This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D97 − 17b (Reapproved 2022)

Designation: 15/22

Standard Test Method for

Pour Point of Petroleum Products1,2
This standard is issued under the fixed designation D97; 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.
This standard has been approved for use by agencies of the U.S. Department of Defense.

1. Scope mercury or mercury-containing products, or both, is prohibited

1.1 This test method covers and is intended for use on any by local or national law. Users must determine legality of sales
petroleum product.3 A procedure suitable for black specimens, in their location.
cylinder stock, and nondistillate fuel oil is described in 8.8. The 1.6 This standard does not purport to address all of the
cloud point procedure formerly part of this test method now safety concerns, if any, associated with its use. It is the
appears as Test Method D2500. responsibility of the user of this standard to establish appro-
priate safety, health, and environmental practices and deter-
1.2 Currently there is no ASTM test method for automated
mine the applicability of regulatory limitations prior to use.
Test Method D97 pour point measurements.
1.7 This international standard was developed in accor-
1.3 Several ASTM test methods offering alternative proce- dance with internationally recognized principles on standard-
dures for determining pour points using automatic apparatus ization established in the Decision on Principles for the
are available. None of them share the same designation number Development of International Standards, Guides and Recom-
as Test Method D97. When an automatic instrument is used, mendations issued by the World Trade Organization Technical
the ASTM test method designation number specific to the Barriers to Trade (TBT) Committee.
technique shall be reported with the results. A procedure for
testing the pour point of crude oils is described in Test Method 2. Referenced Documents
D5853.
2.1 ASTM Standards:4
1.4 The values stated in SI units are to be regarded as D117 Guide for Sampling, Test Methods, and Specifications
standard. No other units of measurement are included in this for Electrical Insulating Liquids
standard. D396 Specification for Fuel Oils
1.5 WARNING—Mercury has been designated by many D2500 Test Method for Cloud Point of Petroleum Products
regulatory agencies as a hazardous substance that can cause and Liquid Fuels
serious medical issues. Mercury, or its vapor, has been dem- D5853 Test Method for Pour Point of Crude Oils
onstrated to be hazardous to health and corrosive to materials. D6300 Practice for Determination of Precision and Bias
Use caution when handling mercury and mercury-containing Data for Use in Test Methods for Petroleum Products,
products. See the applicable product Safety Data Sheet (SDS) Liquid Fuels, and Lubricants
for additional information. The potential exists that selling D7962 Practice for Determination of Minimum Immersion
Depth and Assessment of Temperature Sensor Measure-
ment Drift
1
This test method is under the jurisdiction of ASTM International Committee E1 Specification for ASTM Liquid-in-Glass Thermometers
D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct
responsibility of ASTM Subcommittee D02.07 on Flow Properties. The technically E644 Test Methods for Testing Industrial Resistance Ther-
equivalent standard as referenced is under the jurisdiction of the Energy Institute mometers
Subcommittee SC-C-4. E1137 Specification for Industrial Platinum Resistance Ther-
Current edition approved Nov. 1, 2022. Published November 2022. Originally
approved in 1927, replacing D47. Last previous edition approved in 2017 as
mometers
D97 – 17b. DOI: 10.1520/D0097-17BR22. E2877 Guide for Digital Contact Thermometers
This test method was adopted as a joint ASTM-IP Standard in 1965.
2
This test method has been developed through the cooperative effort between
ASTM and the Energy Institute, London. ASTM and IP standards were approved by
4
ASTM and EI technical committees as being technically equivalent but that does not For referenced ASTM standards, visit the ASTM website, www.astm.org, or
imply both standards are identical. contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
3
Statements defining this test and its significance when applied to electrical Standards volume information, refer to the standard’s Document Summary page on
insulating oils of mineral origin will be found in Guide D117. the ASTM website.

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 D97 − 17b (2022)
2.2 Energy Institute Standards:5 3.1.3.2 Discussion—PET is an acronym for portable elec-
Specifications for IP Standard Thermometers tronic thermometers, a subset of digital contact thermometers
(DCT).
3. Terminology 3.1.4 pour point, n—in petroleum products, the lowest
3.1 Definitions: temperature at which movement of the test specimen is
3.1.1 black oil, n—lubricant containing asphaltic materials. observed under prescribed conditions of test.
Black oils are used in heavy-duty equipment applications, such 3.1.5 residual fuel, n—a liquid fuel containing bottoms
as mining and quarrying, where extra adhesiveness is desired. remaining from crude distillation or thermal cracking; some-
3.1.2 cylinder stock, n—lubricant for independently lubri- times referred to as heavy fuel oil.
cated engine cylinders, such as those of steam engines and air 3.1.5.1 Discussion—Residual fuels comprise Grades 4, 5,
compressors. Cylinder stock are also used for lubrication of and 6 fuel oils, as defined in Specification D396.
valves and other elements in the cylinder area.
3.1.3 digital contact thermometer (DCT), n—an electronic 4. Summary of Test Method
device consisting of a digital display and associated tempera- 4.1 After preliminary heating, the sample is cooled at a
ture sensing probe. specified rate and examined at intervals of 3 °C for flow
3.1.3.1 Discussion—This device consists of a temperature characteristics. The lowest temperature at which movement of
sensor connected to a measuring instrument; this instrument the specimen is observed is recorded as the pour point.
measures the temperature-dependent quantity of the sensor,
computes the temperature from the measured quantity, and 5. Significance and Use
provides a digital output. This digital output goes to a digital
5.1 The pour point of a petroleum specimen is an index of
display and/or recording device that may be internal or external
the lowest temperature of its utility for certain applications.
to the device. These devices are sometimes referred to as
“digital thermometers.”
6. Apparatus
6.1 Test Jar, cylindrical, of clear glass, flat bottom, 33.2 mm
to 34.8 mm outside diameter, and 115 mm to 125 mm in
5
height. The inside diameter of the jar can range from 30.0 mm
Available from Energy Institute, 61 New Cavendish St., London, W1G 7AR,
U.K., http://www.energyinst.org.

NOTE 1—Dimensions are in millimetres (not to scale).

FIG. 1 Apparatus for Pour Point Test

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 D97 − 17b (2022)
to 32.4 mm, within the constraint that the wall thickness be no may be necessary to use a 1000 Ω sensor in order to obtain accurate
greater than 1.6 mm. The jar shall have a line to indicate a measurements.
NOTE 2—When the DCT display is mounted on the end to the probe’s
sample height 54 mm 6 3 mm above the inside bottom. See sheath, the test jar with the probe inserted will be unstable. To resolve this,
Fig. 1. it is recommended that the probe be less than 30 cm in length but no less
6.2 Temperature Measuring Device—Either liquid-in-glass than 15 cm. A 5 cm long stopper, that has a low thermal conductivity, with
approximately half of it inserted in the sample tube will improve stability.
thermometer as described in 6.2.1 or Digital Contact Ther-
mometer (DCT) meeting the requirements described in 6.2.2.6 6.2.2.1 The DCT calibration drift shall be checked at least
6.2.1 Liquid-in-Glass Thermometers, having the following annually by either measuring the ice point or against a
ranges and conforming to the requirements prescribed in reference thermometer in a constant temperature bath at the
Specification E1 or Specifications for IP Standard Thermom- prescribed immersion depth to ensure compliance with 6.2.2.
eters: See Practice D7962.
Temperature Thermometer NOTE 3—When a DCT’s calibration drifts in one direction over several
Number calibration checks, that is, ice point, it may be an indication of deteriora-
Thermometer Range ASTM IP tion of the DCT.
High cloud and pour −38 °C to +50 °C 5C 1C
Low cloud and pour −80 °C to +20 °C 6C 2C 6.3 Cork, to fit the test jar, bored centrally for the test
Melting point +32 °C to +127 °C 61C 63C temperature measuring device.
6.2.1.1 Since separation of liquid column thermometers
6.4 Jacket, watertight, cylindrical, metal, flat-bottomed,
occasionally occurs and may escape detection, thermometers
115 mm 6 3 mm depth, with inside diameter of 44.2 mm to
should be checked immediately prior to the test and used only
45.8 mm. It shall be supported in a vertical position in the
if they prove accurate within 61 °C (for example ice point).
cooling bath (see 6.7) so that not more than 25 mm projects out
6.2.2 Digital Contact Thermometer Requirements:
of the cooling medium, and shall be capable of being cleaned.
Parameter Requirement
DCT Guide E2877 Class F or better 6.5 Disk, cork or felt, 6 mm thick to fit loosely inside the
jacket.
Nominal temperature rangeA High Pour: –38 °C to 50 °C
Low Pour: –80 °C to 20 °C 6.6 Gasket Ring Form, about 5 mm in thickness, to fit
Melt Point: 32 °C to 127 °C snugly around the outside of the test jar and loosely inside the
Display resolution 0.1 °C minimum
AccuracyB ±500 mK (±0.5 °C) jacket. The gasket may be made of rubber, leather, or other
Sensor type Platinum resistance thermometer (PRT), material that is elastic enough to cling to the test jar and hard
thermistor, thermocouple enough to hold its shape. Its purpose is to prevent the test jar
Sensor sheathC 4.2 mm OD maximum
Sensor lengthD Less than 10 mm from touching the jacket.
Immersion depthE Less than 40 mm per Practice D7962
Sample immersion depth Tip of sheath between 10 mm and 15 mm
6.7 Bath or Baths, maintained at prescribed temperatures
below sample meniscus with a firm support to hold the jacket vertical. The required
Fig. 1 bath temperatures may be obtained by refrigeration if
Measurement driftE Less than 500 mK (0.5 °C) per year
Response timeF Less than or equal to 4 s per footnote F
available, otherwise by suitable cooling mixtures. Cooling
Calibration error Less than 500 mK (0.5 °C) over the range of mixtures commonly used for bath temperatures down to those
intended use shown are in Table 1.
Calibration range Consistent with temperature range of use
Calibration data Four data points evenly distributed over the cali-
bration range that is consistent with the range of 7. Reagents and Materials
use. The calibration data is to be included in the
calibration report.
7.1 The following solvents of technical grade are appropri-
Calibration report From a calibration laboratory with demonstrated ate for low-temperature bath media.
competency in temperature calibration which is 7.1.1 Acetone, (Warning—Extremely flammable).
traceable to a national calibration laboratory or
metrology standards body
7.1.2 Alcohol, Ethanol (Warning—Flammable).
7.1.3 Alcohol, Methanol (Warning—Flammable. Vapor
A
The nominal temperature range may be different from the values shown provided harmful).
the calibration and accuracy criteria are met.
B
7.1.4 Petroleum Naphtha, (Warning—Combustible. Vapor
Accuracy is the combined accuracy of the DCT unit, which is the display and
sensor.
harmful).
C
Sensor sheath is the tube that holds the sensing element. The value is the 7.1.5 Solid Carbon Dioxide, (Warning—Extremely cold
outside diameter of the sheath segment containing the sensor element.
D
−78.5 °C).
The physical length of the temperature sensing element.
E
As determined by Practice D7962 or an equivalent procedure.
F
Response Time—The time for a DCT to respond to a step change in tempera- 8. Procedure
ture. The response time is 63.2 % of the step change time as determined per
Section 9 of Test Methods E644. The step change evaluation begins at 20 °C ±
8.1 Pour the specimen into the test jar to the level mark.
5 °C air to 77 °C ± 5 °C with water circulating at 0.9 m ⁄s ± 0.09 m ⁄s past the When necessary, heat the specimen in a bath until it is just
sensor. sufficiently fluid to pour into the test jar.
NOTE 1—When making measurements below –40 °C with a PRT, it NOTE 4—It is known that some materials, when heated to a temperature
higher than 45 °C during the preceding 24 h, do not yield the same pour
6
Supporting data have been filed at ASTM International Headquarters and may point results as when they are kept at room temperature for 24 h prior to
be obtained by requesting Research Report RR:D02-1826. Contact ASTM Customer testing. Examples of materials which are known to show sensitivity to
Service at [email protected]. thermal history are residual fuels, black oils, and cylinder stocks.

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 D97 − 17b (2022)
TABLE 1 Cooling Mixtures and Bath Temperatures
Cooling Mixture Bath
Temperature
Ice and water 0 °C ± 1.5 °C

Crushed ice and sodium chloride crystals or –18 °C ± 1.5 °C

Acetone or petroleum naphtha, or methanol or ethanol (see
Section 7) with solid carbon dioxide added to give the desired
temperature

Acetone or petroleum naphtha or methanol or ethanol (see –33 °C ± 1.5 °C

Section 7) with solid carbon dioxide added to give the desired
temperature

Acetone or petroleum naphtha or methanol or ethanol (see –51 °C ± 1.5 °C

Section 7) with solid carbon dioxide added to give the desired
temperature

Acetone or petroleum naphtha or methanol or ethanol (see –69 °C ± 1.5 °C

Section 7) with solid carbon dioxide added to give the desired
temperature

8.1.1 Samples of residual fuels, black oils, and cylinder 8.3.2 Specimens Having Pour Points of −33 °C and
stocks which have been heated to a temperature higher than Below—Heat the specimen without stirring to at least 45 °C in
45 °C during the preceding 24 h, or when the thermal history of a bath maintained at 48 °C 6 1.5 °C. Transfer the test jar to a
these sample types is not known, shall be kept at room bath maintained at 24 °C 6 1.5 °C. When using a liquid bath,
temperature for 24 h before testing. Samples which are known ensure that the liquid level is between the fill mark on the test
by the operator not to be sensitive to thermal history need not jar and the top of the test jar. When the specimen temperature
be kept at room temperature for 24 h before testing. reaches 27 °C, and if using liquid-in-glass thermometers,
8.1.2 Experimental evidence supporting elimination of the remove the high cloud and pour thermometer, and place the
24 h waiting period for some sample types is contained in a low cloud and pour thermometer in position. Transfer the test
research report.7 jar to the cooling bath (see 8.6.1).
8.2 In the case of pour points above 36 °C, use a higher 8.4 See that the disk, gasket, and the inside of the jacket are
range temperature measuring device (6.2) such as IP 63C or clean and dry. Place the disk in the bottom of the jacket. Place
ASTM 61C, or a digital contact thermometer. Close the test jar the gasket around the test jar, 25 mm from the bottom. Insert
with the cork carrying the test temperature measuring device the test jar in the jacket. Never place a jar directly into the
(6.2). Adjust the position of the cork and temperature measur- cooling medium.
ing device so the cork fits tightly, the temperature measuring
8.5 After the specimen has cooled to allow the formation of
device and the jar are coaxial, and the temperature measuring
paraffin wax crystals, take great care not to disturb the mass of
device is immersed to the correct depth.
specimen nor permit the thermometer to shift in the specimen;
8.2.1 For liquid-in-glass, the thermometer bulb should be
any disturbance of the spongy network of wax crystals will
immersed so the beginning of the capillary is 3 mm below the
lead to low and erroneous results.
surface of the specimen.
8.2.2 For digital contact thermometers, the probe should be 8.6 Pour points are expressed in integers that are positive or
immersed so the end of the probe is 10 mm to 15 mm below the negative multiples of 3 °C. Begin to examine the appearance of
surface of the specimen. the specimen when the temperature of the specimen is 9 °C
8.3 For the measurement of pour point, subject the speci- above the expected pour point (estimated as a multiple of
men in the test jar to the following preliminary treatment: 3 °C). At each test temperature that is a multiple of 3 °C below
8.3.1 Specimens Having Pour Points Above −33 °C—Heat the starting temperature remove the test jar from the jacket. To
the specimen without stirring to 9 °C above the expected pour remove condensed moisture that limits visibility wipe the
point, but to at least 45 °C, in a bath maintained at 12 °C above surface with a clean cloth moistened in alcohol (ethanol or
the expected pour point, but at least 48 °C. Transfer the test jar methanol). Tilt the jar just enough to ascertain whether there is
to a bath maintained at 24 °C 6 1.5 °C and commence a movement of the specimen in the test jar. If movement of
observations for pour point. When using a liquid bath, ensure specimen in the test jar is noted, then replace the test jar
that the liquid level is between the fill mark on the test jar and immediately in the jacket and repeat a test for flow at the next
the top of the test jar. temperature, 3 °C lower. Typically, the complete operation of
removal, wiping, and replacement shall require not more than
3 s.
7
8.6.1 If the specimen has not ceased to flow when its
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1377. Contact ASTM Customer temperature has reached 27 °C, transfer the test jar to a jacket
Service at [email protected]. in a cooling bath maintained at 0 °C 6 1.5 °C. As the specimen

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 D97 − 17b (2022)
continues to get colder, transfer the test jar to a jacket in the 10.1.1 Lubricating Oil: 8
next lower temperature cooling bath in accordance with Table 10.1.1.1 Repeatability—The difference between successive
2. test results, obtained by the same operator using the same
8.6.2 If the specimen in the jar does not show movement apparatus under constant operating conditions on identical test
when tilted, hold the jar in a horizontal position for 5 s, as material would, in the long run, in the normal and correct
noted by an accurate timing device, and observe the specimen operation of this test method, exceed 6 °C only in one case in
carefully. If the specimen shows any signs of movement before twenty. Differences greater than this should be considered
5 s has passed, replace the test jar immediately in the jacket and suspect.
repeat a test for flow at the next temperature, 3 °C lower. 10.1.1.2 Reproducibility—The difference between two
single and independent test results, obtained by different
8.7 Continue in this manner until a point is reached at which operators working in different laboratories on identical test
the specimen shows no movement when the test jar is held in material would, in the long run, in the normal and correct
a horizontal position for 5 s. Record the observed reading of operation of this test method, exceed 9 °C only in one case in
the test thermometer. twenty. Differences greater than this should be considered
8.8 For black specimen, cylinder stock, and residual fuel suspect.
specimen, the result obtained by the procedure described in 8.1 10.1.1.3 The precision statements8 were derived from a
through 8.7 is the upper (maximum) pour point. If required, 1998 interlaboratory test program using Practice D6300. Par-
determine the lower (minimum) pour point by heating the ticipants analyzed five sets of duplicate base oils, three sets of
sample while stirring, to 105 °C, pouring it into the jar, and duplicate multigrade lubricating oils, and one set each of
determining the pour point as described in 8.4 through 8.7. duplicate hydraulic oils and automatic transmission fluid in the
temperature range of –51 °C to –11 °C. Seven laboratories
8.9 Some specifications allow for a pass/fail test or have participated with the manual Test Method D97. Information on
pour point limits at temperatures not divisible by 3 °C. In these the type of samples and their average pour points are in
cases, it is acceptable practice to conduct the pour point Research Report RR:D02-1499.8
measurement according to the following schedule: Begin to
NOTE 6—The precision statements are the derived values rounded up to
examine the appearance of the specimen when the temperature
the next testing interval value. The actual derived precision values appear
of the specimen is 9 °C above the specification pour point. in Table X1.1.
Continue observations at 3 °C intervals as described in 8.6 and
10.1.2 Middle Distillate and Residual Fuel: 9
8.7 until the specification temperature is reached. Report the
10.1.2.1 Repeatability—The difference between successive
sample as passing or failing the specification limit.
test results obtained by the same operator using the same
apparatus under constant operation conditions on identical test
9. Calculation and Report
material would, in the long run, in the normal and correct
9.1 Add 3 °C to the temperature recorded in 8.7 and report operation of this test method, exceed 3 °C only in one case in
the result as the Pour Point, ASTM D97. For black oil, and so twenty. Differences greater than this should be considered
forth, add 3 °C to the temperature recorded in 8.7 and report suspect.
the result as Upper Pour Point, ASTM D97, or Lower Pour 10.1.2.2 Reproducibility—The difference between two
Point, ASTM D97, as required. single and independent test results, obtained by different
operators working in different laboratories on identical test
10. Precision and Bias material would, in the long run, in the normal and correct
operation of this test method, exceed 9 °C only in one case in
10.1 Precision—The precision of this test method as deter- twenty. Differences greater than this should be considered
mined by the statistical examination of the interlaboratory test suspect.
results is as follows: 10.1.2.3 The precision statements9 were prepared with data
NOTE 5—The precision statements were developed using liquid-in-glass on sixteen middle distillate and residual fuels tested by twelve
thermometers corresponding to those in Specification E1 or IP Specifica- cooperators. The fuels had pour points ranging from −33 °C to
tions for IP Standard Thermometers. +51 °C.
NOTE 7—The precision statements are the derived values rounded up to
the next testing interval value. The actual derived precision values can be
seen in Table X1.1.
NOTE 8—The precisions in 10.1.2 are not known to have been derived
TABLE 2 Bath and Sample Temperature Ranges using Practice D6300.
Bath Temperature Sample Temperature
Setting, °C Range, °C
10.2 Bias—There being no criteria for measuring bias in
48 ± 1.5 or 12 above Preheat to at least 45 or 9 these test-product combinations, no statement of bias can be
expected pour point above expected pour point made.
24 ± 1.5 Start to 27
0 ± 1.5 27 to 9
8
–18 ± 1.5 9 to –6 Supporting data (the results of the 1998 interlaboratory cooperative test
–33 ± 1.5 –6 to –24 program) have been filed at ASTM International Headquarters and may be obtained
–51 ± 1.5 –24 to –42 by requesting Research Report RR:D02-1499. Contact ASTM Customer Service at
–69 ± 1.5 –42 to –60 [email protected].
9
Based on the results of the 1983 interlaboratory cooperative test program.

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 D97 − 17b (2022)
11. Keywords
11.1 petroleum products; pour point

APPENDIXES

(Nonmandatory Information)

X1. ACTUAL DERIVED PRECISION VALUES

X1.1 See Table X1.1.

TABLE X1.1 Actual Derived Precision Values

95 % Confidence 1998 Research Program 1983 Research Program
Lubricating Oil, °C Middle Distillate and
Residual Fuels, °C
Repeatability 5.3 2.5
Reproducibility 8.0 6.6

X2. THERMOMETER SPECIFICATIONS

X2.1 See Table X2.1.

TABLE X2.1 Thermometer Specifications

Low cloud and pour High cloud and pour Melting point
Range °C –80 to +20 –38 to +50 32 to 127
Immersion mm 76 108 79
Graduation at each °C 1 1 0.2
Longer lines at each °C 5 5 1
Figured at each °C 10 10 2
Scale error, max °C 1 down to –33 0.5 0.2
2 below –33
Expansion chamber to permit heating to °C 60 100 150
Overall length mm 230 ± 5 230 ± 5 380 ± 5
Stem diameter mm 6 to 8 6 to 8 6 to 8
Bulb length mm 7.0 to 10 7.0 to 10 18 to 28
Bulb diameter mm 5.0 to stem 5.5 to stem 5.0 to 6.0
Distance from bottom of bulb to line at °C –70 –38 32
mm 100 to 120 120 to 130 105 to 115
Length of scale/range mm 70 to 100 65 to 85 200 to 240

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 D97 − 17b (2022)

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