type J thermocouple with the sors may be used, provided the calibration of the sensor and its
junction head fused to the lower tip of the thermowell, or any associated recording instrument can be traced back to a
other device that meets the requirements in this paragraph and primary pressure standard. Sensors of the diaphragm type have
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6.3.1.2. The tip of the sensor shall be located above the top of
the packing or the topmost glass plate and in close proximity to
been found satisfactory. Vacuum gages based on hot wires,
radiation, or electrical conductivity detectors are not recom-

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the reflux divider but not in contact with the liquid reflux. The
location of the vapor temperature sensor shall be proved by the
mended.
6.3.2.1 The gage for measuring subatmospheric pressures
test method described in Annex A4. The sensor shall have a shall have an accuracy at least equal to that stated as follows:
cooling time of not more than 175 s, as described in Annex A5. Distillation Pressure Accuracy
6.3.1.2 The vapor temperature measuring device shall have ASTM D2892-01kpa mm Hg kPa mm Hg
an accuracy https://standards.iteh.ai/catalog/standards/sist/fb3f034b-9666-4d47-8f8c-a847014e5fdf/astm-d2892-01
of 0.5°C or better and be measured with a 100-13.3
13.3-1.33
760 to 100
99 to 10
0.13
0.013
1.0
0.1
resolution of 0.1°C or better. The liquid temperature measuring 1.33-0.266 9 to 2 0.006 0.06
device shall have an accuracy of 1.0°C or better and be
measured with a resolution of 0.5°C or better. Temperatures are 6.3.2.2 Noncertified gages shall be calibrated from a non-
recorded either manually or automatically. tilting McLeod gage or a secondary electronic standard trace-
6.3.1.3 Temperature sensors shall be calibrated as described able to a primary standard. A basic calibration procedure is
in Annex A6. Alternatively certified sensors may be used, described in Annex A6. Recalibrate when either the sensor or
provided the calibration of the sensor and its associated the instrument is repaired or serviced. Verification of the
recording instrument can be traced back to a primary tempera- calibration of the electronic pressure sensors is to be made on
ture standard. Temperature sensors are calibrated over the full a regular basis. A frequency of at least once a month is
range of temperature (from 0 to 400°C) at the time of first use recommended. Verification of the calibration of the sensors can
of the sensor in combination with its associated instrument. be accomplished using the procedures described in Annex A6
Recalibrate when either the sensor or the instrument is repaired or against a certified reference system.
or serviced. Verification of the calibration of the temperature 6.3.3 Boilup Rate—The boilup rate is normally controlled
sensors is to be made on a regular basis. For vapor temperature by sensing the pressure drop in the column. The pressure drop
sensors, verification at least once a month is recommended and during operation is measured by means of a manometer or
for liquid temperature sensors once every six months. Verifi- pressure transducer connected between the flask and the
cation of the calibration of the sensors can be accomplished condenser. Prevention of condensation in the connecting tube
potentiometrically by the use of standard precision resistance can be accomplished by injecting a very small flow of nitrogen
or by distilling a pure compound with accurately known (8 cm3/s) between the pressure drop sensor manometer and the
boiling point. flask (see Fig. 1) or by placing a small water-cooled condensor
6.3.2 Vacuum Gage—A nontilting McLeod gage or a mer- between the flask and the pressure drop sensor. Alternatively,
cury manometer are primary standards and can be used without the boilup rate can be controlled from the measurement of take
calibration when properly used and maintained. A mercury off rate.

6
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.

D 2892
7. Verification of Apparatus Performance actual operating conditions. Appendix X2, in principle, mea-
7.1 Test Method D 2892 provides a standard framework for sures the combined effect of all factors affecting the results of
the laboratory distillation of crude oils in order to produce cuts Test Method D 2892.
of defined quality (for further testing) and the concurrent 7.6.1 The minimum tray number as defined in Appendix X2
production of a boiling point curve. As the quantity require- is a measure of overall cut quality, and the difference between
ments and cut points might be widely different between nominal cut point (AET) and effective cut point (ECP as
companies and application areas, this test method does not defined in Appendix X2) provides a measure for the correct-
standardize on equipment design but on equipment perfor- ness of the AET. However, insufficient data are available right
mance. now to define the allowable tolerances in a rigid statistical way.
7.2 The nature of the test method (the use of large sample Moreover, the test method described is very labor intensive and
quantities and very time consuming) and the nature of the precludes its use on a regular, short time interval basis and,
product being tested (highly volatile and unstable material), therefore, its use as a mandatory statistical control technique.
precludes the use of standard statistical control techniques. 7.6.2 Appendix X2, therefore, provides only recommended
Moreover, this test method does not produce a single result, nor guidelines for statistical control on column performance, in-
is the series of results (the boiling point curve) derived under cluding both correctness of AET and column efficiency. It is the
rigidly defined conditions (see 4.2). responsibility of the laboratory to provide for sufficient quality
7.3 Equipment performance in the context of Test Method controls to guarantee conformance to the test method.
D 2892 consists of two elements; the efficiency of the column, 8. Sampling
defining cut quality, and the correctness of the cut point (AET), 8.1 Obtain a sample for distillation in accordance with
defining the boiling point curve. instructions given in Practice D 4057 or D 4177. The sample
7.4 The correctness of the AET is mainly, but not only, must be received in a sealed container and show no evidence of
dependent on the accuracy of the (vapor) temperature and leakage.
(operating) pressure sensors (Annex A6). Other factors affect- 8.2 Cool the sample to between 0 and 5°C by placing it in
ing the accuracy and precision of the boiling point curve are:
iTeh Standards
a refrigerator for several hours (preferably overnight) before
7.4.1 The location of the temperature and pressure sensor opening.
(Annex A4). 8.3 If the sample appears waxy or too viscous, raise the
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7.4.2 The dynamic response of the sensors (Annex A5).
7.4.3 The correct operation of the reflux divider (Annex
temperature to 5°C above its pour point.
8.4 Agitate the sample by whatever means are appropriate

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A7). to its size to ensure that it is well-mixed.
7.4.4 The heat loss from the column (Annex A3). 8.5 Determine the water content of the sample by Test
7.4.5 The efficiency of the column (Annex A1). Method D 4006 or any other suitable method. If the water
7.4.6 These factors are basically covered through the appro- content exceeds 0.3 % volume, the sample shall be dehydrated
priate annexes. However, it should be realized that this ASTMtakes D2892-01
prior to fractional distillation. A suitable practice for dehydra-
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of individual components and does not cover the tion of wet crude oil samples is described in Appendix X1.
combined effect of small deviations. Moreover, the aforemen-
NOTE 2—Attempts to distill wet crude oil samples in glass columns
tioned tests are all done under more or less static conditions, might result in breakage of the glassware, which poses a potential fire
not necessarily representative for the behavior of the system hazard. Moreover, the presence of water will effect the accuracy of
under actual dynamic conditions. distillation yield in the naphtha region. These effects are more pronounced
7.5 Cut quality is mainly defined by the efficiency of the for heavy crude oils, containing low amounts of hydrocarbons boiling
column (Annex A1), but is also affected by: below 100°C, than for light crudes where there is usually sufficient
7.5.1 The correct operation of the reflux divider (reflux hydrocarbon vapor generated to form an azeotrope and drive the water
vapors through the column without problems.
ratio) (Annex A7).
7.5.2 The heat loss from the column, that is, internal reflux 9. Preparation of Apparatus
(Annex A3).
9.1 Clean and dry the distillation column and all the
7.5.3 The dynamic hold up of the column (Annex A2). ancillary glass apparatus before the distillation begins.
7.5.4 Column efficiency is covered in this test method 9.2 Ensure that the system is leak-free and all heaters,
through Table 1 and Annex A1. However, Table 1 only control devices, and instruments are on and in working order.
provides an assumption on efficiency and is not a guarantee. A clock or other timing device should be ready for use.
Annex A1 only provides a check under static conditions,
infinite reflux ratio, rather low actual temperatures and a binary 10. Procedure
component system. Hence, although there is some safeguard on 10.1 Charging:
standard performance, through conformance to Annex A1, 10.1.1 The charge size shall be such that the dynamic hold
Annex A2, Annex A3, and Annex A7, again it remains up as determined in accordance with Annex A2 is between 1
questionable whether this is truly representative for columns and 4 % of the charge when operating at 75 % of maximum
under actual operating conditions. boilup (see Table 1). Chill the flask to a temperature not lower
7.6 Theoretically, an overall performance check, like the then 0°C.
one described in Appendix X2, is capable of verifying the 10.1.2 Insert the stirring device or place some pieces of
performance of a column and the correctness of the AET under glass or porcelain into the flask to control bumping.

7
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.

D 2892
10.1.3 Determine the density of the sample by Test Method 10.3.2 Regulate the heat input as necessary to establish and
D 941, D 1217, or D 1298. maintain a boilup rate approximately 75 % of maximum. Fig.
10.1.4 Calculate to within 65 % the mass of crude petro- 3 can be used as a guide for Propak. Rates for other sizes can
leum corresponding to the desired volume of the charge. Weigh be estimated by multiplying the boilup rate in Table 1 by the
to the nearest 1 % this quantity of sample into the flask. cross-sectional area of the column and dividing by the sum of
10.1.5 Attach the flask to the column and connect the the reflux ratio + 1.
pressure drop measuring device. Install the heating system, 10.3.3 Commence takeoff at a reflux ratio of 5:1 and total
stirrer, and support device. (Warning—Poisonous H2S gas is cycle time of not over 30 s nor less than 18 s.
frequently evolved from crude oil and precautions must be 10.3.4 Take off distillate in separate and consecutive frac-
taken either to absorb the gas that passes through the cold trap tions of suitable size. The recommended size of fraction is that
or to vent it to a safe place.) corresponding to 5 or 10°C in vapor temperature. Collect
10.2 Debutanization: fractions boiling below 65°C in receivers cooled to 0°C or
10.2.1 For necessary apparatus refer to 6.1.5 and 6.1.6. below. When the vapor temperature reaches 65°C, refrigerant
10.2.2 Begin circulation of refrigerant at a temperature no in the condenser and related coolers can be discontinued and
higher than −20°C in the condenser, distillate cooler, and water at ambient temperature substituted.
receiver, if so equipped. 10.3.5 At the end of each fraction and at each cut point,
10.2.3 Record the barometric pressure at the beginning and record the following observations:
periodically throughout the distillation. 10.3.5.1 Time in hours and minutes,
10.2.4 Apply heat to the flask at such a rate that vapors 10.3.5.2 Volume in millilitres,
reach the top of the column between 20 and 50 min after 10.3.5.3 Vapor temperature in °C to the nearest 0.5°C,
startup. Adjust heat input so as to achieve a pressure drop of 10.3.5.4 Temperature of the boiling liquid in °C to the
less than 0.13 kPa/m (1.0 mm Hg/m) in packed columns or less nearest 1°C,
than 0.065 kPa (0.5 mm Hg) in real plate columns. Program 10.3.5.5 Atmospheric pressure in kPa (mm Hg), and
automated equipment in accordance with the preceding direc- 10.3.5.6 Pressure drop in the column in kPa (mm Hg).
tions. Turn on the stirring device if used.
iTeh Standards
10.2.5 Allow the column to operate at total reflux until the
10.3.6 If signs of flooding are observed, reduce the heating
rate while continuing takeoff until steady conditions are
restored. If a cut point is encountered during this period, stop
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vapor temperature reaches equilibrium but not longer than 15
min after the first drop of condensate appears in the reflux the distillation,
condition cuts.
cool the charge, and recombine the off-
Restart the distillation with a period at total
divider.
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10.2.6 Record the vapor temperature as the initial vapor
temperature.
reflux, not to exceed 15 min, to restore operating conditions
before continuing takeoff. Do not make a cut within 5°C of
startup.
10.2.7 Stop the circulation of the refrigerant and observe the
10.3.7 Continue taking cuts until the desired maximum
vapor temperature. When the vapor temperature reaches 15°C, ASTMvapor
D2892-01
temperature is reached or until the charge shows signs of
start the circulation of refrigerant again.
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cracking. Pronounced cracking is evidenced by a fog appearing
10.2.8 If the vapor temperature drops below 15°C, continue
refluxing for at least 15 min. Repeat 10.2.7. If the vapor
temperature remains at 15°C or rises, continue with the
atmospheric distillation. (Warning—The following three steps
should not be done until after the first naphtha cut has been
removed to ensure that all the light gases have been recovered.)
10.2.9 Remove and weigh the dry ice traps containing light
hydrocarbon liquid after carefully wiping them dry.
10.2.10 Sample the contents of the first dry ice trap using a
10 to 50 mL pressure vessel evacuated to no lower than 26.6
kPa (200 mm Hg). Keep all containers at the temperature of
dry ice to ensure no loss of volatiles. The first trap next to the
condenser should contain all of the sample. If condensate is
found in the second trap, sample both traps or combine the
contents before sampling.
10.2.11 Submit the trap sample and gas balloon, if used, for
analysis by Test Method D 2427 to be reported on a fixed-gas
free basis.
10.3 Distillation at Atmospheric Pressure:
10.3.1 Maintain a temperature below −20°C in the lines of
the distillate cooler and receiver as well as in the condenser.
Turn on the column mantle heat controller and maintain the
column jacket temperature 0 to 5°C below the vapor tempera- FIG. 3 Expected Takeoff Rates at 5:1 Reflux Ratio for
ture. Fractionators Using Propak

8
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.

D 2892
in the flask and later at the reflux divider. Do not allow the 10.4.4 Apply heat to the boiler and reestablish reflux at any
vapor temperature to exceed 210°C nor the temperature of the moderate rate in the reflux divider for about 15 min to reheat
boiling liquid to exceed 310°C. the column to operating temperature. Momentarily stop heat
10.3.8 Shut off the reflux valve and the heating system. input and raise the pressure with N2 for 1 min to drop the
Allow the contents to cool to such a temperature that the holdup into the distillation flask.
distillation can be commenced at 13.3 kPa (100 mm Hg) 10.4.5 Reapply heat to the distillation flask and adjust the
without flooding. This temperature can be estimated by adding rate of heating to maintain a constant pressure drop equivalent
the DT between the liquid and vapor temperatures found for the to the boilup rate of approximately 75 % of the maximum rate
column during atmospheric operation to the expected initial for this pressure and begin takeoff without delay. The approxi-
vapor temperature at the reduced pressure, or by subtracting mate pressure drops required for this purpose are indicated in
the DT from the last recorded liquid temperature. Fig. 3. Maintain a column insulation temperature 0 to 5°C
NOTE 3—Cooling of the liquid in the flask can be accelerated by
below the vapor temperature throughout the operation.
blowing a gentle stream of compressed air onto the flask after its heating 10.4.6 Remove separately, cuts of suitable size as in 10.3.4.
mantle has been removed. Avoid strong jets of cold air. Alternately, turn 10.4.7 At the end of each distillate fraction and at each cut
on coolant in the quench coil of the flask, if used. point, record the following observations:
10.3.9 Weigh all fractions and determine their densities. 10.4.7.1 Time in hours and minutes,
10.3.10 Submit the first distillate fraction for analysis by gas 10.4.7.2 Volume in millilitres observed at ambient tempera-
chromatography. ture,
10.4 Distillation at 13.3 kPa (100 mm Hg): 10.4.7.3 Vapor temperature in °C to the nearest 0.5°C with
10.4.1 If further cuts at higher temperatures are required, correction, if any,
distillation can be continued at reduced pressures, subject to 10.4.7.4 Temperature of the boiling liquid in °C to the
the maximum temperature that the boiling liquid will stand nearest 1°C,
without significant cracking. This is about 310°C in most cases. 10.4.7.5 Pressure drop in the column in kPa (mm Hg),
Notable exceptions are crude oils containing heat-sensitive 10.4.7.6 Operating pressure measured at the top of the
iTeh Standards
sulfur compounds. In any case, do not make a cut within 5°C
of the temperature at startup because the column will not be at
column in kPa (mm Hg) absolute with correction, if any, and
10.4.7.7 AET using the equations given in Annex A8. Table
equilibrium.
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10.4.2 Connect a vacuum pumping and control system to
the apparatus as shown in Fig. 1.
3 is provided only as a guide in estimating the cutpoints during
distillation.
10.4.8 Continue taking cuts until the desired maximum
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10.4.3 Start the vacuum pump and adjust the pressure
downward gradually to the value of 13.3 kPa (100 mm Hg) or
point is reached or until the charge shows signs of cracking.
Pronounced cracking is evidenced by the evolution of gases as
set the pressure regulator at this value. The temperature of the indicated by rising pressure as well as a fog appearing in the
liquid in the flask must be below that at which it will boil ASTM D2892-01
at flask (see Note 3). Do not allow the temperature of the boiling
13.3 kPa (100 mm Hg). If the liquid boils before this pressure liquid to exceed 310°C. (Warning—Automatic vacuum con-
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is reached, increase the pressure and cool further until the trollers could mask a slight rise in pressure due to cracking.
desired pressure can be achieved without boiling. Vigilance is required to avoid this.)

TABLE 3 Conversion of Temperatures to Atmospheric Equivalent from Measurements at 13.3 kPa (100 mm Hg)

NOTE 1—Numbers calculated by Eq A8.1 and Eq A8.3, using 100.0 mm Hg as pressure input.
Temperature,
0 1 2 3 4 5 6 7 8 9
°C
50 107.9 109.0 110.1 111.3 112.4 113.6 114.7 115.8 116.9 118.1
60 119.2 120.3 121.5 122.6 123.7 124.9 126.0 127.1 128.3 129.4
70 130.5 131.6 132.8 133.9 135.0 136.2 137.3 138.4 139.5 140.7
80 141.8 142.9 144.0 145.2 146.3 147.4 148.5 149.7 150.8 151.9
90 153.0 154.2 155.3 156.4 157.5 158.7 159.8 160.9 162.0 163.2
100 164.3 165.4 166.5 167.6 168.8 169.9 171.0 172.1 173.2 174.4
110 175.5 176.6 177.7 178.8 179.9 181.1 182.2 183.3 184.4 185.5
120 186.6 187.8 188.9 190.0 191.1 192.2 193.3 194.5 195.6 196.7
130 197.8 198.9 200.0 201.1 202.2 203.4 204.5 205.6 206.7 207.8
140 208.9 210.0 211.1 212.2 213.4 214.5 215.6 216.7 217.8 218.9
150 220.0 221.1 222.2 223.3 224.4 225.5 226.7 227.8 228.9 230.0
160 231.1 232.2 233.3 234.4 235.5 236.6 237.7 238.8 239.9 241.0
170 242.1 243.2 244.3 245.4 246.5 247.6 248.7 249.8 250.9 252.0
180 253.1 254.2 255.3 256.4 257.5 258.6 259.7 260.8 261.9 263.0
190 264.1 265.2 266.3 267.4 268.5 269.6 270.7 271.8 272.9 274.0
200 275.1 276.2 277.3 278.4 279.5 280.6 281.7 282.8 283.9 285.0
210 286.0 287.1 288.2 289.3 290.4 291.5 292.6 293.7 294.8 295.9
220 297.0 298.1 299.1 300.2 301.3 302.4 303.5 304.6 305.7 306.8
230 307.9 308.9 310.0 311.1 312.2 313.3 314.4 315.5 316.6 317.6
240 318.7 319.8 320.9 322.0 323.1 324.2 325.2 326.3 327.4 328.5
250 329.6 330.7 331.7 332.8 333.9 335.0 336.1 337.1 338.2 339.3

9
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.

D 2892
10.4.9 Shut off the reflux valve and the heating system. coolant in the condenser to warm as in 10.5.3.
Allow the contents to cool to such a temperature that the 10.5.6 When the final cut point has been reached, or when
distillation can be commenced at a lower pressure without limits of boiling liquid temperature and column pressure
boiling. This temperature can be estimated by adding the DT prevent further distillation, turn off the reflux valve and heating
between the liquid and vapor temperatures found for the system and allow to cool with the vacuum still applied.
column during operation to the expected initial vapor tempera-
10.5.7 When the temperature of the residue in the flask has
ture at the lower pressure, or by subtracting the DT from the
last recorded liquid temperature. fallen below 230°C, shut off the vacuum pump. Vent the
10.4.10 Weigh all fractions and determine their densities at fractionating unit with nitrogen or other inert gas. Do not use
15°C. air. (Warning—Air is suspected of initiating explosions in
10.5 Distillation at Lower Pressures: fractionating units that are vented while too hot, such as at the
10.5.1 If the final cut point has not been reached, distillation end of a run.)
can be continued at a lower pressure subject to the same 10.5.8 Stop circulation of coolant in the condenser and
limitation as before (see 10.4.1). Only one pressure level ancillary equipment. Disconnect the flask. Recover the static
between 13.3 kPa (100 mm Hg) and 0.266 kPa (2 mm Hg) is holdup of the column (wettage) by distilling a small quantity of
permitted. Where the maximum cut point is 400°C AET, the solvent such as toluene in a separate flask to wash the column,
minimum pressure is recommended. condenser, and takeoff system. Evaporate the solvent from the
10.5.2 Adjust the pressure to the desired level. If the liquid collected residue at 10°C above the boiling point of the solvent,
boils before the pressure is reached, increase the pressure and using a small purge of nitrogen. For distillations not involving
cool further until the desired pressure can be achieved without disagreement, or by mutual consent, the holdup can be esti-
boiling. Follow the procedure in 10.4.4. mated using a graph similar to Fig. 4. The density of the holdup
10.5.3 Circulate cooling water in the condenser and liquid is estimated by extrapolation of the density line for the
cooler either at ambient temperature or warmed to a tempera- preceding cuts. The static holdup can be treated as a separate
ture that will ensure that wax does not crystallize in the
small cut or blended into the bottoms before inspections are
iTeh Standards
condenser or takeoff lines. Alternatively, leave the cooling coils
full of water but vented and not circulating, or else circulate a
made. The latter must be done if other analyses besides density
are to be performed on the residue.
stream of air instead of water as a coolant.
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10.5.4 Continue vacuum operation as in 10.4.5 through
10.4.8. During this operation, a reflux ratio of 2:1 is allowed if
10.5.9 Weigh all fractions and the residue in the flask and
determine their densities at 15°C by Test Method D 4052 or by

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mutually agreed upon in advance and noted in the report.
Correct observed and corrected vapor temperatures to AET
another
necessary.
suitable method. Convert the density to 15°C, if

using the equations given in Annex A8. Table 4 and Table 5 are
NOTE 4—Heavier flasks, such as those for 50 and 70-mm diameter
provided only as a guide in estimating the cutpoints during
distillation. ASTM D2892-01
columns, are not normally removed for weighing. In these cases the
residue can be discharged at a temperature not over 200°C into a tared
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10.5.5 Check periodically that the condensate drips nor- container for weighing. Nitrogen pressure of approximately 6.7 kPa (50
mally in the condenser and that the distillate flows smoothly mm Hg) will be sufficient for this. Wettage in these cases will include that
into the takeoff line. If crystallization is observed, allow the of the column and the flask together.

TABLE 4 Conversion of Temperatures to Atmospheric Equivalent from Measurements at 1.33 kPa (10 mm Hg)

NOTE 1—Numbers calculated by Eq A8.1 and Eq A8.3, using 10.00 mm Hg as pressure input.
Temperature,
0 1 2 3 4 5 6 7 8 9
°C
50 165.1 166.3 167.6 168.8 170.1 171.3 172.6 173.8 175.1 176.3
60 177.6 178.8 180.1 181.3 182.6 183.8 185.1 186.3 187.6 188.8
70 190.1 191.3 192.6 193.8 195.1 196.3 197.5 198.8 200.0 201.3
80 202.5 203.7 205.0 206.2 207.5 208.7 209.9 211.2 212.4 213.6
90 214.9 216.1 217.3 218.6 219.8 221.0 222.3 223.5 224.7 226.0
100 227.2 228.4 229.6 230.9 232.1 233.3 234.6 235.8 237.0 238.2
110 239.5 240.7 241.9 243.1 244.3 245.6 246.8 248.0 249.2 250.4
120 251.7 252.9 254.1 255.3 256.5 257.7 259.0 260.2 261.4 262.6
130 263.8 265.0 266.2 267.4 268.7 269.9 271.1 272.3 273.5 274.7
140 275.9 277.1 278.3 279.5 280.7 281.9 283.1 284.3 285.5 286.7
150 287.9 289.1 290.3 291.6 292.7 293.9 295.1 296.3 297.5 298.7
160 299.9 301.1 302.3 303.5 304.7 305.9 307.1 308.3 309.5 310.7
170 311.9 313.1 314.3 315.4 316.6 317.8 319.0 320.2 321.4 322.6
180 323.8 324.9 326.1 327.3 328.5 329.7 330.9 332.0 333.2 334.4
190 335.6 336.8 338.0 339.1 340.3 341.5 342.7 343.8 345.0 346.2
200 347.4 348.5 349.7 350.9 352.1 353.2 354.4 355.6 346.8 357.9
210 359.1 360.3 361.4 362.6 363.8 364.9 366.1 367.3 368.4 369.6
220 370.8 371.9 373.1 374.3 375.4 376.6 377.8 378.9 380.1 381.2
230 382.4 383.6 384.7 385.9 387.0 388.2 389.4 390.5 391.7 392.8
240 394.0 395.1 396.3 397.4 398.6 399.8 400.9 402.1 403.2 404.4
250 405.5 406.7 407.8 409.0 410.1 411.3 412.4 413.5 414.7 415.8

10
NOTICE: This standard has either been superceded and replaced by a new version or discontinued.
Contact ASTM International (www.astm.org) for the latest information.

D 2892
TABLE 5 Conversion of Temperatures to Atmospheric Equivalent from Measurements at 0.266 kPa (2 mm Hg)

NOTE 1—Numbers calculated by Eq A8.1 and Eq A8.3, using 2.00 mm Hg as pressure input.
Temperature,
0 1 2 3 4 5 6 7 8 9
°C
50 200.3 201.6 203.0 204.3 205.6 206.9 208.3 209.6 210.9 212.2
60 213.5 214.9 216.2 217.5 218.8 220.1 221.4 222.8 224.1 225.4
70 226.7 228.0 229.3 230.6 231.9 233.2 234.5 235.8 237.1 238.5
80 239.8 241.1 242.4 243.7 245.0 246.3 247.6 248.9 250.2 251.5
90 252.7 254.0 255.3 256.6 257.9 259.2 260.5 261.8 263.1 264.4
100 265.7 267.0 268.2 269.5 270.8 272.1 273.4 274.7 275.9 277.2
110 278.5 279.8 281.1 282.3 283.6 284.9 286.2 287.4 288.7 290.0
120 291.3 292.5 293.8 295.1 296.4 297.6 298.9 300.2 301.4 302.7
130 304.0 305.2 306.5 307.8 309.0 310.3 311.5 312.8 314.1 315.3
140 316.6 317.8 319.1 320.4 321.6 322.9 324.1 325.4 326.6 327.9
150 329.1 303.4 331.6 332.9 334.1 335.4 336.6 337.9 339.1 340.4
160 341.6 342.9 344.1 345.3 346.6 347.8 349.1 350.3 351.5 352.8
170 354.0 355.3 356.5 357.7 359.0 360.2 361.4 362.7 363.9 365.1
180 366.4 367.6 368.8 370.0 371.3 372.5 373.7 374.9 376.2 377.4
190 378.6 379.8 381.1 382.3 383.5 384.7 385.9 387.2 388.4 389.6
200 390.8 392.0 393.2 394.5 395.7 396.9 398.1 399.3 400.5 401.7
210 402.9 404.2 405.4 406.6 407.8 409.0 410.2 411.4 412.6 413.8
220 415.0 416.2 417.4 418.6 419.8 421.0 422.2 423.4 424.6 425.8
230 427.0 428.2 429.4 430.6 431.8 433.0 434.2 435.4 436.5 437.7
240 438.9 440.1 441.3 442.5 443.7 444.9 446.1 447.2 448.4 449.6
250 450.8 452.0 453.2 454.3 455.5 456.7 457.9 459.1 460.2 461.4

11. Calculation v 5 m/d (4)


11.1 Calculate the mass % of each distillate fraction and the where:

iTeh Standards
residue to the 0.1 mass %, using Eq 1. d = density of the fraction or residue at 15°C, g/mL,
mass % 5 100~m/M! (1) m = mass of fraction or residue corrected for loss, g, and
v = volume of fraction, mL.
where:
m = mass of fraction or residue, (https://standards.iteh.ai)
g, and
11.5 Calculate the volume % of each distillate fraction to the
nearest 0.1 volume %, using Eq 5.
M = mass of dry crude oil charged, g.
Document
11.1.1 The first fraction is the gas fraction collected in the
balloon. If this fraction is less than 0.1 mass %, it can be
Preview vol % 5 100~v/V!
11.6 Calculate the volume % gain or loss to the nearest 0.1
(5)

ignored. volume %, using Eq 6.


ASTM
11.1.2 The second fraction (or first, if no gas is collected) is D2892-01 Loss 5 100 2 ~ (100~v/V!! (6)
the condensate in the dry ice trap. With density at 15°C
https://standards.iteh.ai/catalog/standards/sist/fb3f034b-9666-4d47-8f8c-a847014e5fdf/astm-d2892-01
Usually, the above expression is negative due to volume
calculated from the gas chromatographic data on a fixed gas
expansion. Normalize any apparent expansion or contraction
free basis, its volume can be computed.
among fractions boiling below 150°C in proportion to their
11.1.3 The holdup is treated either as a separate cut or added
yields.
to the residue fraction, in accordance with agreement. The
amount of holdup is determined by actual recovery by solvent NOTE 5—In view of the foregoing rules for establishing yields, the ratio
washing, as directed in 10.5.8, or estimated from Fig. 4. of mass to volume is not precise enough to be used to calculate the density
11.2 Calculate the percent loss to the nearest 0.1 mass %, of any distillate fractions or residue.
using Eq 2. 12. Report
Loss 5 100 2 ~ (100~m/M!! (2) 12.1 A summary sheet for the run must include:
The weight loss as calculated above must not be greater than 12.1.1 The mass of the dry sample charged, g,
0.4 %, otherwise the distillation must be discarded. Losses less 12.1.2 The density of the sample at 15°C, g/mL,
than this should be allocated two thirds to the trap cut and one 12.1.3 The volume of the sample at 15°C, mL,
third to the first naphtha cut. Where there is no trap cut, the 12.1.4 The gain or loss in mass and volume to the nearest
acceptable losses are to be normalized among all cuts. 0.1 %,
11.3 Calculate the volume of the sample of crude oil in 12.1.5 The volume and mass % of each fraction to the
millilitres at 15°C, using Eq 3. nearest 0.1 %,
12.1.6 The cumulative volume and mass percentages, and
V 5 ~M/D! (3)
12.1.7 The mass of water, if any.
where: 12.2 The gas, debutanized naphtha, and succeeding frac-
D = density of charge at 15°C, g/mL, tions are listed in order of ascending boiling point with residue
M = mass of dry charge, g, and recorded last.
V = volume of charge, mL. 12.3 The observations made in 10.3.5, 10.4.7, and 10.5.4 are
11.4 Calculate the volume of each fraction and of the included as a second sheet, which is normally attached to the
residue in millilitres at 15°C, using Eq 4. summary sheet.

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