ASTM D6892-03(2008)

NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
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Designation: D6892 − 03(Reapproved 2008)
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 (´) indicates an editorial change since the last revision or reapproval.
1. Scope 2.2 Energy Institute Standard:
IP15Test Method for Pour Point of Petroleum Products
1.1 This test method covers the determination of the pour
point of petroleum products by an automatic instrument that
3. Terminology
tilts the test jar to detect movement of the surface of the test
specimen with an optical device, after being removed from a 3.1 Definitions:
regulated, stepped-bath cooling jacket. 3.1.1 pour point, n—in petroleum products, the lowest
temperature at which movement of the test specimen is
1.2 This test method is designed to cover the range of
observed under prescribed conditions of test.
temperatures from −57 to +51°C; however, the range of
temperatures included in the 1998 interlaboratory test program 3.2 Definitions of Terms Specific to This Standard:
only covered the temperature range from −51 to −11°C. 3.2.1 no-flow point, n—in petroleum products, the tempera-
ture of the test specimen at which a wax crystal structure or
1.3 Test results from this test method can be determined at
viscosity increase, or both, impedes movement of the surface
either 1 or 3°C testing intervals.
of the test specimen under the conditions of the test.
1.4 This test method is not intended for use with crude oils.
3.2.1.1 Discussion—The no-flow point occurs when, upon
NOTE 1—The applicability of this test method on residual fuel samples
cooling, the formation of wax crystal structures or viscosity
has not been verified. For further information on the applicability, refer to
increase,orboth,hasprogressedtothepointwheretheapplied
13.4.
observation device no longer detects movement under the
1.5 The values stated in SI units are to be regarded as
conditions of the test. The preceding observation temperature
standard. No other units of measurement are included in this
at which flow of the test specimen is last observed is the pour
standard.
point.
1.6 This standard does not purport to address all of the
3.2.2 tilting, vt—technique of movement where the test jar
safety concerns, if any, associated with its use. It is the
in a vertical position is moved towards a horizontal position to
responsibility of the user of this standard to establish appro-
induce specimen movement.
priate safety and health practices and determine the applica-
3.2.2.1 Discussion—When the test jar is tilted and held in a
bility of regulatory limitations prior to use.
horizontal position for 5 s without detection of movement of
the surface of the specimen, this is the no-flow point and the
2. Referenced Documents
test is complete.
2.1 ASTM Standards:
D97Test Method for Pour Point of Petroleum Products 4. Summary of Test Method
D4057Practice for Manual Sampling of Petroleum and
4.1 After insertion of the specimen into the automatic pour
Petroleum Products
point apparatus and initiation of the testing program, the
D4177Practice for Automatic Sampling of Petroleum and
specimen is heated and then cooled according to a prescribed
Petroleum Products
profile. The specimen surface is examined periodically for
movement using an optical camera system mounted on top of
the specimen test jar, while tilting the specimen test jar. The
This test method is under the jurisdiction of ASTM Committee D02 on test jar is removed from the jacketed cooling chamber prior to
PetroleumProductsandLubricantsandisthedirectresponsibilityofSubcommittee
eachexamination.Thelowesttemperature,whenmovementof
D02.07 on Flow Properties.
the surface of the specimen is detected, is recorded as the pour
Current edition approved Dec. 15, 2008. Published February 2009.Originally
point determined by this Test Method D6892.
approved in 2003. Last previous edition approved in 2003 as D6892–03. DOI:
10.1520/D6892-03R08.
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standard’s Document Summary page on Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR,
the ASTM website. U.K., http://www.energyinst.org.uk.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6892 − 03 (2008)
FIG. 1 Schematic of Cooling/Heating Block and Cooling Circulating Bath
5. Significance and Use
5.1 Thepourpointofapetroleumproductisanindexofthe
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.
5.2 Petroleum blending operations require precise measure-
ment of the pour point.
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
toTest Method D97 or IP15, 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 D97 or IP15 (in 3°C intervals) the precision data
were derived for the 3°C intervals. For statements on bias relative to Test
Method D97 or IP15, see the research report.
FIG. 2 Picture of Apparatus
5.5 Thistestmethodhascomparablerepeatabilityandbetter
reproducibility relative to Test Method D97 or IP15 as
measuredinthe1998interlaboratoryprogram(seeSection13).
the specimen. The apparatus shall be equipped with a user
6. Apparatus
interface, cooling/heating block assembly with cylindrical
jacket with an inside diameter of 44.2 to 45.8 mm, and about
6.1 Automatic Apparatus —Theautomaticpourpointappa-
115 mm in depth to accept the test jar) robotic mechanisms for
ratus described in this test method (see Fig. 2) consists of a
lifting,tilting,replacingthetestjar,opticalcamerasystem,and
microprocessor controlled measuring unit that is capable of
a temperature measuring device.
heatingthespecimentoprogrammedtemperatures,coolingthe
specimen according to programmed cooling profiles, mechani-
6.2 Test Jar—Clear, cylindrical glass, flat bottom (dark-
cally manipulating the test jar according to the programmed
ened),31.5 60.5mminsidediameterand120 62mmheight
test procedure, while optically observing the surface of the
with a wall thickness of 1.25 6 0.25 mm. The jar shall be
specimen for movement, using a camera system mounted on
markedwithalinetoindicatesamplefillingheightcorrespond-
top of the specimen test jar and recording the temperature of
ing to 45 6 0.5 mL.
6.3 Temperature Probe—Capableofmeasurementfrom+70
The sole source of supply of the Herzog Model MP852 or HCP852 known to
to −80°C with a resolution of 0.1°C. The temperature probe
the committee at this time is Walter Herzog, Lauda, Germany. If you are aware of
shall be suspended in the center axis of the test jar and the top
alternative suppliers, please provide this information to ASTM International
ofthetemperaturesensingzoneimmersedbelowthesurfaceof
Headquarters.Your comments will receive careful consideration at a meeting of the
responsible technical committee, which you may attend. the specimen.
D6892 − 03 (2008)
10. Calibration and Verification
10.1 Ensure that all of the manufacturer’s instructions for
calibrating, checking, and operating the apparatus are fol-
lowed.
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
FIG. 3 Assembled Apparatus
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
6.4 Circulating Bath—Refrigeration unit, equipped with a
Method D97 for sample treatment.
circulating pump, capable of maintaining the liquid cooling
11.2 Insert the test jar into the apparatus and start the test in
medium at a temperature at least 20°C lower than the lowest
accordance with the manufacturer’s instructions.
expected pour point to be measured. The circulating bath is
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.
7. Reagents and Materials
11.4 When the expected pour point is known to be at or
below −33°C, preselect a starting temperature of 45°C.
7.1 Bath Cooling Medium—Suitable for use in the circulat-
ing bath (an example is methyl alcohol-anhydrous).
11.5 When the expected pour point is not known, preselect
(Warning—Flammable.Liquidcauseseyeburns.Vaporharm-
a starting temperature of 45°C. When the expected pour point
ful. May be fatal or cause blindness if swallowed or inhaled.)
is not known and the sample must be heated to allow transfer
into the test jar, preselect a starting temperature corresponding
7.2 Cleaning Solvents—Suitableforcleaninganddryingthe
to the preheat temperature. (Warning—Exercise care when
test jar and temperature measuring device, such as; petroleum
selectingstartingtemperaturesabove45°C.Sampleswhichare
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