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 − 17

Designation: 15/95

Standard Test Method for

Pour Point of Petroleum Products1
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* 1.6 This standard does not purport to address all of the
1.1 This test method covers and is intended for use on any safety concerns, if any, associated with its use. It is the
petroleum product.2 A procedure suitable for black specimens, responsibility of the user of this standard to establish appro-
cylinder stock, and nondistillate fuel oil is described in 8.8. The priate safety and health practices and determine the applica-
cloud point procedure formerly part of this test method now bility of regulatory limitations prior to use.
appears as Test Method D2500.
2. Referenced Documents
1.2 Currently there is no ASTM test method for automated
2.1 ASTM Standards:3
Test Method D97 pour point measurements.
D117 Guide for Sampling, Test Methods, and Specifications
1.3 Several ASTM test methods offering alternative proce- for Electrical Insulating Oils of Petroleum Origin
dures for determining pour points using automatic apparatus D396 Specification for Fuel Oils
are available. None of them share the same designation number D2500 Test Method for Cloud Point of Petroleum Products
as Test Method D97. When an automatic instrument is used, and Liquid Fuels
the ASTM test method designation number specific to the D5853 Test Method for Pour Point of Crude Oils
technique shall be reported with the results. A procedure for D6300 Practice for Determination of Precision and Bias
testing the pour point of crude oils is described in Test Method Data for Use in Test Methods for Petroleum Products and
D5853. Lubricants
1.4 The values stated in SI units are to be regarded as D7962 Practice for Determination of Minimum Immersion
standard. No other units of measurement are included in this Depth and Assessment of Temperature Sensor Measure-
standard. ment Drift
E1 Specification for ASTM Liquid-in-Glass Thermometers
1.5 WARNING—Mercury has been designated by many
E644 Test Methods for Testing Industrial Resistance Ther-
regulatory agencies as a hazardous material that can cause
mometers
central nervous system, kidney and liver damage. Mercury, or
E1137 Specification for Industrial Platinum Resistance Ther-
its vapor, may be hazardous to health and corrosive to
mometers
materials. Caution should be taken when handling mercury and
E2877 Guide for Digital Contact Thermometers
mercury containing products. See the applicable product Ma-
terial Safety Data Sheet (MSDS) for details and EPA’s 2.2 Energy Institute Standards:4
website—http://www.epa.gov/mercury/faq.htm—for addi- Specifications for IP Standard Thermometers
tional information. Users should be aware that selling mercury
3. Terminology
and/or mercury containing products into your state or country
may be prohibited by law. 3.1 Definitions:
3.1.1 black oil, n—lubricant containing asphaltic materials.
Black oils are used in heavy-duty equipment applications, such
1
This test method is under the jurisdiction of ASTM Committee D02 on as mining and quarrying, where extra adhesiveness is desired.
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
Subcommittee D02.07 on Flow Properties.
Current edition approved Jan. 1, 2017. Published January 2017. Originally
3
approved in 1927, replacing D47. Last previous edition approved in 2016 as For referenced ASTM standards, visit the ASTM website, www.astm.org, or
D97 – 16. DOI: 10.1520/D0097-17. contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
In the IP, this test method is under the jurisdiction of the Standardization Standards volume information, refer to the standard’s Document Summary page on
Committee. This test method was adopted as a joint ASTM-IP Standard in 1965. the ASTM website.
2 4
Statements defining this test and its significance when applied to electrical Available from Energy Institute, 61 New Cavendish St., London, W1G 7AR,
insulating oils of mineral origin will be found in Guide D117. U.K., http://www.energyinst.org.

*A Summary of Changes section appears at the end of this standard

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 D97 − 17
3.1.2 cylinder stock, n—lubricant for independently lubri- 4. Summary of Test Method
cated engine cylinders, such as those of steam engines and air 4.1 After preliminary heating, the sample is cooled at a
compressors. Cylinder stock are also used for lubrication of specified rate and examined at intervals of 3 °C for flow
valves and other elements in the cylinder area. characteristics. The lowest temperature at which movement of
3.1.3 digital contact thermometer (DCT), n—an electronic the specimen is observed is recorded as the pour point.
device consisting of a digital display and associated tempera-
ture sensing probe. 5. Significance and Use
3.1.3.1 Discussion—This device consists of a temperature 5.1 The pour point of a petroleum specimen is an index of
sensor connected to a measuring instrument; this instrument the lowest temperature of its utility for certain applications.
measures the temperature-dependent quantity of the sensor,
computes the temperature from the measured quantity, and 6. Apparatus
provides a digital output. This digital output goes to a digital
display and/or recording device that may be internal or external 6.1 Test Jar, cylindrical, of clear glass, flat bottom, 33.2 mm
to the device. These devices are sometimes referred to as a to 34.8 mm outside diameter, and 115 mm to 125 mm in
“digital thermometer”. height. The inside diameter of the jar can range from 30.0 mm
3.1.3.2 Discussion—Portable electronic thermometers to 32.4 mm, within the constraint that the wall thickness be no
(PET) is an acronym sometimes used to refer to a subset of the greater than 1.6 mm. The jar shall have a line to indicate a
devices covered by this definition. sample height 54 mm 6 3 mm above the inside bottom. See
Fig. 1.
3.1.4 pour point, n—in petroleum products, the lowest
temperature at which movement of the test specimen is 6.2 Temperature Measuring Device—Either liquid-in-glass
observed under prescribed conditions of test. thermometer as described in 6.2.1 or Digital Contact Ther-
mometer (DCT) meeting the requirements described in 6.2.2.5
3.1.5 residual fuel, n—a liquid fuel containing bottoms
remaining from crude distillation or thermal cracking; some-
times referred to as heavy fuel oil. 5
Supporting data have been filed at ASTM International Headquarters and may
3.1.5.1 Discussion—Residual fuels comprise Grades 4, 5, be obtained by requesting Research Report RR:D02-1826. Contact ASTM Customer
and 6 fuel oils, as defined in Specification D396. Service at [email protected].

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

FIG. 1 Apparatus for Pour Point Test

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 D97 − 17
6.2.1 Liquid-in-Glass Thermometers, having the following than 15 cm. A 5 cm long stopper, that has a low thermal conductivity, with
ranges and conforming to the requirements prescribed in approximately half of it inserted in the sample tube will improve stability.
Specification E1 or Specifications for IP Standard Thermom- 6.2.2.1 The DCT calibration drift shall be checked at least
eters: annually by either measuring the ice point or against a
Temperature Thermometer reference thermometer in a constant temperature bath at the
Number prescribed immersion depth to ensure compliance with 6.2.2.
Thermometer Range ASTM IP
High cloud and pour −38 °C to +50 °C 5C 1C
See Test Method D7962.
Low cloud and pour −80 °C to +20 °C 6C 2C NOTE 2—When a DCT’s calibration drifts in one direction over several
Melting point +32 °C to +127 °C 61C 63C
calibration checks, that is, ice point, it may be an indication of deteriora-
6.2.1.1 Since separation of liquid column thermometers tion of the DCT.
occasionally occurs and may escape detection, thermometers 6.3 Cork, to fit the test jar, bored centrally for the test
should be checked immediately prior to the test and used only temperature measuring device.
if they prove accurate within 61 °C (for example ice point).
6.2.2 Digital Contact Thermometer Requirements: 6.4 Jacket, watertight, cylindrical, metal, flat-bottomed,
115 mm 6 3 mm depth, with inside diameter of 44.2 mm to
Parameter Requirement
DCT Guide E2877 Class G or better
45.8 mm. It shall be supported in a vertical position in the
cooling bath (see 6.7) so that not more than 25 mm projects out
Temperature range –65 °C to 90 °C of the cooling medium, and shall be capable of being cleaned.
Display resolution 1 °C minimum, preferably 0.1 °C 6.5 Disk, cork or felt, 6 mm thick to fit loosely inside the
jacket.
Sensor type PRT, thermistor, thermocouple
6.6 Gasket Ring Form, about 5 mm in thickness, to fit
Sensor 3 mm OD sheath with a sensing element less
than 10 mm in length
snugly around the outside of the test jar and loosely inside the
jacket. The gasket may be made of rubber, leather, or other
Minimum immersion Less than 40 mm per Test Method D7962 material that is elastic enough to cling to the test jar and hard
Sample immersion depth Between 10 mm and 15 mm in the sample.
enough to hold its shape. Its purpose is to prevent the test jar
Fig. 1 from touching the jacket.
Display accuracy ±500 mK (±0.5 °C) for combined probe and 6.7 Bath or Baths, maintained at prescribed temperatures
sensor with a firm support to hold the jacket vertical. The required
Response time less than or equal to 25 s as defined in
bath temperatures may be obtained by refrigeration if
Specification E1137 available, otherwise by suitable cooling mixtures. Cooling
mixtures commonly used for bath temperatures down to those
Drift less than 500 mK (0.5 °C) per year
shown are in Table 1.
Calibration error less than 500 mK (0.5 °C) over the range of
intended use. 7. Reagents and Materials
Calibration range –40 °C or lower to 85 °C 7.1 The following solvents of technical grade are appropri-
ate for low-temperature bath media.
Calibration data 4 data points evenly distributed over calibration
range with data included in calibration report.
7.1.1 Acetone, (Warning—Extremely flammable).
7.1.2 Alcohol, Ethanol (Warning—Flammable).
Calibration report From a calibration laboratory with demonstrated 7.1.3 Alcohol, Methanol (Warning—Flammable. Vapor
competency in temperature calibration which is
traceable to a national calibration laboratory or
harmful).
metrology standards body 7.1.4 Petroleum Naphtha, (Warning—Combustible. Vapor
NOTE 1—When the DCT display is mounted on the end to the probe’s harmful).
sheath, the test jar with the probe inserted will be unstable. To resolve this, 7.1.5 Solid Carbon Dioxide, (Warning—Extremely cold
it is recommended that the probe be less than 30 cm in length but no less −78.5 °C).

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 D97 − 17
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. Procedure 8.3.1 Specimens Having Pour Points Above −33 °C—Heat

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

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 D97 − 17
specimen in the test jar is noted, then replace the test jar NOTE 4—The precision statements were developed using liquid-in-glass
immediately in the jacket and repeat a test for flow at the next thermometers corresponding to those in Specification E1 or IP Specifica-
tions for IP Standard Thermometers.
temperature, 3 °C lower. Typically, the complete operation of
removal, wiping, and replacement shall require not more than 10.1.1 Lubricating Oil: 7
3 s. 10.1.1.1 Repeatability—The difference between successive
8.6.1 If the specimen has not ceased to flow when its test results, obtained by the same operator using the same
temperature has reached 27 °C, transfer the test jar to a jacket apparatus under constant operating conditions on identical test
in a cooling bath maintained at 0 °C 6 1.5 °C. As the specimen material would, in the long run, in the normal and correct
continues to get colder, transfer the test jar to a jacket in the operation of this test method, exceed 6 °C only in one case in
next lower temperature cooling bath in accordance with Table twenty. Differences greater than this should be considered
2. suspect.
8.6.2 If the specimen in the jar does not show movement 10.1.1.2 Reproducibility—The difference between two
when tilted, hold the jar in a horizontal position for 5 s, as single and independent test results, obtained by different
noted by an accurate timing device, and observe the specimen operators working in different laboratories on identical test
carefully. If the specimen shows any signs of movement before material would, in the long run, in the normal and correct
5 s has passed, replace the test jar immediately in the jacket and operation of this test method, exceed 9 °C only in one case in
repeat a test for flow at the next temperature, 3 °C lower. twenty. Differences greater than this should be considered
suspect.
8.7 Continue in this manner until a point is reached at which
10.1.1.3 The precision statements7 were derived from a
the specimen shows no movement when the test jar is held in
1998 interlaboratory test program using Practice D6300. Par-
a horizontal position for 5 s. Record the observed reading of
ticipants analyzed five sets of duplicate base oils, three sets of
the test thermometer.
duplicate multigrade lubricating oils, and one set each of
8.8 For black specimen, cylinder stock, and residual fuel duplicate hydraulic oils and automatic transmission fluid in the
specimen, the result obtained by the procedure described in 8.1 temperature range of –51 °C to –11 °C. Seven laboratories
through 8.7 is the upper (maximum) pour point. If required, participated with the manual Test Method D97. Information on
determine the lower (minimum) pour point by heating the the type of samples and their average pour points are in
sample while stirring, to 105 °C, pouring it into the jar, and Research Report RR:D02-1499.7
determining the pour point as described in 8.4 through 8.7.
NOTE 5—The precision statements are the derived values rounded up to
8.9 Some specifications allow for a pass/fail test or have the next testing interval value. The actual derived precision values appear
pour point limits at temperatures not divisible by 3 °C. In these in Table X1.1.
cases, it is acceptable practice to conduct the pour point 10.1.2 Middle Distillate and Residual Fuel: 8
measurement according to the following schedule: Begin to 10.1.2.1 Repeatability—The difference between successive
examine the appearance of the specimen when the temperature test results obtained by the same operator using the same
of the specimen is 9 °C above the specification pour point. apparatus under constant operation conditions on identical test
Continue observations at 3 °C intervals as described in 8.6 and material would, in the long run, in the normal and correct
8.7 until the specification temperature is reached. Report the operation of this test method, exceed 3 °C only in one case in
sample as passing or failing the specification limit. twenty. Differences greater than this should be considered
9. Calculation and Report suspect.
10.1.2.2 Reproducibility—The difference between two
9.1 Add 3 °C to the temperature recorded in 8.7 and report single and independent test results, obtained by different
the result as the Pour Point, ASTM D97. For black oil, and so operators working in different laboratories on identical test
forth, add 3 °C to the temperature recorded in 8.7 and report material would, in the long run, in the normal and correct
the result as Upper Pour Point, ASTM D97, or Lower Pour operation of this test method, exceed 9 °C only in one case in
Point, ASTM D97, as required. twenty. Differences greater than this should be considered
10. Precision and Bias suspect.
10.1.2.3 The precision statements8 were prepared with data
10.1 Precision—The precision of this test method as deter-
on sixteen middle distillate and residual fuels tested by twelve
mined by the statistical examination of the interlaboratory test
cooperators. The fuels had pour points ranging from −33 °C to
results is as follows:
+51 °C.
TABLE 2 Bath and Sample Temperature Ranges NOTE 6—The precision statements are the derived values rounded up to
the next testing interval value. The actual derived precision values can be
Bath Temperature Sample Temperature
seen in Table X1.1.
Setting, °C Range, °C
48 ± 1.5 or 12 above Preheat to at least 45 or 9
NOTE 7—The precisions in 10.1.2 are not known to have been derived
expected pour point above expected pour point using Practice D6300.
24 ± 1.5 Start to 27
0 ± 1.5 27 to 9
–18 ± 1.5 9 to –6
7
–33 ± 1.5 –6 to –24 Supporting data (the results of the 1998 interlaboratory cooperative test
–51 ± 1.5 –24 to –42 program) have been filed at ASTM International Headquarters and may be obtained
–69 ± 1.5 –42 to –60 by requesting Research Report RR:D02-1499.
8
Based on the results of the 1983 interlaboratory cooperative test program.

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 D97 − 17
10.2 Bias—There being no criteria for measuring bias in 11. Keywords
these test-product combinations, no statement of bias can be 11.1 petroleum products; pour point
made.

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 − 17

SUMMARY OF CHANGES

Subcommittee D02.07 has identified the location of selected changes to this standard since the last issue
(D97 – 16) that may impact the use of this standard. (Approved Jan. 1, 2017.)

(1) Added new Appendix X2.

(2) Changed “thermometer” to “temperature measuring de-
vice” where appropriate.

Subcommittee D02.07 has identified the location of selected changes to this standard since the last issue
(D97 – 15) that may impact the use of this standard. (Approved Jan. 1, 2016.)

(1) Added new Research Report footnote5 to 6.2.

ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentioned
in this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the risk
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