ASTM D6892-03
(Test Method)Standard Test Method for Pour Point of Petroleum Products (Robotic Tilt Method)
Standard Test Method for Pour Point of Petroleum Products (Robotic Tilt Method)
SIGNIFICANCE AND USE
The pour point of a petroleum product is an index of the lowest temperature of its utility for certain applications. Flow characteristics, such as pour point, can be critical for the correct operation of lubricating systems, fuel systems, and pipeline operations.
Petroleum blending operations require precise measurement of the pour point.
Test results from this test method can be determined at either 1 or 3°C intervals.
This test method yields a pour point in a format similar to Test Method D 97 or IP 15, when the 3°C interval results are reported.
Note 2—Since some users may wish to report their results in a format similar to Test Method D 97 or IP 15 (in 3°C intervals) the precision data were derived for the 3°C intervals. For statements on bias relative to Test Method D 97 or IP 15, see the research report.
This test method has comparable repeatability and better reproducibility relative to Test Method D 97 or IP 15 as measured in the 1998 interlaboratory program.5
FIG. 1 Schematic of Cooling/Heating Block and Cooling Circulating Bath
SCOPE
1.1 This test method covers the determination of the pour point of petroleum products by an automatic instrument that tilts the test jar to detect movement of the surface of the test specimen with an optical device, after being removed from a regulated, stepped-bath cooling jacket.
1.2 This test method is designed to cover the range of temperatures from -57 to +51°lC; however, the range of temperatures included in the 1998 interlaboratory test program only covered the temperature range from -51 to -11°C.
1.3 Test results from this test method can be determined at either 1 or 3°C testing intervals.
1.4 This test method is not intended for use with crude oils.
Note 1—The applicability of this test method on residual fuel samples has not been verified. For further information on the applicability, refer to 1.4.
1.5 The values stated in SI units are regarded as standard.
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 and health practices and determine the applicability of regulatory limitations prior to use.
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An American National Standard
Designation:D6892–03
Standard Test Method for
Pour Point of Petroleum Products (Robotic Tilt Method)
This standard is issued under the fixed designation D6892; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber 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—in petroleum products, the lowest
temperature at which movement of the test specimen is
1.1 This test method covers the determination of the pour
observed under prescribed conditions of test.
point of petroleum products by an automatic instrument that
3.2 Definitions of Terms Specific to This Standard:
tilts the test jar to detect movement of the surface of the test
3.2.1 no-flow point, n—in petroleum products, the tempera-
specimen with an optical device, after being removed from a
ture of the test specimen at which a wax crystal structure or
regulated, stepped-bath cooling jacket.
viscosity increase, or both, impedes movement of the surface
1.2 This test method is designed to cover the range of
of the test specimen under the conditions of the test.
temperatures from −57 to +51°C; however, the range of
3.2.1.1 Discussion—The no-flow point occurs when, upon
temperatures included in the 1998 interlaboratory test program
cooling, the formation of wax crystal structures or viscosity
only covered the temperature range from −51 to −11°C.
increase,orboth,hasprogressedtothepointwheretheapplied
1.3 Test results from this test method can be determined at
observation device no longer detects movement under the
either 1 or 3°C testing intervals.
conditions of the test. The preceding observation temperature
1.4 This test method is not intended for use with crude oils.
at which flow of the test specimen is last observed is the pour
NOTE 1—The applicability of this test method on residual fuel samples
point.
has not been verified. For further information on the applicability, refer to
3.2.2 tilting, vt—technique of movement where the test jar
13.4.
in a vertical position is moved towards a horizontal position to
1.5 The values stated in SI units are regarded as standard.
induce specimen movement.
1.6 This standard does not purport to address all of the
3.2.2.1 Discussion—When the test jar is tilted and held in a
safety concerns, if any, associated with its use. It is the
horizontal position for 5 s without detection of movement of
responsibility of the user of this standard to establish appro-
the surface of the specimen, this is the no-flow point and the
priate safety and health practices and determine the applica-
test is complete.
bility of regulatory limitations prior to use.
4. Summary of Test Method
2. Referenced Documents
4.1 After insertion of the specimen into the automatic pour
2.1 ASTM Standards:
point apparatus and initiation of the testing program, the
D97 Test Method for Pour Point of Petroleum Products
specimen is heated and then cooled according to a prescribed
D4057 Practice for Manual Sampling of Petroleum and
profile. The specimen surface is examined periodically for
Petroleum Products
movement using an optical camera system mounted on top of
D4177 Practice for Automatic Sampling of Petroleum and
the specimen test jar, while tilting the specimen test jar. The
Petroleum Products
test jar is removed from the jacketed cooling chamber prior to
2.2 IP Standard:
eachexamination.Thelowesttemperature,whenmovementof
IP15 Test Method for Pour Point of Petroleum Products
the surface of the specimen is detected, is recorded as the pour
point determined by this Test Method D6892.
3. Terminology
3.1 Definitions: 5. Significance and Use
5.1 Thepourpointofapetroleumproductisanindexofthe
1 lowest temperature of its utility for certain applications. Flow
This test method is under the jurisdiction of ASTM Committee D02 on
characteristics, such as pour point, can be critical for the
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.07 on Flow Properties.
correct operation of lubricating systems, fuel systems, and
Current edition approved July 10, 2003. Published September 2003.
pipeline operations.
Annual Book of ASTM Standards, Vol 05.01.
5.2 Petroleum blending operations require precise measure-
Annual Book of ASTM Standards, Vol 05.02.
Available from Institute of Petroleum (IP), 61 New Cavendish St., London,
ment of the pour point.
WIG 7AR, U.K.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D6892–03
FIG. 1 Schematic of Cooling/Heating Block and Cooling Circulating Bath
5.3 Test results from this test method can be determined at
either 1 or 3°C intervals.
5.4 This test method yields a pour point in a format similar
toTestMethodD97orIP15,whenthe3°Cintervalresultsare
reported.
NOTE 2—Since some users may wish to report their results in a format
similar to Test MethodD97 or IP15 (in 3°C intervals) the precision data
were derived for the 3°C intervals. For statements on bias relative to Test
MethodD97 or IP15, see the research report.
5.5 Thistestmethodhascomparablerepeatabilityandbetter
reproducibility relative to Test Method D97 or IP15 as
measured in the 1998 interlaboratory program.
6. Apparatus
6.1 Automatic Apparatus —Theautomaticpourpointappa-
ratus described in this test method (see Fig. 2) consists of a
microprocessor controlled measuring unit that is capable of
FIG. 2 Picture of Apparatus
heatingthespecimentoprogrammedtemperatures,coolingthe
specimen according to programmed cooling profiles, mechani-
cally manipulating the test jar according to the programmed
lifting,tilting,replacingthetestjar,opticalcamerasystem,and
test procedure, while optically observing the surface of the a temperature measuring device.
specimen for movement, using a camera system mounted on
6.2 Test Jar—Clear, cylindrical glass, flat bottom (dark-
top of the specimen test jar and recording the temperature of ened), 31.5 6 0.5 mm inside diameter and 120 6 2 mm height
the specimen. The apparatus shall be equipped with a user
with a wall thickness of 1.25 6 0.25 mm. The jar shall be
interface, cooling/heating block assembly with cylindrical markedwithalinetoindicatesamplefillingheightcorrespond-
jacket with an inside diameter of 44.2 to 45.8 mm, and about
ing to 45 6 0.5 mL.
115 mm in depth to accept the test jar) robotic mechanisms for 6.3 Temperature Probe—Capableofmeasurementfrom+70
to −80°C with a resolution of 0.1°C. The temperature probe
shall be suspended in the center axis of the test jar and the top
ofthetemperaturesensingzoneimmersedbelowthesurfaceof
Supporting data have been filed atASTM International Headquarters and may
the specimen.
be obtained by requesting Research Report RR: D02-1499.
The sole source of supply of the Herzog Model MP852 or HCP852 known to
6.4 Circulating Bath—Refrigeration unit, equipped with a
the committee at this time is Walter Herzog, Lauda, Germany. If you are aware of
circulating pump, capable of maintaining the liquid cooling
alternative suppliers, please provide this information to ASTM International
medium at a temperature at least 20°C lower than the lowest
Headquarters.Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. expected pour point to be measured. The circulating bath is
D6892–03
10.2 A sample with a well-documented pour point can be
used to verify the performance of the automatic apparatus.
Alternatively, a sample which has been extensively tested in a
pourpointcross-checkprogramcanbeused.Suchverification
materials can also be prepared from intra-company cross
checks.
11. Procedure
11.1 Fillthetestjaruptothemarkedlinewiththespecimen.
When necessary, heat the sample in a water bath or oven until
it is just sufficiently fluid to pour into the test jar.
NOTE 3—Residual fuels have been known to be sensitive to thermal
history. In the case where a residual fuel sample is tested, refer to Test
MethodD97 for sample treatment.
FIG. 3 Assembled Apparatus
11.2 Insert the test jar into the apparatus and start the test in
accordance with the manufacturer’s instructions.
11.3 When the expected pour point is known to be above
connected to the automatic apparatus through suitable means −33°C, preselect a starting temperature which is at least 9°C
for supplying the liquid cooling medium. above the expected pour point, but to at least 45°C.
11.4 When the expected pour point is known to be at or
7. Reagents and Materials below −33°C, preselect a starting temperature of 45°C.
11.5 When the expected pour point is not known, preselect
7.1 Bath Cooling Medium—Suitable for use in the circulat-
a starting temperature of 45°C. When the expected pour point
ing bath (an example is methyl alcohol-anhydrous).
is not known and the sample must be heated to allow transfer
(Warning—Flammable.Liquidcauseseyeburns.Vaporharm-
into the test jar, preselect a starting temperature corresponding
ful. May be fatal or cause blindness if swallowed or inhaled.)
to the preheat temperature. (Warning—Exercise care when
7.2 Cleaning Solvents—Suitableforcleaninganddryingthe
selectingstartingtemperaturesabove45°C.Sampleswhichare
test jar and temperature measuring device, such as; petroleum
fluid at ambient room temperature can also have a low
naphthaoracetone.(Warning—Flammable.Liquidcauseseye
temperature flash point. Use higher start t
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