ASTM D5985-96e1

NOTICE: This standard has either been superseded and replaced by a new version or discontinued.
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e1
Designation: D 5985 – 96 An American National Standard
AMERICAN SOCIETY FOR TESTING AND MATERIALS
100 Barr Harbor Dr., West Conshohocken, PA 19428
Reprinted from the Annual Book of ASTM Standards. Copyright ASTM
Standard Test Method for
Pour Point of Petroleum Products (Rotational Method)
This standard is issued under the fixed designation D 5985; 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 (e) indicates an editorial change since the last revision or reapproval.
e NOTE—Figures A1.1 and A1.2 were editorially corrected in May 1999.
1. Scope IP15 Test Method for Pour Point of Petroleum Products
1.1 This test method covers the determination of pour point
3. Terminology
of petroleum products by an automatic instrument that con-
3.1 Definitions:
tinuously rotates the test specimen against a suspended detec-
3.1.1 pour point, n—in petroleum products, the lowest
tion device during cooling of the test specimen.
temperature at which movement of the test specimen is
1.2 This test method includes the range of temperatures
observed under prescribed conditions of test.
from − 57 to + 51°C.
3.2 Definitions of Terms Specific to This Standard:
NOTE 1—The range of temperatures which were included in the 1992
3.2.1 no-flow point, n—in petroleum products, the tempera-
interlaboratory program only covered the temperature range of − 39
ture of the test specimen at which a wax crystal structure or
to + 6°C (see 13.4).
viscosity increase, or both, impedes movement of the surface
1.3 This test method determines the no-flow point of petro-
of the test specimen under the conditions of the test.
leum products by detection of the crystal structure or viscosity
3.2.2 Discussion—The no-flow point occurs when, upon
increase, or both, in the sample that is sufficient to impede flow
cooling, the formation of wax crystal structures or viscosity
of the specimen.
increase, or both, have progressed to the point where the
1.4 This test method is not intended for use with crude oils.
applied observation device no longer detects movement under
1.5 The values stated in inch-pound units are to be regarded
the conditions of the test. The preceding observation tempera-
as the standard. The values given in parentheses are for
ture, at which flow of the test specimen is last observed, is the
information only.
pour point.
1.6 This standard does not purport to address all of the
3.2.3 D 97/IP15 equivalent pour point, n—in petroleum
safety concerns, if any, associated with its use. It is the
products, the temperature calculated by rounding the no-flow
responsibility of the user of this standard to establish appro-
point to the next higher integer which is a multiple of 3°C.
priate safety and health practices and determine the applica-
3.2.4 Discussion—The no-flow point can be measured with
bility of regulatory limitations prior to use.
a resolution of 0.1°C in this test method. In Test Method D 97
observations for no-flow are in 3°C intervals and when results
2. Referenced Documents
with a similar format to Test Method D 97 are required, this
2.1 ASTM Standards:
calculation shall be performed. Some apparatus can perform
D 97 Test Method for Pour Point of Petroleum Products
this calculation automatically.
D 4057 Practice for Manual Sampling of Petroleum and
3.2.5 rotational, n—in this standard, the technique of turn-
Petroleum Products
ing the test specimen jar in an upright position upon a turntable
D 4177 Practice for Automatic Sampling of Petroleum and
with a stationary positioned, temperature sensor containing
Petroleum Products
pendulum, inserted into the test specimen.
2.2 IP Standards:
3.2.6 Discussion—Upon cooling of the test specimen, the
resultant crystal formation or viscosity increase in the speci-
men exerts force upon the pendulum, offsetting the stationary
position and causing detection of the no-flow point.
This test method is under the jurisdiction of ASTM Committee D-2 on
Petroleum Products and Lubricantsand is the direct responsibility of Subcommittee
D02.07on Flow Properties.
Current edition approved July 10, 1996. Published September 1996.
2 4
Annual Book of ASTM Standards, Vol 05.01. Available from Institute of Petroleum, 61 New Cavendish St., London, England
Annual Book of ASTM Standards, Vol 05.02. W1M 8AR.
D 5985
4. Summary of Test Method 20°C colder than the lowest expected pour point to be
measured.
4.1 After inserting the test specimen into the automatic pour
point apparatus, and initiation of the program, the test speci-
7. Reagents and Material
men is heated and then cooled by maintaining a constant
7.1 Methyl Alcohol, anhydrous, for use as cooling medium
temperature differential between the cooling block and the
in circulating bath.
sample. The test specimen is continuously tested for flow
7.2 Cleaning Solvents, suitable for cleaning and drying the
characteristics by rotating the test specimen cup at approxi-
specimen cup and pendulum, such as petroleum naptha and
mately 0.1 rpm against a stationary, counter-balanced, sphere-
acetone.
shaped pendulum. The temperature of the test specimen at
which a crystal structure or a viscosity increase, or both, within
NOTE 3—Warning: Flammable. Liquid causes eye burns. Vapor harm-
the test specimen causes the displacement of the pendulum is
ful. May be fatal or cause blindness if swallowed or inhaled.
recorded with a resolution of 0.1°C. The test specimen is then
8. Sampling
heated to the original starting temperature.
8.1 Obtain a sample in accordance with Practices D 4057 or
5. Significance and Use
by D 4177.
5.1 The pour point of a petroleum product is an index of the
8.2 Samples of very viscous materials can be warmed until
lowest temperature of its utility for certain applications. Flow
they are reasonably fluid before they are transferred; however,
characteristics, such as pour point, can be critical for the
no sample shall be heated more than is absolutely necessary.
correct operation of lubricating systems, fuel systems, and
The sample shall not be heated and transferred into the test
pipeline operations.
specimen cup unless its temperature is 70°C or lower.
5.2 Petroleum blending operations require precise measure-
NOTE 4—In the event the sample has been heated above this tempera-
ment of the pour point.
ture, allow the sample to cool until its temperature is at least 70°C before
5.3 This test method can determine the temperature of the
transferring.
test specimen with a resolution of 0.1°C at which either
crystals have formed or viscosity increases sufficiently to
9. Preparation of Apparatus
impede movement of the petroleum product.
9.1 Prepare the instrument for operation in accordance with
5.4 This test method yields a D 97/IP15 equivalent pour
the manufacturer’s instructions.
point when the 3°C interval results are reported.
9.2 Clean and dry the test specimen cup and the cooling
NOTE 2—Since some users may wish to report their results in a format well using suitable solvents as prescribed by the apparatus
similar to Test Method D 97 (in 3°C intervals) the precisions were derived
manufacturer.
for the temperatures rounded to the 3°C intervals. The term equivalent is
9.3 Prepare the refrigerated circulating bath for operation in
intended to mean in the same format. For statements on bias relative to
accordance with the manufacturer’s instructions and allow it to
Test Method D 97, see 13.3.
attain a temperature at least 20°C lower than the expected pour
5.5 This test method has better repeatability and comparable
point of the sample.
reproducibility relative to Test Method D 97 as measured in the
1992 interlaboratory program.
10. Calibration and Standardization
10.1 Ensure that all of the manufacturer’s instructions for
6. Apparatus
calibrating, checking, and operating the apparatus are fol-
6.1 Automatic Apparatus —The automatic pour point appa-
lowed.
ratus described in the Annex A1 consists of a microprocessor
10.2 Adjust the position of the measuring pendulum, when
controlled measuring unit that is capable of heating, cooling,
necessary, according to the manufacturer’s instructions.
rotating, and recording the temperature of the test specimen.
10.3 A sample with a well documented pour point can be
The apparatus shall be equipped with a digital display, cooling/
used to verify performance of the apparatus. Alternatively, a
heating block assembly, turntable, test specimen cup and
sample which has been extensively tested in a pour point
measuring head containing a counter-balanced pendulum and
interlaboratory study can be used.
temperature measuring device.
6.2 Test Specimen Cup—The test specimen cup is a flat
11. Procedure
bottom aluminum cup with the dimensions in A1.2. To indicate
11.1 Transfer the specimen into the
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