ASTM D5949-96
(Test Method)Standard Test Method for Pour Point of Petroleum Products (Automatic Pressure Pulsing Method)
Standard Test Method for Pour Point of Petroleum Products (Automatic Pressure Pulsing Method)
SCOPE
1.1 This test method covers the determination of pour point of petroleum products by an automatic instrument that applies a controlled burst of nitrogen gas onto the specimen surface while the specimen is being cooled and detects movement of the surface of the test specimen with an optical device.
1.2 This test method is designed to cover the range of temperatures from 57 to +51°C. However, the range of temperatures included in the 1992 interlaboratory test program only covered the temperature range from 39 to +6°C and the range of temperatures included in the 1998 interlaboratory test program was from 51 to 11°C. (see 13.4).
1.3 Test results from this test method can be determined at 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 or residual fuel samples has not been verified. For further information on applicability, refer to 13.4.
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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Designation: D 5949 – 96 An American National Standard
Standard Test Method for
Pour Point of Petroleum Products (Automatic Pressure
Pulsing Method)
This standard is issued under the fixed designation D 5949; 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.
INTRODUCTION
This test method covers an alternative procedure for the determination of pour point of petroleum
products Test Method D 97/IP15 using an automatic apparatus. The results from this test method based
on observations at 3°C temperature intervals have been found to be equivalent to Test Method
D 97/IP15. When specification requires Test Method D 97/IP15, do not substitute this test method.
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 applies
3.1 Definitions:
a controlled burst of nitrogen gas onto the specimen surface
3.1.1 pour point, n—in petroleum products, the lowest
while the specimen is being cooled and detects movement of
temperature at which movement of the test specimen is
the surface of the test specimen with an optical device.
observed under the prescribed conditions of the test.
1.2 This test method includes the range of temperatures
3.2 Definition of Terms Specific to This Standard:
from −57 to +51°C.
3.2.1 no-flow point, n—in petroleum products, the tempera-
NOTE 1—The range of temperatures which was included in the 1992
ture of the test specimen at which a wax crystal structure or
interlaboratory test program only covered the temperature range of −39
viscosity increase, or both, impedes movement of the surface
to +6°C (see 13.4).
of the test specimen under the conditions of the test.
1.3 Test results from this test method can also be determined
3.2.1.1 Discussion—The no-flow point occurs when, upon
at 1 and 2°C testing intervals; however, precision data on these
cooling, the formation of wax crystal structures or viscosity
testing intervals are not available.
increase or both has progressed to the point where the applied
1.4 This test method is not intended for use with crude oils.
observation device no longer detects movement under the
1.5 The values stated in SI units are regarded as standard.
conditions of the test. The preceding observation temperature,
1.6 This standard does not purport to address all of the
at which flow of the test specimen is last observed, is the pour
safety concerns, if any, associated with its use. It is the
point.
responsibility of the user of this standard to establish appro-
3.2.2 D 97/IP15 equivalent pour point, n—in petroleum
priate safety and health practices and determine the applica-
products, the temperature calculated by rounding the no-flow
bility of regulatory limitations prior to use.
point of the test specimen to the next higher integer which is a
multiple of 3°C.
2. Referenced Documents
3.2.2.1 Discussion—Test results from this test method can
2.1 ASTM Standards:
be determined at 1, 2, or 3°C intervals. Should the user wish to
D 97 Test Method for Pour Point of Petroleum Products
provide results with a similar format to Test Method D 97/
D 4057 Practice for Manual Sampling of Petroleum and
IP15, then testing at 3°C intervals shall be used.
Petroleum Products
3.2.3 pulse, n—a controlled burst of nitrogen gas of a fixed
D 4177 Practice for Automatic Sampling of Petroleum and
pressure and flow rate sufficient to cause movement on the
Petroleum Products
surface of the test specimen without fracturing the wax
2.2 IP Standard:
structure which may be formed in the specimen.
3.2.4 Peltier device, n—a solid state thermoelectric device
constructed with dissimilar semiconductor materials, config-
This test method is under the jurisdiction of ASTM Committee D-2 on
ured in such a way that it will transport heat to or away from
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.07.0D on Wax Related Viscometric Properties of Fuels and Oils.
Current edition approved Apr. 10, 1996. Published June 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.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 5949
a test specimen dependent on the direction of electric current surface movement and recording the temperature of the speci-
applied to the device. men as described in detail in Annex A1. It is specifically
designed to detect the lowest temperature at which movement
4. Summary of Test Method
of the surface of the specimen is observed upon application of
4.1 After inserting the test specimen into the automatic pour the pulse.
point apparatus, and initiation of the test program, the test 6.2 The apparatus shall be equipped with a specimen cup, an
specimen is heated and then cooled by a Peltier device at a rate array of optical detectors, light source, pressure pulsing unit,
of 1.5 6 0.1°C/min. At temperature intervals of 1, 2 or 3°C, digital display, Peltier device, and a specimen temperature
depending on the selection made by the user, a moving force in measuring device.
the form of a pressurized pulse of nitrogen gas is imparted onto 6.3 The pressure pulsing unit consists of a stainless steel
the surface of the specimen. Multiple optical detectors are used tubing, 250 6 2 mm long and 1.1 6 0.1 mm inside diameter.
in conjunction with a light source to monitor movement of the This tubing is connected to a constant pressure source at one
surface of the specimen. The lowest temperature at which end, which serves as an inlet. The other end of the tubing,
movement of the specimen surface is observed upon applica- which serves as the outlet, is bent and positioned such that it is
tion of a pulse of nitrogen gas is recorded as the pour point, pointing to the center of the specimen at an acute angle. The
Test Method D 5949.
distance between the outlet and the center of the specimen is 8
6 2 mm.
5. Significance and Use
6.4 The Peltier device shall be capable of heating or cooling
5.1 The pour point of a petroleum product is an index of the the test specimen at a rate of 1.5 6 0.1°C/min.
lowest temperature of its utility for certain applications. Flow 6.5 The temperature measuring device in the specimen cup
characteristics, like pour point can be critical for the correct shall be capable of measuring the temperature of the test
operation of lubricating oil systems, fuel systems, and pipeline specimen from −80 to +70°C at a resolution of 0.1°C.
operations. 6.6 The apparatus shall be equipped with fittings to permit
5.2 Petroleum blending operations require precise measure- the circulation of water or other liquid cooling media to remove
ment of the pour point. heat generated by the Peltier device and other electronic
5.3 In most cases, this test method does not require the use components of the apparatus.
of mechanical refrigeration apparatus (see 7.1). 6.7 The apparatus shall be equipped with fittings to permit
5.4 This test method yields a Test Method D 97/IP15 the delivery of nitrogen gas to the pressure pulsing unit.
equivalent pour point when the 3°C interval results are
7. Reagents and Materials
reported.
7.1 Coolant—Tap water or other liquid heat exchange
NOTE 2—Since some users may wish to report their results in a format
medium sufficient to remove heat generated by the Peltier
similar to Test Method D 97 (in 3°C intervals) the precisions were derived
device and other electronic components from the apparatus. To
from the temperatures rounded to the 3° intervals. The term equivalent is
intended to mean—in the same format. For statements on bias relative to achieve specimen cooling to −60°C, supply circulation of
Test Method D 97, see 13.3.
liquid cooling medium at +25°C or lower to the apparatus.
Obtain cooling performance data from the apparatus manufac-
5.5 Test results from this test method can also be determined
turer if lower specimen temperatures are desired or if the tap
at 1 or 2°C intervals to improve resolution; however, precision
water temperature is higher than 25°C.
data on these temperature intervals are not available.
7.2 Dry Nitrogen Gas—Nitrogen gas with a dew point
5.6 This test method has better repeatability and reproduc-
below the lowest temperature attained by the specimen.
ibility relative to Test Method D 97/IP15 as measured in the
1992 interlaboratory test program.
NOTE 3—Warning: Compressed gas.
NOTE 4—Warning: Inert gas can be an asphyxiant when inhaled.
6. Apparatus
7.3 Adjustable Volume Pipette, capable of dispensing
6.1 Automatic Apparatus —The automatic pour point appa-
0.150 6 0.005 mL of sample.
ratus described in this test method consists of a microprocessor
7.4 Cotton Swabs, plastic shaft cotton swabs to clean the
controlled test chamber that is capable of heating and cooling
sample cup.
the test specimen, providing a controlled pulse of nitrogen gas
onto the specimen surface, optically detecting the specimen
8. Sampling
8.1 Obtain a sample in accordance with Practice D 4057 or
by Practice D 4177.
The results of this interlaboratory test program are available from ASTM
8.2 Samples of very viscous materials may be warmed until
Headquarters in the form of a research report. Request RR:D02-1312.
The following instrument has been found suitable for use in this test method:
they are reasonably fluid before they are transferred; however,
Phase Technology Pour Point Analyzer model series 30, 50 and 70 available from
no sample shall be heated more than is absolutely necessary.
Phase Technology, Richmond, B.C. Canada, V7A 5C9. The various model series
mentioned above are differentiated by their cooling capacities; however, all of them
are capable of covering the entire temperature range specified in the scope.
This pour point analyzer is covered by a patent. Interested parties are invited to A suitable pipette is the Eppendorf pipette available from Brinkmann Instru-
submit information regarding the identification of an alternative to this patented item ments Inc., One Cantiague Rd., P.O. Box 1019, Westbury, NY 11590-0207.
to the ASTM Headquarters. Your comments will receive careful consideration at a Suitable cotton swabs are Q-tips available from Cheesebrough Ponds, Trumbull
meeting of the responsible technical committe
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