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An American National Standard

Designation: D 97 – 02

Designation: 15/95

Standard Test Method for

Pour Point of Petroleum Products1
This standard is issued under the fixed designation D 97; 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.

This test method has been adopted for use by government agencies to replace Method 201 of Federal Test Methods Standard No. 791b,
and Method 4452 of Federal Test Method Standard No. 141A.

This test method was adopted as a joint ASTM-IP Standard in 1965.

1. Scope E 1 Specification for ASTM Thermometers7

1.1 This test method is intended for use on any petroleum E 77 Test Method for Inspection and Verification of Ther-
product.2 A procedure suitable for black specimens, cylinder mometers7
stock, and nondistillate fuel oil is described in 8.8. A procedure 2.2 IP Standards:
for testing the fluidity of a residual fuel oil at a specified Specifications for IP Standard Thermometers8
temperature is described in the appendix. 3. Terminology

iTeh Standards
1.2 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 3.1 Definitions:
responsibility of the user of this standard to establish appro- 3.1.1 black oil, n—lubricant containing asphaltic materials.

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priate safety and health practices and determine the applica-
bility of regulatory limitations prior to use. For specific hazard
Black oils are used in heavy-duty equipment applications, such
as mining and quarrying, where extra adhesiveness is desired.
3.1.2 cylinder stock, n—lubricant for independently lubri-
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statements, see Section 7.
cated engine cylinders, such as those of steam engines and air
2. Referenced Documents compressors. Cylinder stock are also used for lubrication of
2.1 ASTM Standards: valves and other elements in the cylinder area.
D 117 Guide for Sampling, Test Methods, Specifications, ASTM D97-023.1.3 pour point, n—in petroleum products, the lowest
temperature at which movement of the test specimen is
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Guide for Electrical Insulating Oils of Petroleum
Origin 3 observed under prescribed conditions of test.
D 396 Specification for Fuel Oils 4 3.1.4 residual fuel, n—a liquid fuel containing bottoms
D 1659 Test Method for Maximum Fluidity Temperature of remaining from crude distillation or thermal cracking; some-
Residual Fuel Oil5 times referred to as heavy fuel oil.
D 2500 Test Method for Cloud Point of Petroleum Oils4 3.1.4.1 Discussion—Residual fuels comprise Grades 4, 5,
D 3245 Test Method for Pumpability of Industrial Fuel and 6 fuel oils, as defined in Specification D 396.
6
Oils
4. Summary of Test Method
4.1 After preliminary heating, the sample is cooled at a
specified rate and examined at intervals of 3°C for flow
1
This test method is under the jurisdiction of ASTM Committee D02 on characteristics. The lowest temperature at which movement of
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee the specimen is observed is recorded as the pour point.
D02.07 on Flow Properties.
Current edition approved March 10, 2002. Published May 2002. Originally
published as D 97 – 27. In 1927, revised and replaced former D 47. Last previous
5. Significance and Use
edition D 97 – 96a. 5.1 The pour point of a petroleum specimen is an index of
In the IP, this test method is under the jurisdiction of the Standardization the lowest temperature of its utility for certain applications.
Committee.
2
Statements defining this test and its significance when applied to electrical
insulating oils of mineral origin will be found in Guide D 117.
3
Annual Book of ASTM Standards, Vol 10.03.
4 7
Annual Book of ASTM Standards, Vol 05.01. Annual Book of ASTM Standards, Vol 14.03.
5 8
Discontinued; see 1984 Annual Book of ASTM Standards, Vol 05.01. Methods for Analysis and Testing, IP Standards for Petroleum and its Products,
6
Annual Book of ASTM Standards, Vol 05.02 Part I, Vol 2.

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

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 D 97
6. Apparatus 6.5 Disk, cork or felt, 6 mm thick to fit loosely inside the
6.1 Test Jar, cylindrical, of clear glass, flat bottom, 33.2 to jacket.
34.8-mm outside diameter, and 115 to 125 mm in height. The 6.6 Gasket, to fit snugly around the outside of the test jar
inside diameter of the jar can range from 30.0 to 32.4 mm, and loosely inside the jacket. The gasket may be made of
within the constraint that the wall thickness be no greater than rubber, leather, or other material that is elastic enough to cling
1.6 mm. The jar shall have a line to indicate a sample height 54 to the test jar and hard enough to hold its shape. Its purpose is
6 3 mm above the inside bottom. See Fig. 1. to prevent the test jar from touching the jacket.
6.2 Thermometers, having the following ranges and con- 6.7 Bath or Baths, maintained at prescribed temperatures
forming to the requirements prescribed in Specification E 1 for with a firm support to hold the jacket vertical. The required
thermometers: bath temperatures may be obtained by refrigeration if avail-
Thermometer
able, otherwise by suitable freezing mixtures. Freezing mix-
Temperature Number tures commonly used for temperatures down to those shown
Thermometer Range ASTM IP are as follows:
High cloud and pour −38 to + 50°C 5C 1C For Tempera-
Low cloud and pour −80 to + 20°C 6C 2C tures Down
Melting point + 32 to + 127°C 61C 63C
Ice and water 9°C
6.2.1 Since separation of liquid column thermometers occa- Crushed ice and sodium chloride crystals −12°C
Crushed ice and calcium chloride crystals −27°C
sionally occurs and may escape detection, thermometers Acetone or petroleum naphtha (see Section 6) chilled in a −57°C
should be checked immediately prior to the test and used only covered metal beaker with an ice-salt mixture to − 12°C then
if they prove accurate within6 1°C (for example ice point). with enough solid carbon dioxide to give the desired
temperature.
6.3 Cork, to fit the test jar, bored centrally for the test
thermometer. NOTE 1—There are automatic pour point testers available and in use
6.4 Jacket, watertight, cylindrical, metal, flat-bottomed, 115 which may be advantageous in the saving of test time, permit the use of
smaller samples, and have other factors which may merit their use. If
6 3-mm depth, with inside diameter of 44.2 to 45.8 mm. It automatic testers are used, the user must ensure that all of the manufac-

iTeh Standards
shall be supported in a vertical position in the cooling bath (see
6.7) so that not more than 25 mm projects out of the cooling
medium, and shall be capable of being cleaned.
turer’s instructions for calibration, adjustment, and operation of the
instrument are followed. It must be reported that the pour point was
determined by an automatic instrument. In any case of dispute, the pour
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ASTM D97-02
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NOTE 1—Dimensions are in millimetres (not to scale).

FIG. 1 Apparatus for Pour Point Test

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 D 97
point as determined by the manual method described herein shall be the gasket around the test jar, 25 mm from the bottom. Insert
considered the reference test. the test jar in the jacket. Never place a jar directly into the
cooling medium.
7. Reagents and Materials
8.5 After the specimen has cooled to allow the formation of
7.1 The following solvents of technical grade are appropri- paraffin wax crystals, take great care not to disturb the mass of
ate for low-temperature bath media. specimen nor permit the thermometer to shift in the specimen;
7.1.1 Acetone, (Warning—Extremely flammable). any disturbance of the spongy network of wax crystals will
7.1.2 Alcohol, Ethanol (Warning—Flammable). lead to low and erroneous results.
7.1.3 Alcohol, Methanol (Warning—Flammable. Vapor 8.6 Pour points are expressed in integers that are positive or
harmful). negative multiples of 3°C. Begin to examine the appearance of
7.1.4 Petroleum Naphtha, (Warning—Combustible. Vapor the specimen when the temperature of the specimen is 9°C
harmful). above the expected pour point (estimated as a multiple of 3°C).
7.1.5 Solid Carbon Dioxide, (Warning—Extremely At each test thermometer reading that is a multiple of 3°C
cold − 78.5°C). below the starting temperature remove the test jar from the
jacket. To remove condensed moisture that limits visibility
8. Procedure
wipe the surface with a clean cloth moistened in alcohol
8.1 Pour the specimen into the test jar to the level mark. (ethanol or methanol). Tilt the jar just enough to ascertain
When necessary, heat the specimen in a water bath until it is whether there is a movement of the specimen in the test jar. The
just sufficiently fluid to pour into the test jar. complete operation of removal, wiping, and replacement shall
NOTE 2—It is known that some materials, when heated to a temperature require not more than 3 s.
higher than 45°C during the preceding 24 h, do not yield the same pour 8.6.1 If the specimen has not ceased to flow when its
point results as when they are kept at room temperature for 24 h prior to temperature has reached 27°C, transfer the test jar to the next
testing. Examples of materials which are known to show sensitivity to lower temperature bath in accordance with the following
thermal history are residual fuels, black oils, and cylinder stocks. schedule:

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8.1.1 Samples of residual fuels, black oils, and cylinder Specimen is at 1 27°C, move to 0°C bath,
stocks which have been heated to a temperature higher than Specimen is at 1 9°C, move to 2 18°C bath,
45°C during the preceding 24 h, or when the thermal history of Specimen is at 2 6°C, move to 2 33°C bath,

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these sample types is not known, shall be kept at room
temperature for 24 h before testing. Samples which are known
Specimen is at 2 24°C, move to 2 51°C bath,
Specimen is at 2 42°C, move to 2 69°C bath. (1)

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by the operator not to be sensitive to thermal history need not 8.6.2 As soon as the specimen in the jar does not flow when
be kept at room temperature for 24 h before testing. tilted, hold the jar in a horizontal position for 5 s, as noted by
8.1.2 Experimental evidence supporting elimination of the an accurate timing device and observe carefully. If the speci-
24-h waiting period for some sample types is contained in a men shows any movement, replace the test jar immediately in
research report.9 ASTM D97-02
the jacket and repeat a test for flow at the next temperature, 3°C
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8.2 Close the test jar with the cork carrying the high-pour lower.
thermometer (5.2). In the case of pour points above 36°C, use 8.7 Continue in this manner until a point is reached at which
a higher range thermometer such as IP 3C or ASTM 61C. the specimen shows no movement when the test jar is held in
Adjust the position of the cork and thermometer so the cork fits a horizontal position for 5 s. Record the observed reading of
tightly, the thermometer and the jar are coaxial, and the the test thermometer.
thermometer bulb is immersed so the beginning of the capillary 8.8 For black specimen, cylinder stock, and nondistillate
is 3 mm below the surface of the specimen. fuel specimen, the result obtained by the procedure described
8.3 For the measurement of pour point, subject the speci- in 8.1 through 8.7 is the upper (maximum) pour point. If
men in the test jar to the following preliminary treatment: required, determine the lower (minimum) pour point by heat-
8.3.1 Specimens Having Pour Points Above − 33°C—Heat ing the sample while stirring, to 105°C, pouring it into the jar,
the specimen without stirring to 9°C above the expected pour and determining the pour point as described in 8.4 through 8.7.
point, but to at least 45°C, in a bath maintained at 12°C above 8.9 Some specifications allow for a pass/fail test or have
the expected pour point, but at least 48°C. Transfer the test jar pour point limits at temperatures not divisible by 3°C. In these
to a water bath maintained at 24°C and commence observa- cases, it is acceptable practice to conduct the pour point
tions for pour point. measurement according to the following schedule: Begin to
8.3.2 Specimens Having Pour Points of − 33°C and examine the appearance of the specimen when the temperature
Below—Heat the specimen without stirring to 45°C in a bath of the specimen is 9°C above the specification pour point.
maintained at 48°C and cool to 15°C in a water bath main- Continue observations at 3°C intervals as described in 8.6 and
tained at 6°C. Remove the high cloud and pour thermometer, 8.7 until the specification temperature is reached. Report the
and place the low cloud and pour thermometer in position. sample as passing or failing the specification limit.
8.4 See that the disk, gasket, and the inside of the jacket are
clean and dry. Place the disk in the bottom of the jacket. Place 9. Calculation and Report
9.1 Add 3°C to the temperature recorded in 8.7 and report
the result as the Pour Point, ASTM D 97. For black oil, and so
9
Available from ASTM International Headquarters. Request RR:D02-1377. forth, add 3°C to the temperature recorded in 8.7 and report the

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 D 97
result as Upper Pour Point, ASTM D 97, or Lower Pour Point, working in different laboratories on identical test material,
ASTM D 97, as required. would in the long run, in the normal and correct operation of
this test method, exceed 6°C only in one case in twenty.
10. Precision and Bias
Differences greater than this should be considered suspect.
10.1 Lubricating Oil and Distillate and Residual Fuel Oil. 10.2 Bias—There being no criteria for measuring bias in
10
these test-product combinations, no statement of bias can be
10.1.1 Repeatability—The difference between successive made.
test results, obtained by the same operator using the same
apparatus under constant operating conditions on identical test 10.3 The precision statements were prepared with data on
material, would in the long run, in the normal and correct ten new (unused) mineral oil-based lubricants and sixteen
operation of this test method, exceed 3°C only in one case in assorted fuel oils tested by twelve cooperators. The mineral
twenty. Differences greater than this should be considered oil-based lubricants had pour points ranging from − 48
suspect. to − 6°C while the fuel oils had pour points ranging from − 33
10.1.2 Reproducibility—The difference between two single to + 51°C. The following precision data were obtained:
and independent test results, obtained by different operators Mineral Oil
Lubricants Fuel Oils
95 % Confidence
10
Repeatability,° C 2.87 2.52
The cloud point procedure formerly part of this test method now appears as Reproducibility, °C 6.43 6.59
Test Method D 2500.

APPENDIX

(Nonmandatory Information)

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X1. TEST FOR FLUIDITY OF A RESIDUAL FUEL OIL AT A SPECIFIED TEMPERATURE

X1.1 General (https://standards.iteh.ai)

X1.1.1 The low-temperature flow properties of a waxy fuel
X1.2 Scope
X1.2.1 This method covers the determination of the fluidity
Documentreceived
oil depend on handling and storage conditions. Thus, they may
not be truly indicated by pour point. The pour point test does
Preview
of a residual fuel oil at a specified temperature in an as-
condition.
not indicate what happens when an oil has a considerable head
of pressure behind it, such as when gravitating from a storage X1.3 Definition
ASTM D97-02
tank or being pumped along a pipeline. Failure to flow at the X1.3.1 fluidity temperature—the sample when tested in an
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pour point is normally attributed to the separation of wax from as-received condition is considered “fluid at the temperature of
the fuel; however, it can also be due to the effect of viscosity the test” if it will flow 2 mm in 1 min in a 12.5 mm U-tube
in the case of very viscous fuel oils. In addition pour points of under a maximum pressure of 152 mm of mercury.
residual fuels are influenced by the previous thermal history of
the specimens. A loosely knit wax structure built up on cooling X1.4 Summary of Test Method
of the oil can be normally broken by the application of X1.4.1 A sample of fuel in its as-received condition is
relatively little pressure. cooled at the specified temperature for 30 min in the standard
X1.1.2 The usefulness of the pour point test in relation to U-tube and is tested for movement under prescribed pressure
residual fuel oils is open to question, and the tendency to conditions.
regard the pour point as the limiting temperature at which a
fuel will flow can be misleading. The problem of accurately X1.5 Significance and Use
specifying the handling behavior of fuel oil is important, and X1.5.1 This method may be used as a “go-no-go” procedure
because of the technical limitations of the pour point test, for operational situations where it is necessary to ascertain the
various pumpability tests have been devised to assess the fluidity of a residual oil under prescribed conditions in an
low-temperature flow characteristics of heavy residual fuel as-received condition. The conditions of this method simulate
oils. Test Method D 3245 is one such method. However, most those of a pumping situation where the oil is expected to flow
alternative methods tend to be time-consuming and as such do through a 12-mm pipe under slight pressure at a specified
not find ready acceptance as routine control tests for determin- temperature. Fluidity, like Test Method D 97, is used to define
ing low-temperature flow properties. One method which is cold flow properties. It differs from D 97, however, in that (a)
relatively quick and easy to perform and has found limited it is restricted to residual fuel oil and (b) a prescribed pressure
acceptance as a“ go-no-go” method is based on the appendix is applied to the sample. The latter represents an attempt to
method to the former Test Method D 1659 – 65. The method is overcome the technical limitations of the Pour Point Method
described as follows. where gravity-induced flow is the criterion. Test Method