ASTM D5853-95
(Test Method)Standard Test Method for Pour Point of Crude Oils
Standard Test Method for Pour Point of Crude Oils
SCOPE
1.1 This test method covers two procedures for the determination of the pour point temperatures of crude oils down to -36oC. One method provides a measure of the maximum (upper) pour point temperature (Procedure A) and is described in 9.1; the other method provides a measure of the minimum (lower) pour point temperature (Procedure B) and is described in 9.2.
1.2 The use of this test method is limited to use for crude oils. Pour point temperatures of other petroleum products can be determined by Test Method D97.
1.3 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use. For specific hazard statements, see Section 7.
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Designation: D 5853 – 95 An American National Standard
Designation: 441/99
Standard Test Method for
Pour Point of Crude Oils
This standard is issued under the fixed designation D 5853; 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 3.1.1 pour point, n—the lowest temperature at which move-
ment of the test specimen is observed under the conditions of
1.1 This test method covers two procedures for the deter-
the test.
mination of the pour point temperatures of crude oils down
3.1.2 maximum (upper) pour point, n—the pour point ob-
to − 36°C. One method provides a measure of the maximum
tained after the test specimen has been subjected to a pre-
(upper) pour point temperature (Procedure A) and is described
scribed treatment designed to enhance gelation of wax crystals
in 9.1; the other method provides a measure of the minimum
and solidification of the test specimen.
(lower) pour point temperature (Procedure B) and is described
3.1.3 minimum (lower) pour point, n—the pour point ob-
in 9.2.
tained after the test specimen has been subjected to a pre-
1.2 The use of this test method is limited to use for crude
scribed treatment designed to delay gelation of wax crystals
oils. Pour point temperatures of other petroleum products can
and solidification of the test specimen.
be determined by Test Method D 97.
1.3 This standard does not purport to address all of the
4. Summary of Test Method
safety concerns, if any, associated with its use. It is the
4.1 After preliminary heating, the test specimen is cooled at
responsibility of the user of this standard to establish appro-
a specified rate and examined at intervals of 3°C for flow
priate safety and health practices and determine the applica-
characteristics. The lowest temperature at which movement of
bility of regulatory limitations prior to use. For specific hazard
the test specimen is observed is recorded as the pour point.
statements, see Section 7.
5. Significance and Use
2. Referenced Documents
5.1 The pour point of a crude oil is an index of the lowest
2.1 ASTM Standards:
temperature of handleability for certain applications.
D 97 Test Method for Pour Point of Petroleum Products
5.2 This is the only pour point method specifically designed
D 130 Test Method for Detection of Copper Corrosion from
for crude oils.
Petroleum Products by the Copper Strip Tarnish Test
5.3 The maximum and minimum pour point temperatures
D 323 Test Method for Vapor Pressure of Petroleum Prod-
2 provide a temperature window where a crude oil, depending on
ucts (Reid Method)
its thermal history, might appear in the liquid as well as the
D 4057 Practice for Manual Sampling of Petroleum and
3 solid state.
Petroleum Products
5.4 The test method can be used to supplement other
D 4177 Practice for Automatic Sampling of Petroleum and
3 measurements of cold flow behavior. It is especially useful for
Petroleum Products
4 the screening of the effect of wax interaction modifiers on the
E 1 Specification for ASTM Thermometers
flow behavior of crude oils.
E 77 Test Method for Inspection and Verification of Ther-
mometers
6. Apparatus
6.1 Pour Point Test Apparatus Assembly (see Fig. 1):
3. Terminology
6.1.1 Test Jar, cylindrical, of clear glass, flat bottomed,
3.1 Definitions of Terms Specific to This Standard:
outside diameter 33.2 to 34.8 mm, and height 115 to 125 mm.
The inside diameter of the jar can range from 30.0 to 32.4 mm,
This test method is under the jurisdiction of ASTM Committee D-2 on
within the constraint that the wall thickness shall be no greater
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
than 1.6 mm. The jar shall have a line to indicate a sample
D02.07 on Flow Properties.
Current edition approved Oct. 10, 1995. Published December 1995.
height 54 6 3 mm above the inside bottom. The inside of the
Annual Book of ASTM Standards, Vol 05.01.
test jar (up to the mark) shall be visibly clean and free of
Annual Book of ASTM Standards, Vol 05.02.
4 scratches.
Annual Book of ASTM Standards, Vol 14.03.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 5853
NOTE 1—All dimensions are stated in millimetres.
FIG. 1 Apparatus for Pour Point Test
6.1.2 Thermometers, having ranges shown in the following position is essential. The bath temperature shall be monitored
table and conforming to the requirements prescribed in Speci- by means of the appropriate thermometer (6.1.2) or any other
fication E 1 for thermometers: temperature measuring device capable of measuring and dis-
playing the designated temperature with the required precision
Thermometer
Number
and accuracy. The required bath temperatures shall either be
Thermometer Temperature Range
ASTM IP
maintained by refrigeration or by suitable freezing mixtures
(Note 1) and shall maintain the designated temperatures to
High cloud and pour −38 to +50°C 5C 1C
Low cloud and pour −80 to +20°C 6C 2C
within6 1.5°C.
Melting point +32 to +127°C 61C 63C
NOTE 1—The cooling mixtures commonly used are as follows :
6.1.2.1 Since separation of liquid column thermometers
For Temperatures
occasionally occurs and may escape detection, the ice point of
Down To
the thermometers shall be checked prior to the test and used Ice and water 9°C
Crushed ice and sodium chloride crystals −12°C
only if they are accurate within6 1°C (see Test Method E 77).
Crushed ice and calcium chloride crystals −27°C
6.1.3 Cork, to fit the test jar, center bored for the test
Acetone or petroleum naphtha (see Section 7) −57°C
thermometer. chilled in a covered metal beaker with an
ice-salt mixture to −12°C and then with
6.1.4 Jacket, watertight, cylindrical, metal, flat bottomed,
enough solid carbon dioxide to give the
115 6 3 mm depth, with inside diameter of 44.2 to 45.8 mm.
desired temperature.
It shall be supported in a vertical position in the cooling bath
6.2 Water Bath—The size and shape of the bath are op-
(6.1.7) so that no more than 25 mm projects out of the cooling
tional, but a support to hold the test jar immersed in the bath to
medium. The jacket shall be capable of being cleaned.
above the sample height in the test jar and in a firm vertical
6.1.5 Disk, cork or felt, 6 mm thick to fit loosely inside the
position is required. The required bath temperature may be
jacket.
maintained by any suitable means, provided the temperature
6.1.6 Gasket, to fit snugly around the outside of the test jar
can be monitored and controlled to the designated temperature
and loosely inside the jacket. The gasket shall be made of
(61°C (9.1.4; 9.2.4)).
rubber, leather, or other material that is sufficiently elastic to
6.3 Pressure Vessel, constructed of stainless steel according
cling to the test jar and hard enough to hold its shape. Its
purpose is to prevent the test jar from touching the jacket.
This pressure vessel is identical to the pressure vessel described in Test Method
6.1.7 Cooling Bath or Baths, of a type suitable for obtaining
D 130.
the required temperatures. The size and shape of the bath are
The results of the cooperative test program from which these values have been
options, but a support to hold the jacket firmly in a vertical derived are filed at ASTM Headquarters. Request RR:D02-1371.
D 5853
to the dimensions given in Fig. 2, and capable of withstanding 7.1.1 Acetone.
a test pressure of 700 kPa. Alternative designs for the pressure
NOTE 2—Warning: Extremely flammable.
vessel cap and synthetic rubber gasket may be used provided
7.1.2 Alcohol, Ethanol.
that the internal dimensions of the pressure vessel are the same
as those shown in Fig. 2.
NOTE 3—Warning: Flammable.
6.4 Timing Device, capable of measuring up to 30 s with a
7.1.3 Alcohol, Methanol.
resolution of at least 0.1 s and an accuracy of 60.2 s or better.
NOTE 4—Warning: Flammable. Vapor harmful.
7. Reagents and Materials
7.1.4 Petroleum Naphtha.
7.1 The following solvents of technical grade are appropri-
ate for low-temperature bath media. NOTE 5—Warning: Combustible. Vapor harmful.
FIG. 2 Pressure Vessel
D 5853
NOTE 6—Typical petroleum naptha used for cleaning purposes are VM
the expected pour point, whichever is higher.
and P napthas.
9.1.4.1 As soon as the test specimen has reached the
7.2 Toluene, technical grade. required temperature, remove the cork carrying the thermom-
eter and stir the test specimen gently with a spatula or similar
NOTE 7—Warning: Flammable. Vapor harmful.
device. Put the cork carrying the thermometer back in place
7.3 Solid Carbon Dioxide.
(see 9.1.2).
9.1.5 Ensure that the disk, gasket, and the inside of the
NOTE 8—Warning: Extremely cold (−78.5°C).
jacket are clean and dry. Place the disk in the bottom of the
8. Sampling, Test Samples, and Test Specimens
jacket. Place the disk and jacket in the cooling medium a
minimum of 10 min before the test jar is inserted. The use of
NOTE 9—Sampling is defined as all steps required to obtain a portion of
a jacket cover, while the empty jacket is cooling, is permitted.
the contents of any pipe, tank, or other system and to place the sample into
the laboratory test container. Remove the test jar from the water bath and dry with a tissue.
Place the gasket around the test jar, 25 mm from the bottom.
8.1 Laboratory Sample—It is essential that the sample
Insert the test jar into the jacket in the first bath maintained at
received by the laboratory is representative of the batch or lot
21°C and commence observations for pour point. Never place
of crude oil from which it was taken. Practices D 4057 and
a test jar directly into the cooling medium.
D 4177 provide guidance for obtaining such representative
9.1.6 Exercise care not to disturb the mass of test specimen
samples.
nor permit the thermometer to shift in the test specimen; any
8.2 Preparation of Test Samples—The pour point of crude
disturbance of the spongy network of wax crystals will lead to
oils is very sensitive to trace amounts of high melting waxes.
a lower pour point and erroneous results (Note 12).
Exercise meticulous care to ensure such waxes, if present, are
either completely melted or, if volatility constraints prevent
NOTE 13—With dark colored materials, such as crude oils, it is
heating to complete melting, homogeneously suspended in the
impractical to observe, in the test jar, the onset of crystallization and
sample (Appendix X1). Inspect the walls of the original
network formation in the test specimen. Hence, it is presumed that
container to ensure that no high melting point material is left network formation will begin at the very early stages of the cooling
sequence.
sticking to the wall.
9.1.7 Pour points are expressed in temperatures which are
NOTE 10—It is not possible to define universal mandatory rules for the
positive or negative multiples of 3°C. Begin to examine the
preparation of crude oil test samples. Guidelines for sample handling for
the most common situations are given in Appendix X1.
appearance of the test specimen when the temperature of the
test specimen is 9°C above the expected pour point (estimated
9. Procedure
as a multiple of 3°C). At each test thermometer reading which
9.1 Procedure A for Maximum (Upper) Pour Point:
is a multiple of 3°C below the starting temperature, remove the
9.1.1 Pour the test sample into the test jar to the level mark.
test jar from the jacket. When necessary, remove moisture that
If necessary, reheat the test sample to a temperature at least
limits visibility of the test specimen by wiping the surface of
20°C above the expected pour point (8.2 and Appendix X1) but
the test jar with a clean cloth moistened in alcohol at
not higher than a temperature of 60°C (see Note 11).
approximately the temperature of the test specimen in the jar.
Then tilt the jar just enough to ascertain whether there is
NOTE 11—Warning: The vapor pressure of crude oils at temperatures
movement of the test specimen in the jar. When movement is
higher than 60°C will usually exceed 100 kPa. Under these circumstances
the sample container may rupture. Opening of the container may induce observed, immediately return the test jar into the jacket. The
foaming with resultant loss of sample and possible injury to personnel.
complete operation of removal and replacement shall require
not more than 3 s.
9.1.2 Immediately close the test jar with the cork carrying
9.1.7.1 If the test specimen has not ceased to flow when its
the high cloud and pour thermometer, or, if the expected pour
temperature has reached 30°C, transfer the test jar to the next
point is above 36°C, the melting point thermometer. Adjust the
lower temperature bath per the following schedule:
position of the cork and thermometer so the cork fits tightly, the
thermometer and the jar are coaxial, and the thermometer bulb (a) If the test specimen is at + 30°C, move to 0°C bath;
is immersed to a depth that places the beginning of the (b) If the test specimen is at + 9°C, move to − 18°C bath;
capillary 3 mm below the surface of the test specimen. (c) If the test specimen is at − 9°C, move to − 33°C bath; and
9.1.3 Keep the test jar with the test specimen at room (d) If the test specimen is at − 24°C, move to − 51°C bath.
temperature (between 18 and 24°C) for at least 24 h.
9.1.7.2 As soon as the test specimen in the jar does not flow
when tilted, hold the jar in a horizontal position for 5 s, as
NOTE 12—The pour point of a crude oil is dependent on the state of
shown by an accurate timing device (6.4) and observe care-
crystallization of the wax in the test specimen. In crude oils, achieving
fully. If the test specimen shows any movement, replace the
equilibrium between crystallized wax and dissolved wax is a rather slow
process. However, experience has shown that in a majority of cases, such test jar immediately in the jacket and repeat a test for flow at
an equilibrium is reached within 24 h.
the next temperature, 3°C lower.
9.1.4 If the expected pour point is greater than 36°C, heat 9.1.8 Continue in this manner until a point is reached at
which the test specimen shows no movement when the test jar
the sample to 9°C above the expected pour point. If the
expected pour point is less than 36°C, heat the sample to a is held in a horizontal position for 5 s. Record the observed
reading of the test temperature.
temperature of 45 6 1°C. Maintain the water bath (6.2) to heat
the sample at 48 6 1°C or at a temperature 12°C higher than 9.1.8.1 If the test specimen has r
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