ASTM D97-17b(2022)
(Test Method)Standard Test Method for Pour Point of Petroleum Products
Standard Test Method for Pour Point of Petroleum Products
SIGNIFICANCE AND USE
5.1 The pour point of a petroleum specimen is an index of the lowest temperature of its utility for certain applications.
SCOPE
1.1 This test method covers and is intended for use on any petroleum product.3 A procedure suitable for black specimens, cylinder stock, and nondistillate fuel oil is described in 8.8. The cloud point procedure formerly part of this test method now appears as Test Method D2500.
1.2 Currently there is no ASTM test method for automated Test Method D97 pour point measurements.
1.3 Several ASTM test methods offering alternative procedures for determining pour points using automatic apparatus are available. None of them share the same designation number as Test Method D97. When an automatic instrument is used, the ASTM test method designation number specific to the technique shall be reported with the results. A procedure for testing the pour point of crude oils is described in Test Method D5853.
1.4 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.
1.5 WARNING—Mercury has been designated by many regulatory agencies as a hazardous substance that can cause serious medical issues. Mercury, or its vapor, has been demonstrated to be hazardous to health and corrosive to materials. Use caution when handling mercury and mercury-containing products. See the applicable product Safety Data Sheet (SDS) for additional information. The potential exists that selling mercury or mercury-containing products, or both, is prohibited by local or national law. Users must determine legality of sales in their location.
1.6 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use.
1.7 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.
General Information
Relations
Standards Content (Sample)
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
1,2
Pour Point of Petroleum Products
ThisstandardisissuedunderthefixeddesignationD97;thenumberimmediatelyfollowingthedesignationindicatestheyearoforiginal
adoptionor,inthecaseofrevision,theyearoflastrevision.Anumberinparenthesesindicatestheyearoflastreapproval.Asuperscript
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 mercuryormercury-containingproducts,orboth,isprohibited
bylocalornationallaw.Usersmustdeterminelegalityofsales
1.1 This test method covers and is intended for use on any
3 in their location.
petroleum product. Aprocedure suitable for black specimens,
1.6 This standard does not purport to address all of the
cylinderstock,andnondistillatefueloilisdescribedin8.8.The
safety concerns, if any, associated with its use. It is the
cloud point procedure formerly part of this test method now
responsibility of the user of this standard to establish appro-
appears as Test Method D2500.
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
areavailable.Noneofthemsharethesamedesignationnumber
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 inTest Method
2. Referenced Documents
D5853.
2.1 ASTM Standards:
1.4 The values stated in SI units are to be regarded as
D117Guide for Sampling, Test Methods, and Specifications
standard. No other units of measurement are included in this
for Electrical Insulating Liquids
standard.
D396Specification for Fuel Oils
D2500Test Method for Cloud Point of Petroleum Products
1.5 WARNING—Mercury has been designated by many
and Liquid Fuels
regulatory agencies as a hazardous substance that can cause
D5853Test Method for Pour Point of Crude Oils
serious medical issues. Mercury, or its vapor, has been dem-
D6300Practice for Determination of Precision and Bias
onstrated to be hazardous to health and corrosive to materials.
Data for Use in Test Methods for Petroleum Products,
Use caution when handling mercury and mercury-containing
Liquid Fuels, and Lubricants
products. See the applicable product Safety Data Sheet (SDS)
D7962Practice for Determination of Minimum Immersion
for additional information. The potential exists that selling
Depth and Assessment of Temperature Sensor Measure-
ment Drift
This test method is under the jurisdiction of ASTM International Committee
E1Specification for ASTM Liquid-in-Glass Thermometers
D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct
E644Test Methods for Testing Industrial Resistance Ther-
responsibility ofASTM Subcommittee D02.07 on Flow Properties. The technically
equivalent standard as referenced is under the jurisdiction of the Energy Institute mometers
Subcommittee SC-C-4.
E1137SpecificationforIndustrialPlatinumResistanceTher-
Current edition approved Nov. 1, 2022. Published November 2022. Originally
mometers
approved in 1927, replacing D47. Last previous edition approved in 2017 as
E2877Guide for Digital Contact Thermometers
D97–17b. DOI: 10.1520/D0097-17BR22.
This test method was adopted as a joint ASTM-IP Standard in 1965.
This test method has been developed through the cooperative effort between
ASTMandtheEnergyInstitute,London.ASTMandIPstandardswereapprovedby
ASTMandEItechnicalcommitteesasbeingtechnicallyequivalentbutthatdoesnot For referenced ASTM standards, visit the ASTM website, www.astm.org, or
imply both standards are identical. contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
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.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D97 − 17b (2022)
2.2 Energy Institute Standards: 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.
Blackoilsareusedinheavy-dutyequipmentapplications,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.
4. Summary of Test Method
3.1.3 digital contact thermometer (DCT), n—an electronic
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
displayand/orrecordingdevicethatmaybeinternalorexternal
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 TestJar,cylindrical,ofclearglass,flatbottom,33.2mm
to 34.8mm outside diameter, and 115mm to 125mm in
height. The inside diameter of the jar can range from 30.0mm
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
D97 − 17b (2022)
may be necessary to use a 1000Ω sensor in order to obtain accurate
to 32.4mm, within the constraint that the wall thickness be no
measurements.
greater than 1.6mm. The jar shall have a line to indicate a
NOTE 2—When the DCT display is mounted on the end to the probe’s
sample height 54mm 6 3mm above the inside bottom. See
sheath,thetestjarwiththeprobeinsertedwillbeunstable.Toresolvethis,
Fig. 1.
it is recommended that the probe be less than 30 cm in length but no less
than15cm.A5cmlongstopper,thathasalowthermalconductivity,with
6.2 Temperature Measuring Device—Either liquid-in-glass
approximately half of it inserted in the sample tube will improve stability.
thermometer as described in 6.2.1 or Digital Contact Ther-
6.2.2.1 The DCT calibration drift shall be checked at least
mometer (DCT) meeting the requirements described in 6.2.2.
annually by either measuring the ice point or against a
6.2.1 Liquid-in-Glass Thermometers, having the following
reference thermometer in a constant temperature bath at the
ranges and conforming to the requirements prescribed in
prescribed immersion depth to ensure compliance with 6.2.2.
Specification E1 or Specifications for IP Standard Thermom-
See Practice D7962.
eters:
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 3mm depth, with inside diameter of 44.2mm to
should be checked immediately prior to the test and used only
45.8mm. It shall be supported in a vertical position in the
if they prove accurate within 61°C (for example ice point).
coolingbath(see6.7)sothatnotmorethan25mmprojectsout
6.2.2 Digital Contact Thermometer Requirements:
of the cooling medium, and shall be capable of being cleaned.
Parameter Requirement
6.5 Disk, cork or felt, 6mm thick to fit loosely inside the
DCT Guide E2877 Class F or better
jacket.
A
Nominal temperature range High Pour: –38 °C to 50 °C
Low Pour: –80 °C to 20 °C 6.6 Gasket Ring Form, about 5mm 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
B jacket. The gasket may be made of rubber, leather, or other
Accuracy ±500 mK (±0.5 °C)
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
C
Sensor sheath 4.2 mm OD maximum
D from touching the jacket.
Sensor length Less than 10 mm
E
Immersion depth Less than 40 mm per Practice D7962
6.7 Bath or Baths, maintained at prescribed temperatures
Sample immersion depth Tip of sheath between 10 mm and 15 mm
with a firm support to hold the jacket vertical. The required
below sample meniscus
Fig. 1
bath temperatures may be obtained by refrigeration if
E
Measurement drift Less than 500 mK (0.5 °C) per year
available, otherwise by suitable cooling mixtures. Cooling
F
Response time Less than or equal to 4 s per footnote F
mixtures commonly used for bath temperatures down to those
Calibration error Less than 500 mK (0.5 °C) over the range of
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-
7. Reagents and Materials
bration range that is consistent with the range of
use. The calibration data is to be included in the
7.1 The following solvents of technical grade are appropri-
calibration report.
ate for low-temperature bath media.
Calibration report From a calibration laboratory with demonstrated
competency in temperature calibration which is
7.1.1 Acetone, (Warning—Extremely flammable).
traceable to a national calibration laboratory or
7.1.2 Alcohol, Ethanol (Warning—Flammable).
metrology standards body
7.1.3 Alcohol, Methanol (Warning—Flammable. Vapor
A
harmful).
The nominal temperature range may be different from the values shown provided
the calibration and accuracy criteria are met.
7.1.4 Petroleum Naphtha, (Warning—Combustible. Vapor
B
Accuracy is the combined accuracy of the DCT unit, which is the display and
harmful).
sensor.
C
7.1.5 Solid Carbon Dioxide, (Warning—Extremely cold
Sensor sheath is the tube that holds the sensing element. The value is the
outside diameter of the sheath segment containing the sensor element.
−78.5°C).
D
The physical length of the temperature sensing element.
E
As determined by Practice D7962 or an equivalent procedure.
8. Procedure
F
Response Time—The time for a DCT to respond to a step change in tempera-
ture. The response time is 63.2 % of the step change time as determined per
8.1 Pour the specimen into the test jar to the level mark.
Section 9 of Test Methods E644. The step change evaluation begins at 20 °C ±
When necessary, heat the specimen in a bath until it is just
5 °C air to 77 °C ± 5 °C with water circulating at 0.9 m ⁄s ± 0.09 m ⁄s past the
sensor.
sufficiently fluid to pour into the test jar.
NOTE 1—When making measurements below –40°C with a PRT, it
NOTE4—Itisknownthatsomematerials,whenheatedtoatemperature
higher than 45°C during the preceding 24h, do not yield the same pour
point results as when they are kept at room temperature for 24h prior to
Supporting data have been filed atASTM International Headquarters and may
beobtainedbyrequestingResearchReportRR:D02-1826.ContactASTMCustomer testing. Examples of materials which are known to show sensitivity to
Service at service@astm.org. thermal history are residual fuels, black oils, and cylinder stocks.
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°Cduringthepreceding24h,orwhenthethermalhistoryof 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 24h before testing. Samples which are known ensure that the liquid level is between the
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