Designation: D5236 − 03 (Reapproved 2011)

Standard Test Method for

Distillation of Heavy Hydrocarbon Mixtures (Vacuum Potstill
Method)1
This standard is issued under the fixed designation D5236; 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 (´) indicates an editorial change since the last revision or reapproval.

1. Scope 1.5.4 Annex A4—Practice for Conversion of Observed Va-

por Temperature to Atmospheric Equivalent Temperature
1.1 This test method covers the procedure for distillation of
(AET), and
heavy hydrocarbon mixtures having initial boiling points
1.5.5 Annex A5—Test Method for Determination of Wet-
greater than 150°C (300°F), such as heavy crude oils, petro-
tage.
leum distillates, residues, and synthetic mixtures. It employs a
potstill with a low pressure drop entrainment separator oper- 1.6 The values stated in SI units are to be regarded as the
ated under total takeoff conditions. Distillation conditions and standard. The values given in parentheses are for information
equipment performance criteria are specified and typical appa- only.
ratus is illustrated. 1.7 This standard does not purport to address all of the
1.2 This test method details the procedures for the produc- safety concerns, if any, associated with its use. It is the
tion of distillate fractions of standardized quality in the gas oil responsibility of the user of this standard to establish appro-
and lubricating oil range as well as the production of standard priate safety and health practices and determine the applica-
residue. In addition, it provides for the determination of bility of regulatory limitations prior to use. For specific
standard distillation curves to the highest atmospheric equiva- warnings, see 6.5.4.2, 6.5.6.3, 6.9.3, 9.5, 9.7, and A2.3.1.3.
lent temperature possible by conventional distillation.
2. Referenced Documents
1.3 The maximum achievable atmospheric equivalent tem-
2.1 ASTM Standards:2
perature (AET) is dependent upon the heat tolerance of the
D941 Test Method for Density and Relative Density (Spe-
charge. For most samples, a temperature up to 565°C (1050°F)
cific Gravity) of Liquids by Lipkin Bicapillary Pycnom-
can be attained. This maximum will be significantly lower for
eter (Withdrawn 1993)3
heat sensitive samples (for example, heavy residues) and might
D1217 Test Method for Density and Relative Density (Spe-
be somewhat higher for nonheat sensitive samples.
cific Gravity) of Liquids by Bingham Pycnometer
1.4 The recommended distillation method for crude oils up D1250 Guide for Use of the Petroleum Measurement Tables
to cutpoint 400°C (752°F) AET is Test Method D2892. This D1298 Test Method for Density, Relative Density (Specific
test method can be used for heavy crude oils with initial boiling Gravity), or API Gravity of Crude Petroleum and Liquid
points greater than 150°C (302°F). However, distillation curves Petroleum Products by Hydrometer Method
and fraction qualities obtained by these methods are not D1480 Test Method for Density and Relative Density (Spe-
comparable. cific Gravity) of Viscous Materials by Bingham Pycnom-
1.5 This test method contains the following annexes: eter
D2892 Test Method for Distillation of Crude Petroleum
1.5.1 Annex A1—Test Method for Determination of Tem-
(15-Theoretical Plate Column)
perature Response Time,
D4057 Practice for Manual Sampling of Petroleum and
1.5.2 Annex A2—Practice for Calibration of Sensors, Petroleum Products
1.5.3 Annex A3—Test Method for Dehydration of a Wet D4177 Practice for Automatic Sampling of Petroleum and
Sample of Oil, Petroleum Products

1 2
This test method is under the jurisdiction of ASTM Committee D02 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
D02.08 on Volatility. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved Dec. 1, 2011. Published April 2012. Originally the ASTM website.
3
approved in 1992. Last previous edition approved in 2007 as D5236–03(2007). The last approved version of this historical standard is referenced on
DOI: 10.1520/D5236-03R11. www.astm.org.

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

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 D5236 − 03 (2011)
D5002 Test Method for Density and Relative Density of 4.2 The mass of each fraction is obtained. Distillation yields
Crude Oils by Digital Density Analyzer by mass are calculated from the mass of each fraction relative
to the total mass recovery.
3. Terminology
4.3 The density of each fraction is obtained. Distillation
3.1 Definitions of Terms Specific to This Standard: yields by volume are calculated from the volume computed for
3.1.1 boil-up rate, n—the quantity of vapor entering the each fraction at 15°C (59°F) relative to the total recovery.
distillation head per unit time.
3.1.1.1 Discussion—It is approximately equal to the takeoff 4.4 Distillation curves of temperature versus mass or vol-
rate, differing only by the parasitic heat losses. It is expressed ume percent, or both, are drawn using the data from 4.2 and
in millilitres per hour for a head of any given internal diameter 4.3.
or millilitres per hour per square centimetre of cross-sectional
area of the throat for comparative purposes. 5. Significance and Use
3.1.2 condenser, n—the apparatus connected to the outlet of 5.1 This test method is one of a number of tests conducted
the distillation head in which condensation of the product on heavy hydrocarbon mixtures to characterize these materials
occurs. for a refiner or a purchaser. It provides an estimate of the yields
of fractions of various boiling ranges.
3.1.3 distillation flask, n—the flask, of glass or metal, in
which the charge is boiled. 5.2 The fractions made by this test method can be used
3.1.3.1 Discussion—The flask is sometimes called a kettle alone or in combination with other fractions to produce
or pot. samples for analytical studies and quality evaluations.
3.1.4 distillation head, n—the section immediately above 5.3 Residues to be used in the manufacture of asphalt can
the distillation flask containing the entrainment separator. also be made but may not always be suitable. The long heat
3.1.5 distillation pressure (or operating pressure), n—the soaking that occurs in this test method may alter some of the
pressure measured in the distillation head just before the outlet properties.
to the recovery system. NOTE 1—While the practice of reblending distillates with residue can be
3.1.6 distillation temperature (or vapor temperature), done to produce a lighter residue, it is not recommended because it
produces blends with irregular properties.
n—the temperature of the vapors in the distillation head at the
point of measurement. 5.4 Details of cutpoints must be mutually agreed upon
3.1.7 loading, n—the volume of charge relative to the before the test begins.
cross-sectional area of the neck. 5.5 This is a complex procedure involving many interacting
3.1.8 pressure drop, n—the difference between the operating variables. It is most important that at the time of first use of a
pressure and the pressure measured in the distillation flask. new apparatus, its components be checked as detailed in Annex
3.1.8.1 Discussion—It is a result of the friction developed A1 and Annex A2 and that the location of the vapor tempera-
by driving the vapors through the system expressed in kilopas- ture sensor be verified as detailed in 6.5.3 and Fig. 1.
cals (mm Hg).
6. Apparatus
3.1.9 spillover point, n—the lowest point in the head above
the entrainment separator over which the vapors can flow to the 6.1 Four sizes of apparatus, based upon the internal diam-
condensing region. eter of the distillation head (25, 36, 50, and 70 mm), are
3.1.10 static hold-up (or wettage), n—the amount of liquid allowed.4 The apparatus (see Fig. 2) consists of a flask with
material remaining on the inside of the walls of the apparatus heating mantles, an upper compensator, and a head containing
after the distillation has been completed. an entrainment separator. Attached to the head are the vapor
3.1.10.1 Discussion—In this test method, it includes wet- temperature sensor, a connection for the vacuum gage, a
tage of the distillation flask in the case of the steel flasks, but condenser, a rundown line, a product receiver(s), and a vacuum
not in the case of glass flasks that are removed for weighing pumping line with pump. The parts are connected by vacuum-
after the distillation is completed. tight joints to facilitate servicing.
3.1.11 takeoff rate, n—the quantity of product removed per 6.2 Distillation Flask:
unit time. 6.2.1 The sizes specified for flasks are at least 50 % larger
3.1.11.1 Discussion—It is approximately equal to the than the size of the charge to provide space for suppression of
boil-up rate differing only by parasitic heat losses. foam and for bubble breaking. The size of the charge for each
size of still is determined from the loading factor. The
4. Summary of Test Method recommended loading factor is between 200 and 400 mL of
4.1 A weighed volume of sample is distilled at absolute charge per square centimetre of cross sectional area in the neck
pressures between 6.6 and 0.013 kPa (50 and 0.1 mm Hg) at of the head. Table 1 shows the range of charge volume that is
specified distillation rates. Cuts are taken at preselected tem- recommended with each size of apparatus.
peratures. Records of vapor temperature, operating pressure,
and other variables are made at intervals, including at each
cutpoint. 4
Cooke, Industrial and Engineering Chemistry, Vol 55, 1963, p. 36.

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 D5236 − 03 (2011)

STILL HEAD DIMENSION CHART

Size A B C D E F G H I
25 mm 85 mm 75 mm 64 mm 47 mm ID 40 mm OD 4–5 mm 35/25 28/15 35 mm
36 mm 90 mm 75 mm 64 mm 68 mm ID 57 mm OD 5–6 mm 65/40 35/25 35 mm
50 mm 110 mm 100 mm 75 mm 94 mm ID 79 mm OD 7–9 mm 75/50 35/25 45 mm
70 mm 140 mm 100 mm 100 mm 131 mm ID 111 mm OD 10–11 mm 102/75 50/30 70 mm

FIG. 1 Distillation Head

6.2.2 Flasks are made of borosilicate glass except those 6.4.1 The flask shall be heated by means of a nickel
larger than 10 L, which are made of stainless steel for reasons reinforced quartz fabric heating mantle on the lower half so
of safety. that boiling rates of up to 150 mL/h per cm2 of the cross
6.2.3 The flask is fitted with a thermowell reaching to within sectional area of the neck can be maintained. A heat density of
6 mm of the bottom and offset from the center to avoid a 0.5 W/cm2 is adequate. Usually two or more circuits are used
stirring bar. In the case of glass flasks, the bottom shall be to improve heat control by applying automatic heat to the
slightly flattened or slightly concave, but not perfectly flat to bottom circuit.
facilitate the rotation of the magnetic stirrer. Steel flasks can 6.4.2 A temperature sensor shall be located between the wall
have a cooling coil for rapid quenching of the distillation in an of the flask and the mantle for control of the skin temperature.
emergency. Fig. 3 shows a typical example. 6.4.3 The upper half of the flask shall be covered with a
6.3 Stirring System—A magnetically driven stirring bar mantle to compensate for heat losses. A heat density of 0.2
approximately 3-mm diameter and 20-mm long shall be W/cm2 is adequate.
provided for the glass flasks, or 6-mm diameter by 50-mm long 6.5 Distilling Head:
for the steel flasks. The edges shall be rounded to minimize 6.5.1 The head shall conform to the details shown in Fig. 1.
grinding the wall of the flask. The external magnetic drive must It shall be made of borosilicate glass and be totally enclosed in
be capable of rotating the bar in the flask when located directly a silvered glass vacuum jacket having a permanent vacuum of
below and touching the mantle. The drive can be used to less than 0.0001 kPa (0.00075 mm Hg).
support the apparatus above. An adjustable jacking mechanism 6.5.2 The head shall be enclosed in a heat insulating system
is recommended for raising and lowering the stirrer. such as a glass fabric mantle capable of maintaining the outer
6.4 Heating System: wall of the glass vacuum jacket at a temperature 5°C below the

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 D5236 − 03 (2011)

FIG. 2 Apparatus

TABLE 1 Standard Charge and Flask Size 6.5.4 The vapor temperature sensor shall be either a plati-
Inside
Throat num resistance thermometer, a thermocouple with the junction
Cross-Sectional Charge, L Flask, L head fused to the lower tip of the well or any other device
Diameter, mm
Area, cm2
which meets the requirements in 6.5.4 and 6.5.4.1. It shall have
25 5 1–2 2–3
36 10 2–4 3–6 a response time of less than 60 s as described in Annex A1.
50 20 4–8 6–12 6.5.4.1 The vapor temperature measuring device shall have
70 40 8–16 12–24
an accuracy of 0.5°C or better and be measured with a
resolution of 0.1°C or better.
internal vapor temperature in the head. For this purpose the 6.5.4.2 The vapor temperature measuring device shall be
vacuum jacket shall have a temperature sensor fastened to the calibrated over the full range of useful temperatures in com-
outer wall of the jacket at a point level with the vapor bination with its associated instrument at the time of first use
temperature sensor and opposite to the outlet arm of the head. and at least once per year thereafter as described in A2.2.2.
6.5.3 The head shall be fitted with an adapter to support the Alternatively, certified sensors may be used, provided the
vapor temperature sensor so that it is held centered in the neck calibration of the sensor and its associated recording instru-
with the top of the sensing tip 3 6 1 mm below the spillover ment can be traced back to a primary temperature standard.
point. This dimension can be checked by removing the Recalibrate when either the sensor or the instrument is repaired
temperature sensor and inserting in its place a copper wire or serviced. (Warning—Vapor temperature measurement is
having a short right angle bend at the bottom. By feeling for the one of the two major sources of error in distillation data.)
spillover point, the distance from the top joint of the adaptor 6.5.4.3 Verification of the calibration of the vapor tempera-
can be found. Laying the wire on the temperature sensor will ture measuring devices is to be made on a regular basis.
then permit checking of this dimension. Verification at least once a month is recommended. Verification

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 D5236 − 03 (2011)

SYSTEM SIZE A B
25 mm 35/25 3L
36 mm 65/40 6L
50 mm 75/50 12 L
70 mm 102/75 24 L

FIG. 3 Distillation Flask

of the calibration of the sensors can be accomplished poten-

tiometrically by the use of standard precision resistance or by
distilling a pure compound with accurately known boiling
point, as described in A2.2.3.
6.5.5 A head trap as illustrated in Fig. 4 shall be fitted to the
adapter described in 6.5.3 for connection to the vacuum sensor.
It shall be kept filled with crushed dry ice at all times while in
service.
6.5.6 A vacuum sensor shall be connected to the sidearm of
the trap. The sensor shall be capable of reading the pressure
with a precision equal to or better than 0.00133 kPa (0.01 mm
Hg), whichever is greater. A non-tilting McLeod gage can
achieve this accuracy when properly used, but a mercury
manometer will permit this accuracy only down to a pressure
of about 1 kPa and then only when read with a good
cathetometer (an instrument based on a telescope mounted on
a vernier scale to determine levels very accurately). Also,
electronic sensors of the diaphragm type have been found
satisfactory. Vacuum gages based on hot wires, radiation, or FIG. 4 Head Trap and Temperature Sensor
conductivity detectors are not recommended.
6.5.6.1 The non-tilting McLeod gage and the mercury
manometer are primary standards and can be used without provided the calibration of the sensor and its associated
calibration when properly used and maintained. Alternatively, recording instrument can be traced back to a primary pressure
a tensimeter or certified electronic sensors may be used, standard.

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 D5236 − 03 (2011)
6.7.1 A pumping line shall be connected from the outlet of
the condenser to the vacuum pump. The pumping line can be
made of heavy-walled rubber or light metal tubing, but its
inside diameter must be greater than half the inside diameter of
the outlet of the condenser and less than 2 m long.
6.7.2 A surge tank of a size at least equal to the capacity of
the flask shall be inserted in the pumping line adjacent to the
pump.
6.7.3 An isolation valve of a diameter at least equal to the
diameter of the pumping line shall be connected between the
surge tank and the vacuum pump.
6.7.4 A dewar type trap made of borosilicate glass, such as
that illustrated in Fig. 5, shall be placed between the top of the
distillation head and the vacuum sensor. It shall be kept filled
with crushed dry ice at all times during the distillation to
protect the vacuum system from contamination with residual
vapors.
6.8 Vacuum Source—A single stage mechanical vacuum
pump capable of maintaining a steady pressure in the system at
all operating pressures shall be connected to the pumping line.
Automatic or manual control can be used.
6.9 Recovery System:
6.9.1 The recovery system is connected to the lower outlet
of the product condenser and consists of a vacuum adapter to
permit removal of distillate receivers without disturbing the
pressure in the system. A suitable manual device is illustrated
in Fig. 6.
6.9.2 Alternatively, either automatic or manual devices can
CONDENSER DIMENSION CHART
be used to collect part or all of the fractions within the system
System Size A B C D
25 mm 51 mm 28 mm 300 mm 35/25
without disturbing the operating pressure until the end of the
36 mm 75 mm 45 mm 300 mm 65/40 run. Heating must be provided when needed to maintain the
50 mm 80 mm 54 mm 400 mm 75/50 product in the liquid state.
70 mm 120 mm 80 mm 400 mm 102/75
6.9.3 The product receivers shall be made of borosilicate
FIG. 5 Condenser glass and large enough for the size of the fractions to be
collected. They shall be calibrated to the nearest 1 % from the
bottom. (Warning—This apparatus operates under high
vacuum and high temperature. It is recommended that these
6.5.6.2 Noncertified gages shall be calibrated from a non-
stills be kept in an enclosure to ensure that in case of an
tilting McLeod gage or a secondary electronic standard trace-
implosion, the operator and others nearby are protected from
able to a primary standard. A basic calibration procedure is
flying debris, but that the front, at least, be transparent and
described in A2.3. Recalibrate when either the sensor or the
removable for access to controls and so forth. Automated stills,
instrument is repaired or serviced.
which are left unattended for long periods, should be equipped
6.5.6.3 Verification of the calibration of pressure sensors is
with an automatic fire extinguisher, automatic quench, and
to be made on a regular basis. A frequency of at least once a
alarm.)
week is recommended. Verification of the calibration of the
sensors can be accomplished using the procedures described in 7. Sampling
A2.3 or against a certified reference system. (Warning—
Measurement of vacuum (operating pressure) is one of the two 7.1 Obtain the sample for distillation in accordance with
major sources of error in the distillation procedure. It is instructions given in Practice D4057 or Practice D4177. The
therefore of prime importance that the instructions on calibra- sample can also be a residue from Test Method D2892.
tion and verification be followed with great care and on a 7.2 The sample must be in a closed container when received
routine basis.) and show no evidence of leakage.
6.6 Condenser—A condenser made of borosilicate glass, 7.3 If the sample looks waxy or has solidified, warm it
shall be connected to the outlet arm of the head (see Fig. 5). It enough to liquefy it and ensure that it is thoroughly mixed
shall have sufficient capacity to condense essentially all vapors before using.
and capable of operating at coolant temperatures up to 70°C to 7.4 If, upon examination, there is evidence of water in the
prevent wax buildup. sample, perform a preliminary distillation as described in
6.7 Pumping Line: Annex A3.

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 D5236 − 03 (2011)
8.4 Calibrate the temperature and pressure sensors as de-
scribed in Annex A2.

9. Procedure
9.1 Determine the density of the sample by one of the
following test methods: Test Method D941, D1217, D1480,
D5002, or D1298. Refer to Guide D1250 to correct densities to
15°C.
9.2 Insert the stirring bar.
9.3 From Table 1, determine the volume of the charge and
calculate the mass to be charged by multiplying its density by
the desired volume.
9.4 Weigh this mass of charge into the flask to the nearest
0.1 %. In the case of flasks too large to handle, the flask can be
put in place and the charge drawn in from a container (weighed
with its transfer line) using a pressure of 90 to 95 kPa in the
still. The charge may need to be warmed to facilitate transfer.
Its mass can be determined from the difference.
9.5 Attach the flask to the column (in the case of smaller
flasks), and put on all the heating mantles. Put the stirring
device in place and turn it on. (Warning—Ensure that the
safety shield is in place.)
9.6 A contiguous cutting scheme may be achieved in one of
two ways, while remaining within the scope of the key aspects
of this method. It may be achieved by gradually reducing the
pressure over the course of the distillation (dynamic) or done
stepwise, by slowing (or stopping) the takeoff rate to allow
INTERMEDIATE RECEIVER DIMENSION CHART
lowering of the operating pressure to achieve the final cut
System Size A B C temperature. In each case, this must be done keeping in mind
25 mm 45 mm 120 mm 35/25
36 mm 51 mm 120 mm 35/25 the necessity to avoid starving the distillation (due to a slow
50 mm 64 mm 150 mm 50/30 takeoff rate), while at the same time avoiding entrainment (by
70 mm 75 mm 150 mm 50/30 reducing too quickly the pressure applied to the system).
FIG. 6 Receiver System 9.7 Apply heat to the flask at a rate that will raise the
temperature of the charge quickly, but no faster than 300°C/h
(540°F/h). Do not exceed a skin temperature on the flask of
8. Preparation of Apparatus 400°C (750°F) or cracking may result on the walls of the flask.
8.1 Clean and dry all glass parts and assemble them with (Warning—Some hydrocarbon mixtures cannot tolerate
freshly lubricated joints as shown in Fig. 2. In the case of ball 400°C for any useful length of time. Reducing the skin
joints, use only enough lubricant to produce a thin continuous temperature may be necessary in these cases.)
film. An excess of lubricant can promote leakage. The rings of
9.8 Turn on the head compensation mantle and maintain the
O-ring joints should be made of Vitron-A5, or silicone of
outer wall of the glass vacuum jacket at a temperature
equivalent hardness, and be lightly lubricated.
approximately 40°C below the temperature of the liquid in the
8.2 Tare the receivers to the nearest 0.1 % of the weight of flask.
the charge.
9.9 Reduce the pressure in the system gradually to a suitable
8.3 To check for leaks, pump the system down to a pressure starting pressure. Choose from Table 2 the highest pressure that
of approximately 0.05 kPa (0.4 mm Hg) and isolate it from the is consistent with the expected initial boiling point as well as
vacuum source. If, after 1 min, the rise in pressure is no greater the lowest pressure that is consistent with the maximum
than 0.01 kPa (0.075 mm Hg), the system is acceptable. If the cutpoint, using Fig. 7 as a guide. A pressure of 0.133 kPa (1.0
rise in pressure is greater than 0.01 kPa (0.075 mm Hg) in 1 mm Hg) has been found satisfactory for starting a material
min, the gage and its connections must be examined and leaks having an initial boiling point of 343°C (650°F) AET, such as
corrected before proceeding. residues from Test Method D2892 distillations.
NOTE 2—Degassing of the charge is sometimes evident before the
5
Vitron A is a registered trademark of DuPont E.I. De Nemours and Co., actual distillation begins. This appears as bubbling at the surface without
Wilmington, DE 19898. generation of condensable vapors.

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 D5236 − 03 (2011)
TABLE 2 Operating Pressures and Distillation Rates
Operating Boil-Up Take-Off Rate, mL/h
Pressure, Rate, mL/
kPa (mm Hg) (h·×·cm 2) 25 mm 36 mm 50 mm 70 mm
6.67 (50) 90–150 450–750 900–1500 1800–3000 3600–6000
1.33 (10) 75–125 375–625 750–1250 1500–2500 3000–5000
0.133 (1) 45–75 225–375 450–750 900–1500 1800–3000
0.0400 (0.3) 30–50 150–250 300–500 600–1000 1200–2000
0.0133 (0.1) 10–20 50–100 100–200 200–400 400–800

FIG. 7 Correction of Vapor Temperature to Atmospheric Equivalent

9.10 When distillation begins, evidenced by vapors entering NOTE 3—Although a range of distillation rates is permitted, 80 % of the
the neck of the flask, reduce the heat input to a level that will maximum allowed is recommended.
maintain the chosen distillation rate from Table 2 (see Note 2). 9.11 In cases in which the observed initial vapor tempera-
Adjust the heat compensator on the head to maintain the outer ture will be 150°C (302°F) or lower, it is desirable to
wall of the glass vacuum jacket at a temperature 5°C below the refrigerate the first fraction receiver to ensure the retention of
vapor temperature. light ends. If solid waxy material appears on the walls, warm

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 D5236 − 03 (2011)
the receiver with an infrared heat lamp or hot air gun to liquify until the temperature of the boiling liquid reaches approxi-
the product in the receiver in order to improve the accuracy of mately 290°C (554°F).
the reading. In automatic operation, the receivers must be 9.17 At this point, if the final cutpoint cannot be achieved
thermostated at a temperature high enough to ensure that no before reaching 320°C (608°F) in the boiling liquid, reduce the
solidification takes place and low enough to prevent evapora- heat input to zero until the distillation slows or stops. This will
tion of light material. take 2 to 10 min depending on the amount of material in the
9.12 When using the dynamic method of pressure reduction, flask. Reduce the pressure slowly to a level that will allow for
calculate a projected final cutpoint using the operating pressure a reasonable amount of overhead product to evolve at the new
and the differential between the vapor and pot temperature as pressure level. A pressure reduction by a factor of five or six
the operating envelope. Estimating that the difference between has been shown to be necessary to produce a viable quantity of
the vapor and the pot temperature remain relatively constant, overhead at the new pressure level.
determine if the final vapor temperature can be achieved at this 9.18 Restore the heat to about 90 % of the previous level
pressure while remaining within the recommended limitations and then adjust to give the desired rate at the lower level (see
of the flask temperature (see 9.18). If the final cutpoint cannot Table 2). Do not take any cuts until the pressure has stabilized
be achieved at the starting pressure, the pressure should be at the new level for at least 2 min. Repeat 9.16 and 9.17 until
gradually lowered toward an operating pressure that will allow a pressure level has been reached that will allow for achieving
the final cut to be taken. This must be done bearing in mind the the final cutpoint before the boiling liquid reaches a tempera-
associated takeoff rates for the vacuum pressures indicated in ture of 320°C (608°F).
Table 2 and the limitations of the pot temperature. The pressure
should be lowered enough to allow the takeoff rate to acceler- 9.19 Continue taking product as long as there is no indica-
ate briefly while the operator is remaining vigilant to avoid tion of incipient cracking. Addition of heat to the flask to
entrainment. The distillation rate at the operating pressure maintain product rate should be done with great care. It is
should fall within the recommendations stated in Table 2 and recommended to achieve the final cutpoint in less than 1 h after
should be allowed to stabilize for at least 2 min before arriving the flask temperature has risen above 310°C (590°F).
at a cutpoint. Experience has shown that reduced crude oil 9.20 The distillation shall be discontinued immediately as
samples typically run well at 0.133 kPa for up to 25 - 30 % of soon as signs of incipient cracking are observed (see Note 4).
the charge volume. Subsequent lowering of the operating
NOTE 4—Cracking will significantly affect the quality of the cuts and
pressure, as described above, has yielded satisfactory results. the residue, for example, the densities and viscosities would be signifi-
Repeat this procedure throughout the remainder of the distil- cantly lower than those obtained without cracking.
lation until an operating pressure has been attained that will NOTE 5—Incipient cracking is usually first observed from a distinct and
allow the final cut temperature to be reached while remaining persistent rise in pressure (for example, >10 % of pressure set point) or an
within the recommended confines of the maximum pot tem- increase of the demand on the vacuum pump capacity. However, auto-
matic vacuum controllers tend to mask these phenomena. Other signs of
perature and temperature/time constraints of flask temperature incipient cracking are the accumulation of thin black deposits on the
(see 9.18). glassware through the column or the appearance of a smoke-like vapor in
9.13 When the receiver is full, or when a cutpoint is the system after the condenser.
reached, isolate the receiver or move to the next one, as the 9.21 When either the final cutpoint or 90 volume % has
case may be. been distilled or incipient cracking is observed, discontinue the
9.13.1 In manual operation, isolate the receiver using the distillation. Discontinue heat input to the flask and heating
vacuum adaptor and vent it to atmospheric pressure before jacket at once and slightly raise the pressure of the system by
replacing it with another tared receiver. Apply vacuum, and reducing the vacuum pump capacity. Allow the residue to cool
when the new receiver is at approximately system pressure, while stirring.
reconnect it to the system.
NOTE 6—Beyond 90 volume % distilled, the flask may be too near
9.13.2 In automatic operation, receivers are changed auto- dryness for safe operation.
matically and do not normally need further attention.
9.22 Remove the flask compensating mantle, or in the case
9.14 Record the following observations: of steel flasks, turn on the air in the quench coil.
9.14.1 Time in hours and minutes,
9.14.2 Volume of distillate in millilitres, 9.23 When the temperature of the residue has fallen below
9.14.3 Vapor temperature to nearest 0.5°C, 150°C (302°F), remove and weigh the flask and contents to
9.14.4 Liquid temperature in the flask in °C, determine the mass of the residue. For larger stills, the residue
9.14.5 Pressure in the head to nearest 1 %, and can be discharged through the charging line using a positive
pressure of about 10 kPa in the still.
9.14.6 Atmospheric equivalent temperature by calculation
as prescribed in Annex A4. 9.24 Weigh all overhead fractions to within 0.1 % of the
9.15 Proceed to 9.18. charge mass.

9.16 Alternatively, the stepwise method can be achieved by 9.25 Determine the relative density of all fractions and
initializing the distillation and operating at the pressure at convert to 15°C (59°F) using Guide D1250 where applicable.
which the distillation stabilizes (see 9.9). Continue taking 9.26 In the case of the smaller stills, recover the wettage by
product and making cuts until the final cutpoint is achieved or boiling up a small quantity of solvent such as toluene in a

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 D5236 − 03 (2011)
separate flask to wash the head and condenser. Evaporate the
solvent in a hood assisted by a stream of air and weigh directly.
This wettage may be treated as a separate fraction and its
density estimated or blended into the residue before inspections
are made. The latter must be done if the residue is to be
analyzed for other than density. For larger stills, follow
instructions given in Annex A5. Note that the holdup in the
latter case includes both the overhead wettage and the wettage
of the flask with residue and must be considered a separate
fraction. Density must be measured in this case.

10. Calculation
10.1 Calculate the weight recovery by adding the masses of
all the fractions plus the holdup or wettage. The total must be
between 99.6 % and 100.1 % of the weight of the charge to be
acceptable. Show the actual loss on the record, and prorate the
loss among all fractions.
10.2 Calculate the volume of each fraction by dividing the
mass of each fraction by its relative density.

11. Report
11.1 A summary sheet for the run must include the follow-
ing:
11.1.1 The mass of the charge in grams,
11.1.2 The density of the charge in grams per millilitre at
15°C to four significant figures,
11.1.3 The volume of the charge in millilitres at 15°C,
11.1.4 The gain or loss in mass and volume to the nearest
0.1 %,
11.1.5 A listing of the fractions in order of boiling point
with the residue recorded last, and
11.1.6 The cumulative mass and volume percentages.
FIG. 8 Distillation Report
11.2 The observations recorded in 9.14 during the distilla-
tion are normally included as a second sheet attached to the under constant operating conditions on identical test materials
summary sheet. Examples of a distillation report and record are would, in the long run, in the normal and correct operation of
illustrated in Fig. 8 and Fig. 9. this test method, exceed the following values only in one case
11.3 Plot curves of temperature in degrees Celsius AET as in twenty:
ordinates against the percents by mass and volume calculated Liquid Volume (LV), % Distilled Repeatability, °C
for the fractions above. A smooth curve through this plot 10 6.1
20 4.5
constitutes the final distillation curve. 30 6.1
40 4.9
12. Precision and Bias 50 5.7
60 4.1
12.1 Precision—The precision of this test method as deter- 70 4.8
mined by the statistical examination of the interlaboratory test 80 4.9
90 4.4
results is as follows:6
12.1.2 Reproducibility—The difference between two single
NOTE 7—The following precision data were developed from data
obtained from a 1986 cooperative program (six samples, five laboratories),
and independent results obtained by different operators work-
a 1988 cooperative program (three samples, four laboratories), and ing in different laboratories on identical material would, in the
individual laboratory data on different samples (five samples, three long run, exceed the following values only in one case in
laboratories). Although these data do not meet the statistical requirements twenty:
of RR:D02-1007, due to the time and cost involved it is unlikely that an
Liquid Volume (LV), % Distilled Reproducibility, °C
additional cooperative program will be initiated soon. 10 16.9
12.1.1 Repeatability—The difference between successive 20 12.8
30 13.5
results obtained by the same operator with the same apparatus 40 11.2
50 14.2
60 8.4
6
Supporting data have been filed at ASTM International Headquarters and may 70 11.4
be obtained by requesting Research Report RR:D02-1288. 80 5.1

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 D5236 − 03 (2011)

FIG. 9 Distillation Record

90 4.4 13. Keywords

12.2 Bias—Since there is no accepted reference material 13.1 crude oils; distillation; heavy oils; potstill; residue;
suitable for determining the bias for the procedure in this test vacuum
method for measuring vacuum distillation characteristics, bias
has not been determined.

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 D5236 − 03 (2011)
ANNEXES

(Mandatory Information)

A1. TEST METHOD FOR DETERMINATION OF TEMPERATURE RESPONSE TIME

A1.1 Scope allowing interpolation to 0.1°C (0.2°F). Set the chart speed at
A1.1.1 The test method in this annex is for the determina- 30 cm/h for readability.
tion of temperature response time based upon the rate of A1.3.3 Insert the sensor into a hole in the center of one side
cooling of the sensor under prescribed conditions. of a closed cardboard box about 30 cm on a side. Hold the
sensor in place by a friction fit on the joint. Allow the sensor to
A1.2 Significance and Use reach equilibrium temperature. Record the temperature when it
A1.2.1 This test method is performed to ensure that the becomes stable.
sensor is able to respond to changes in temperature fast enough A1.3.4 Remove the sensor and insert it into the heated
that no error due to lag is introduced in a rapidly rising thermowell in the beaker of water. After the sensor has reached
temperature curve. a temperature of 70°C (158°F), remove it and immediately
A1.2.2 The importance of this test method is greatest under insert it into the hole in the box. Note with a stopwatch, or
vacuum conditions when the heat content of the vapors is record on the strip chart, the time interval while the sensor
minimal. cools from 30°C (54°F) above to 5°C (9°F) above the tem-
perature recorded in A1.3.3.
A1.3 Procedure
A1.3.5 A time interval in excess of 60 s is unacceptable.
A1.3.1 Arrange a 1-L beaker of water on a hot plate with a
glass thermowell supported vertically in the water. Maintain A1.4 Precision and Bias
the temperature of the water at 80 6 5°C (175 6 9°F). A1.4.1 No statement is made concerning either the preci-
A1.3.2 Connect the sensor to an instrument, preferably with sion or bias of this annex for determining the temperature
a digital readout, with readability to 0.1°C. Alternatively, response time because the result is used to determine whether
connect the sensor to a strip chart recorder of suitable range there is conformance to the stated criteria in this test method.

A2. PRACTICE FOR CALIBRATION OF SENSORS

A2.1 Principle one or more thermocouples or other sensors connected to their

A2.1.1 This practice deals with the basic calibration of respective measuring instruments.
temperature sensors and vacuum sensors and their associated A2.2.2.2 Heat the melting point bath to a temperature 10°C
recording instruments. above the melting point of the metal inside and hold at this
temperature for at least 5 min to ensure that all the metal has
A2.1.2 The temperature sensor with its associated instru-
melted.
ment is calibrated by observing and recording the temperature
of the melting point and boiling point of pure compounds or A2.2.2.3 Discontinue heat input to the melting point bath
eutectic mixtures. and observe and record the cooling curve. When the curve
exhibits a plateau of constant temperature for longer than 1
A2.1.3 The vacuum sensor and its associated instrument is min, the temperature of the recorded plateau is accepted as the
calibrated against a McLeod gage or a certified reference gage calibration temperature. If the freezing plateau is too short, it
over the full operating range of pressure. can be prolonged by employing some heat during the cooling
A2.2 Temperature Sensors cycle. Alternatively, the melt bath may have become contami-
nated or excessively oxidized. In this case, replace the metal.
A2.2.1 Apparatus—A suitable apparatus is shown in Fig.
A2.1. For the freezing point of water, a Dewar flask filled with A2.2.2.4 Record the calibration temperature at each of the
crushed ice and water can be substituted. For the boiling point points in Table A2.1 to the nearest 0.1°C.
of water, use an equilibrium still or ebulliometer, a Tensimeter A2.2.2.5 Set up a correction table by listing the correction to
as shown in Fig. A2.2, or other apparatus for measuring be added algebraically to the observed temperature to give the
vapor-liquid equilibrium. true temperature at each calibration point. A graphical plot of
the above corrections connected by a smooth curve may be
A2.2.2 Procedure A—Vapor Temperature Sensor Calibra-
helpful in routine use.
tion by Melting Point:
A2.2.2.1 Ensure that approximately 0.5 mL of silicone oil or A2.2.3 Procedure B—Vapor Temperature Sensor Verifica-
other inert liquid is in the bottom of the thermowell and insert tion by Boiling Point:

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 D5236 − 03 (2011)

FIG. A2.2 Tensimeter

FIG. A2.1 Melting Point Bath for Temperature Standards TABLE A2.1 Primary Temperature Standards (Melting Points)
Material Temperature, °C
Ice Melting point 0.0
Tin:Lead:Cadmium Melting point 145.0
A2.2.3.1 This practice is not regarded as primary tempera- (50:32:18)
ture reference but is an acceptable procedure for verification of Sn Melting point 231.9
calibrated temperature sensors. Pb Melting point 327.4

A2.2.3.2 Set up the instrument for measuring vapor-liquid

equilibrium, following the instructions of the manufacturer.
TABLE A2.2 Boiling Points at Atmospheric Pressure
Use only pure (>99.9 % purity) liquids with an accurately
Material Temperature, °C
known boiling point. A list of some materials, which have been
Water 100.0
found suitable for this purpose, is given in Table A2.2. n-Heptane 98.5
Tetrahydronaphthalene 207.2
NOTE A2.1—A tensimeter is a convenient instrument to measure
Tetradecane 252.5
vapor-liquid equilibrium.
A2.2.3.3 Follow the instructions of the instrument manufac-
turer and record the temperature at each of the points in Table
A2.2 to the nearest 0.1°C. A2.3.1.2 The only primary standard for the measurement of
A2.2.3.4 Set up a table by listing the correction to be added absolute pressure for pressures below 13.3 kPa is the non-
to the observed temperature to give the true temperature at each tilting McLeod gage because it is calibrated from measurement
of the verification points. If the corrections obtained differ by of its dimensions.
more then 0.4°C from the corrections obtained during calibra- NOTE A2.2—The general principles of construction of McLeod gages
tion (see A2.2.2.1), the system shall be considered as out of are well-established. The dimensions and tolerances of such a gage are
control and the sensor, with its associated instrument, shall be beyond the scope of this test method.
recalibrated. A2.3.1.3 Choose a McLeod gage with a range such that the
desired calibration pressure falls between 10 % and 90 % of the
A2.3 Vacuum Sensors scale. Before refilling with clean mercury, heat the empty
A2.3.1 Apparatus: reference McLeod gage at 250°C for at least 30 min at a
A2.3.1.1 Assemble a vacuum manifold such as that shown pressure below 10 Pa (0.075 mm Hg). Thereafter, carefully
in Fig. A2.3. It must be capable of maintaining steady pressures protect the reference gage from exposure to moisture such as
within 1 % at all desired levels. that from atmospheric air. The use of two reference McLeod

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 D5236 − 03 (2011)
back to a primary standard. Secondary gages shall be re-
certified at a regular basis, but at least once a year.
A2.3.2 Procedure:
A2.3.2.1 Set up the test manifold such as that shown in Fig.
A2.3. Ensure that the test manifold is clean, dry, leak-free, and
can be maintained at a steady pressure at the required level. A
suitable leak test is to pump down to a pressure below 0.01
kPa. Isolate the pump and the bleed valve. Allow the system to
stabilize for at least 2 min. If the pressure rises more than 10 %
in the next 2 min, the system must be checked for leaks and
corrected before continuing with calibration.
A2.3.2.2 Connect the reference (primary) vacuum gage(s)
and the gage(s) to be calibrated to the manifold. The gages
shall have such a range that the desired calibration pressure
falls between 10 % and 90 % of the scale. Insert a dry ice trap
between the manifold and the vacuum pump. Adjust the
pressure to the required level for the test, and run a final leak
test as above.
A2.3.2.3 After steady conditions have been maintained for
at least 3 min, make readings of all gages and compare with the
FIG. A2.3 Calibration of Vacuum Gages
reference gage.
A2.3.2.4 Repeat the above procedure at the other required
gages of different pressure ranges is recommended as a pressure levels. At least three pressure levels, covering between
precaution. If they agree at the test pressure, it is an indication 10 % and 90 % of the scale, are required for each test gage.
that the system is free of moisture and other condensables. A2.3.2.5 Make up a chart of corrections to be added at each
(Warning—Mercury vapor is poisonous. Harmful or fatal if pressure level for each gage tested. This can be used for
inhaled or ingested.) interpolation when necessary. Alternatively, the settings of
A2.3.1.4 Alternatively, certified secondary gages, electronic electronic gages, if so equipped, may be adjusted to eliminate
or otherwise, can be used, provided the output can be traced the error.

A3. TEST METHOD FOR DEHYDRATION OF A WET SAMPLE OF OIL

A3.1 Scope A3.5 Procedure

A3.1.1 The test method in this annex is for dehydrating a A3.5.1 Decant any bulk water that may be present. Weigh
wet sample of oil (>0.1 % water) prior to vacuum distillation by difference to the nearest gram, the required volume of wet
and determining the water content. sample into a distillation flask containing a magnetic stirrer.
A3.2 Summary of Test Method A3.5.2 Attach the flask to the distillation head and pass a
slow (8 cm3/s) stream of nitrogen through the capillary. Vent
A3.2.1 A sufficient quantity of the sample is distilled under the condenser through a trap maintained at the temperature of
atmospheric pressure to 150°C, the hydrocarbon fraction de- dry ice (−70°C (−94°F)).
canted, and dry components recombined. The mass percent of
water is calculated. A3.5.3 Apply heat to the flask, regulating it to attain a
moderate rate. Remove distillate slowly until water ceases to
A3.3 Significance and Use distill and continue for an additional 3 to 5 % of distillate.
A3.3.1 Dehydration is important in order to allow the A3.5.4 Shut off the heating system. Cool the flask and
subsequent distillation to proceed smoothly. contents to below 175°C temperature.
A3.4 Apparatus A3.5.5 Weigh the distillate fraction and residue.
A3.4.1 The dehydration of a wet sample requires apparatus A3.5.6 To separate the water from the distillate fraction,
such as that shown in Fig. 1. Fit the distillation flask with a cool to −5°C and decant the hydrocarbon liquid. Weigh the
capillary line for the passage of nitrogen into the liquid. water.

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 D5236 − 03 (2011)
A3.5.7 Remove the condenser and rinse it with alcohol or where:
acetone to remove adhering drops of water. Dry with air and A = mass of water recovered, g,
replace it. B = mass of charge, g,
A3.5.8 Recombine the cooled decanted fractions with the W = mass percent of water, and
distillation residue, observing the usual precautions against 100 = percentage constant.
losses. If the reblending is done in the original flask, this flask
can be used for the subsequent distillation. Do not recombine A3.8 Precision and Bias
the trap fraction. A3.8.1 No statement is made concerning either the preci-
A3.5.9 Record the quantity of dry oil recovered. sion or bias of this annex for mass percent water because the
A3.7 Calculation test method in this annex is used for sample preparation for
Test Method D5236.
A3.7.1 Calculate the mass percent of water using Eq A3.1:
100 A
W5 (A3.1)
B

A4. PRACTICE FOR CONVERSION OF OBSERVED VAPOR TEMPERATURE TO ATMOSPHERIC EQUIVALENT TEM-
PERATURE (AET)

A4.1 Scope where:

A4.1.1 This practice is for conversion of the actual distilla- P = operating pressure, mm Hg.
tion temperature obtained at sub-ambient pressure to atmo- A4.3.1.2 If the operating pressure <0.266 kPa (<2 mm Hg),
spheric equivalent temperature (AET) corresponding to the calculate A using Eq A4.4 or Eq A4.5:
equivalent boiling point at atmospheric pressure, 101.3 kPa
(760 mm Hg), by means of equations derived by Maxwell and 5.897249 2 0.987672 log10 P
A5 (A4.4)
Bonnell.7 2962.909 2 43.00 log10 P

where:
A4.2 Significance and Use
P = operating pressure, kPa, or
A4.2.1 Final data on atmospheric equivalent temperatures
are to be obtained by computation. Fig. 7 is provided only as
a guide in estimating the AET during distillation. 6.761559 2 0.987672 log10 P
A5 (A4.5)
3000.538 2 43.00 log10 P
A4.3 Calculation
where:
A4.3.1 Convert observed vapor temperature to atmospheric
P = operating pressure, mm Hg.
equivalent temperature using Eq A4.1:
748.1A A4.3.2 The equations are correct only for fractions that have
AET 5 2 273.1(A4.1) a Watson K-factor of 12.0 6 0.2. The K-factor shall be
@ 1/ ~ T1273.1! # 10.3861A 2 0.00051606
assumed to be 12 and any effect of K-factor ignored unless
where: there is mutual agreement to the contrary.
AET = atmospheric equivalent temperature, °C, and
T = observed vapor temperature, °C. A4.3.3 If correction is required, calculate the K-factor using
Eq A4.6:
A4.3.1.1 If the operating pressure $0.266 kPa ($2 mm
Hg), calculate A using Eq A4.2 or Eq A4.3: =3 1.8 ~ B1273.1!
K5 (A4.6)
D
5.143222 2 0.972546 log10 P
A5 (A4.2)
2579.329 2 95.76 log10 P
where:
where:
B = mean average boiling point, °C, and
P = operating pressure, kPa, or D = relative density at 15.6/15.6°C.
By custom, either the mid-vapor temperature of the fraction
5.994295 2 0.972546 log10 P or the midpoint of a gas chromatographic distillation of the
A5 (A4.3)
2663.129 2 95.76 log10 P fraction can be used for the mean average boiling point. In
either case the method must be specified.
7
Maxwell and Bonnell, Industrial Engineering Chemistry , Vol 49, 1957, p. A4.3.3.1 An estimate of the K-factor can be made using Fig.
1187. A4.1.

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 D5236 − 03 (2011)

NOTE 1—Reprinted from API Technical Data Book, June 1980, by permission of American Petroleum Institute.

FIG. A4.1 Watson Characterization Factor of Petroleum Fractions

A4.3.4 Calculate the correction to be applied to the AET t = correction, °C,

using Eq A4.7: Pa = atmospheric pressure, kPa (mm Hg), and
Po = observed pressure, kPa (mm Hg).
F S DG
t 5 21.4 @ K 2 12# log10
Pa
Po
(A4.7)
A4.3.4.1 An estimate of the correction can be made using
where: Fig. A4.2.

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 D5236 − 03 (2011)

FIG. A4.2 Boiling Point Corrections for K—Factor

A5. TEST METHOD FOR DETERMINATION OF WETTAGE

A5.1 Scope A5.4 Procedure

A5.1.1 The test method in this annex is for determining the A5.4.1 Charge the dirty still with a volume of toluene equal
amount of material that remains on the inside walls of the to 10 to 20 % of a normal charge.
apparatus after a distillation is complete. It is intended for use A5.4.2 Apply heat and boil the toluene until all the upper
mainly with stills having flasks too large for easy dismantling, parts are well rinsed (about 3 min), and shut down.
but can also be used for smaller stills.
A5.4.3 After the still has cooled, recover the liquid from
A5.2 Summary of Test Method flask and distill off the solvent in a hood. Elimination of the last
A5.2.1 A small charge of solvent is distilled in the dirty traces can be assisted by a gentle stream of air.
apparatus after a run. The residue is discharged and then freed A5.4.4 Weigh the recovered wettage and determine its
of solvent to recover the wettage. density.
A5.3 Significance and Use A5.4.5 Treat the wettage as a separate fraction.
A5.3.1 Distillation apparatus can retain up to 0.5 % of a A5.5 Precision and Bias
charge on their inside surfaces at the end of a run. A5.5.1 No statement is made concerning either the preci-
A5.3.2 Wettage includes that of the flask because the flask is sion or bias of this annex for measuring wettage because the
not removed for separate treatment. result is used solely within the context of Test Method D5236.

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 D5236 − 03 (2011)
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