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: D5950 − 14

Standard Test Method for

Pour Point of Petroleum Products (Automatic Tilt Method)1
This standard is issued under the fixed designation D5950; 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 (´) 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 using an automatic apparatus.

1. Scope* 2. Referenced Documents

1.1 This test method covers the determination of pour point 2.1 ASTM Standards:2
of petroleum products by an automatic instrument that tilts the D97 Test Method for Pour Point of Petroleum Products
test jar during cooling and detects movement of the surface of D4057 Practice for Manual Sampling of Petroleum and
the test specimen with an optical device. Petroleum Products
D4177 Practice for Automatic Sampling of Petroleum and
1.2 This test method is designed to cover the range of Petroleum Products
temperatures from −66 °C to +51 °C; however, the range of D6708 Practice for Statistical Assessment and Improvement
temperatures included in the 1992 interlaboratory test program of Expected Agreement Between Two Test Methods that
only covered the temperature range from −39 °C to +6 °C, and Purport to Measure the Same Property of a Material
the range of temperatures included in the 1998 interlaboratory
2.2 Energy Institute Standard:3
test program was −51 °C to −11 °C. (See Section 13.)
IP 15 Test Method for Pour Point of Petroleum Products
1.3 Test results from this test method can be determined at
1 °C or 3 °C intervals. 3. Terminology
1.4 This test method is not intended for use with crude oils. 3.1 Definitions:
3.1.1 pour point, n—in petroleum products, the lowest
NOTE 1—The applicability of this test method on residual fuel samples temperature at which movement of the test specimen is
has not been verified. For further information on applicability, refer to
observed under the prescribed conditions of this test method.
13.4.
3.2 Definitions of Terms Specific to This Standard:
1.5 The values stated in SI units are to be regarded as
3.2.1 no-flow point, n—in petroleum products, the tempera-
standard. No other units of measurement are included in this
ture of the test specimen at which a wax crystal structure or
standard.
viscosity increase, or both, impedes movement of the surface
1.6 This standard does not purport to address all of the of the test specimen under the conditions of the test.
safety concerns, if any, associated with its use. It is the 3.2.1.1 Discussion—The no-flow point occurs when, upon
responsibility of the user of this standard to establish appro- cooling, the formation of wax crystal structures or the viscosity
priate safety and health practices and determine the applica- increase, or both, has progressed to the point where the applied
bility of regulatory limitations prior to use. observation device no longer detects movement under the
conditions of the test. The preceding observation temperature,
at which flow of the test specimen is last observed, is the pour
point.

1 2
This test method is under the jurisdiction of ASTM Committee D02 on For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
Subcommittee D02.07 on Flow Properties. Standards volume information, refer to the standard’s Document Summary page on
Current edition approved May 1, 2014. Published June 2014. Originally the ASTM website.
3
approved in 1996. Last previous edition approved in 2012 as D5950 – 12a. DOI: Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR,
10.1520/D5950-14. U.K., http://www.energyinst.org.uk.

*A Summary of Changes section appears at the end of this standard

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 D5950 − 14
TABLE 1 Jacket and Specimen Temperature Cooling Profile
Specimen Temperature, °C Jacket Temperature, °C
+27 > = ST > +9 0 ± 0.5
+9 > = ST > −6 −18 ± 0.5
−6 > = ST > −24 −33 ± 0.5
−24 > = ST > −42 −51 ± 0.5
−42 > = ST > −60 −69 ± 0.5
−60 > = ST > −78 −87 ± 0.5

FIG. 1 Optical Detection System

5.5 This test method yields a pour point in a format similar

to Test Method D97/IP15 when the 3 °C interval results are
reported.
NOTE 3—Since some users may wish to report their results in a format
similar to Test Method D97 (in 3 °C intervals) the precisions were derived
for the temperatures rounded to the 3 °C intervals. For statements on bias
relative to Test Method D97, see 13.3.
5.6 This test method has better repeatability and reproduc-
ibility relative to Test Method D97/IP15 as measured in the
1998 interlaboratory test program. (See Section 13.)
3.2.2 tilting, v—technique of movement where the test jar in
a vertical position is moved towards a horizontal position to 6. Apparatus
induce specimen movement.
3.2.2.1 Discussion—When the test jar is tilted and held in a 6.1 Optical Automatic Pour Point Apparatus4—The auto-
horizontal position for 5 s without detection of specimen matic pour point apparatus described in this test method
movement, this is the no-flow point and the test is complete. consists of a microprocessor controller that is capable of
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controlling one or more independent test cells. The apparatus

4. Summary of Test Method shall include provisions for independently controlling the
temperature of each cell according to the specified cooling
4.1 After preliminary heating, the test specimen is inserted profile, monitoring continuously the specimen temperature,
into the automatic pour point apparatus. After starting the and detecting any movement of the specimen during tilting (see
program, the specimen is cooled according to the cooling Fig. 1). The instrument shall be operated according to the
profile listed in Table 1 and examined at either 1 °C or 3 °C manufacturer’s instructions.
intervals. The lowest temperature at which movement of
specimen is detected, by the automatic equipment, is displayed 6.2 Temperature Probe, IEC 751 Class A: ∆ T = 6
as the pour point. (0.15 + 0.002 |T|), capable of measurement from +70 °C down
to −80 °C. The temperature probe shall be in the center of the
NOTE 2—If the automatic pour apparatus’s preheat option is utilized, test jar and the top of the platinum tip immersed 3 mm below
place the test specimen into the apparatus. After starting the program, the
apparatus will automatically carry out the preliminary heating. the surface of the oil.
6.3 Test Jar, clear cylindrical glass, flat bottom, 34 mm 6
5. Significance and Use 0.5 mm outside diameter, 1.4 mm 6 0.15 mm wall thickness,
5.1 The pour point of a petroleum product is an index of the 120 mm 6 0.5 mm height, thickness of the bottom 2.4 mm
lowest temperature of its utility for certain applications. Flow maximum, marked with a line to indicate the sample height
characteristics, like pour point, can be critical for the correct 54 mm 6 0.5 mm above the inside bottom.
operation of lubricating oil systems, fuel systems, and pipeline 6.4 Jacket, brass, cylindrical, flat bottom, 113 mm 60.2 mm
operations. in depth, 45 +0, −0.1 mm inside diameter. It shall be cooled
5.2 Petroleum blending operations require precise measure- according to the cooling profile specified.
ment of the pour point.
5.3 This test method can determine the pour point of the test 4
The sole source of supply of the ISL Model CPP97-6, CPP97-2, and CPP-5Gs
specimen with a resolution of 1.0 °C. known to the committee at this time is ISL SA, BP 40, 14790 Verson, France. If you
are aware of alternative suppliers, please provide this information to ASTM
5.4 Test results from this test method can be determined at International Headquarters. Your comments will receive careful consideration at a
either 1 °C or 3 °C intervals. meeting of the responsible technical committee,1 which you may attend.

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 D5950 − 14

FIG. 2 Test Jar Cooling Chamber and Cooling System

6.5 Cooling System, either an external system equipped with temperature, allow the sample to cool until its temperature is at least 70 °C
a circulating pump and capable of maintaining a temperature at before transferring.
least 10 °C below the last required jacket temperature level 8.3 For some sample types, such as viscous lube oils that are
(see Table 1 and Fig. 2), or an internal system capable of prone to having entrained air or gas bubbles present in the
maintaining the required jacket temperatures (see Table 1 and sample, the use of an ultrasonic bath (see 6.8) without the
Fig. 2). heater turned on (if so equipped), has been found effective in
6.6 Cork Disk, 6 mm 6 0.2 mm thick to fit loosely inside dissipating bubbles typically within 5 min.
the jacket. Felt may be used but special attention must be paid 9. Preparation of Apparatus
to avoid moisture in the felt disk. The felt disk must be dried
before each test. 9.1 Prepare the instrument for operation in accordance with
the manufacturer’s instructions.
6.7 Cork Ring, to fit snugly around the outside of the test jar
and loosely inside the test cell. Its purpose is to prevent the test 9.2 Clean and dry the test head and test jar using suitable
jar from touching the cooling jacket. solvents as prescribed by the manufacturer.
6.8 Ultrasonic Bath, Unheated—(optional)—with an oper- 9.3 Adjust the set-point of the cooling system, when
ating frequency between 25 kHz to 60 kHz and a typical power necessary, to the appropriate temperature to cool the jackets to
output of ≤100 W, of suitable dimensions to hold container(s) the required temperatures (see Table 1).
placed inside of bath, for use in effectively dissipating and NOTE 5—For most applications, when using an external cooling system,
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removing air or gas bubbles that can be entrained in viscous the recirculating cooler will be set at its lowest operating temperature.
sample types prior to analysis. It is permissible to use ultra- 10. Calibration and Standardization
sonic baths with operating frequencies and power outputs
outside this range, however it is the responsibility of the 10.1 Ensure that all of the manufacturer’s instructions for
laboratory to conduct a data comparison study to confirm that calibrating, checking, and operating the apparatus are fol-
results determined with and without the use of such ultrasonic lowed.
baths does not materially impact results. 10.1.1 A test head simulator, Part No. V02306, is used to
calibrate the equipment. The test head simulator uses precision
7. Reagents and Materials resistors in place of the PT 100 temperature probe to calibrate
7.1 Methyl Alcohol, Anhydrous, for use as cooling medium the jacket and specimen temperature electronics. Follow the
in circulating bath system, when used. manufacturer’s calibration instructions.
7.2 Cleaning Solvents, suitable for cleaning and drying the 10.2 A sample with a well documented pour point can be
test jar and test head, such as petroleum naphtha and hexane. used to verify performance of the apparatus. Alternatively, a
(Warning—Flammable. Liquid causes eye burns. Vapor harm- sample which has been extensively tested in a pour point
ful. May be fatal or cause blindness if swallowed or inhaled.) interlaboratory study can be used.
11. Procedure
8. Sampling
11.1 Pour the sample into the test specimen jar to the scribed
8.1 Obtain a sample in accordance with Practice D4057 or
mark. When necessary, heat the sample in a water bath or oven
Practice D4177.
until it is just sufficiently fluid to pour the sample into the test
8.2 Samples of very viscous materials can be warmed until specimen jar. Samples with an expected pour point above
they are reasonably fluid before they are transferred; however, 36 °C or samples which appear solid at room temperature can
no sample shall be heated more than is absolutely necessary. be heated above 45 °C, but should not be heated above 70 °C
The sample shall not be heated and transferred into the test (see Note 4).
specimen jar unless its temperature is 70 °C or lower.
11.2 Subject the test specimen to the following preliminary
NOTE 4—In the event the sample has been heated above this treatment or use the instrument’s automatic preheat option.

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 D5950 − 14
NOTE 6—Residual fuels have been known to be sensitive to thermal 12. Report
history. In the case where a residual fuel sample is tested, refer to Test
Method D97 for sample treatment. 12.1 Report the temperature recorded in 11.10 together with
the model and testing interval as pour point in accordance with
11.2.1 When the expected pour point (EP) is known to be Test Method D5950.
≤−33 °C, heat the test specimen to 45 °C in a bath or oven
maintained at 48 °C. 13. Precision and Bias
11.2.2 When the expected pour point (EP) is known to be 13.1 Precision—The precision of this test method as deter-
>−33 °C, heat the test specimen to EP + 9 °C, or at least to mined by the statistical examination of the interlaboratory test
45 °C but no higher than 70 °C (see Note 4). results is as follows:
11.3 Place a cork disk at the bottom of the jacket in the 13.1.1 Pour Point at 3 °C Testing Intervals:
required cell and fit a cork ring to the test jar. The cork ring 13.1.1.1 Repeatability—The difference between successive
should be 25 mm 6 3 mm above the bottom of the test jar. test results, obtained by the same operator using the same
apparatus under constant operating conditions on identical test
11.4 Place the test jar in the selected test cell. Attach the material, would in the long run, in the normal and correct
detector head according to the manufacturer’s instructions. operation of this test method, exceed the following, only in one
11.5 Select the desired testing interval (1 °C or 3 °C). case in twenty.
3.9 °C
11.6 Enter the expected pour point (EP). If 3 °C testing 13.1.1.2 Reproducibility—The difference between two
intervals are chosen (11.5) you must enter an expected pour single and independent test results, obtained by different
point that is a multiple of 3 °C. operators working in different laboratories on identical test
11.7 Start the test in accordance with the manufacturer’s material, would in the long run, in normal and correct operation
instructions. of this test method, exceed the following, only in one case in
twenty.
11.8 At this point, the instrument shall monitor the test 6.1 °C
specimen with the optical detector, adjusting the jacket tem- 13.1.2 Pour Point at 1 °C Testing Intervals:
perature to the first temperature level (according to Table 1) 13.1.2.1 Repeatability—The difference between successive
and measuring the specimen temperature. The instrument shall test results, obtained by the same operator using the same
automatically change the jacket temperature in accordance apparatus under constant operating conditions on identical test
with the specimen temperature (according to Table 1). The time material, would in the long run, in the normal and correct
to move the jacket temperature from one level to the next lower operation of this test method, exceed the following, only in one
level shall not exceed 200 s, for jacket temperatures down to case in twenty.
–52 °C. The instrument shall start tilting the specimen (without 2.7 °C
removing it from the jacket) in the prescribed manner when the 13.1.2.2 Reproducibility—The difference between two
temperature of the test specimen is at 9 °C higher than the single and independent test results, obtained by different
expected pour point. If the specimen flows during the tilting operators working in different laboratories on identical test

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movement, the no-flow point is not reached and the jacket material, would in the long run, in normal and correct operation
returns to the waiting vertical position for the next test. The test of this test method, exceed the following, only in one case in
will continue until the jacket is in a complete horizontal twenty.
position and the detector does not detect any movement of the 4.5 °C
specimen for 5 s. This temperature, the no-flow point, plus 1 °C
or 3 °C (depending on the test interval selected) is the pour 13.2 Bias—Since there is no accepted reference material
point of the oil (see Fig. 1). When the pour point is determined, suitable for determining the bias for the procedure in this test
the instrument shall display the pour point result and start to method, bias has not been determined.
reheat the test specimen. 13.3 Relative Bias:
13.3.1 Pour points at 3 °C testing intervals were compared
NOTE 7—For lower jacket temperatures, the time to move from one
jacket temperature level to the next jacket temperature should not exceed to the results from Test Method D97. Relative bias5 among
300 s. Maintain cooling system temperatures as low as possible to attain certain samples was observed; however, the observed bias does
these jacket temperatures in the shortest time period possible and utilize not appear to be of a systematic nature. Biases relative to Test
cooling system with cooling capacity capable to achieve the lowest Method D97/IP15 may conceivably occur for sample types not
temperature of application.
included in the 1998 interlaboratory test program.6
11.9 If the instrument detects the no-flow point on the first
NOTE 9—Large differences in results were observed between methods
tilting cycle (EP + 9 °C), disregard the result and start with for one sample in the 1998 Interlaboratory Test Study. The sample was a
11.1 using a higher expected pour point. high-sulfur winter diesel. When cooled during the performance of a test
11.10 Record the result as the pour point without any
correction. 5
Supporting data (1992 program) have been filed at ASTM International
Headquarters and may be obtained by requesting Research Report RR:D02-1312.
NOTE 8—Residual fuels have been known to be sensitive to thermal 6
Supporting data (1998 program, including information on the types of samples
history. In the case where a residual fuel sample is tested, refer to Test and their average pour points) have been filed at ASTM International Headquarters
Method D97 for sample treatment. and may be obtained by requesting Research Report RR:D02-1499.

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 D5950 − 14
method, this sample formed thin, but very large, crystals, that could be TABLE 2 1 °C Interval Relative Bias Adjustment CPP 5G
described as large plates. These crystals formed wherever sample-glass C CPP5G
contact was made as well as covered the top surface of the sample. The
10 0.53
entire sample, except for this all encasing thin skin of crystals, remained 5 0.33
liquid with apparent low viscosity. When this occurred and the sample was 0 0.13
handled gently, the sample did not pour, but with rougher handling, the -5 -0.07
crust broke and the sample poured readily. Users of this method are -10 -0.27
advised to be alert for differences in results between test methods when -15 -0.47
this behavior is observed in the sample being tested. -20 -0.67
-25 -0.87
13.3.2 Pour point results at 1 °C testing intervals were -30 -1.07
examined for bias relative to the pour point results at 3 °C -35 -1.27
-40 -1.47
intervals. A bias of 1.1 °C on average was observed. -45 -1.67
13.3.2.1 Discussion—It shall be noted that when a specimen -50 -1.87
is tested at 1 °C intervals, statistically the results will be 1 °C -55 -2.07
-60 -2.27
lower than the results produced by 3 °C testing intervals. This
is due to test increment and reporting differences. Differences
greater than 1 °C over a number of samples would be from
another cause. In the interlaboratory test program, the tests at
1 °C intervals yielded pour point lower than those obtained CPP-5Gs can be further improved by applying the bias-
from the tests at 3 °C intervals by 1.1 °C in average. correction outlined in Eq 1. See Table 2. No sample specific
13.4 The precision statements and the relative bias informa- bias was observed.
tion were derived from a 1998 interlaboratory test program.6 X 5 0.96Y 2 0.13 (1)
Participants analyzed two sets of duplicate diesel fuel oils, five
sets of duplicate base oils, three sets of duplicate multigrade where:
lubricating oils, and one set each of duplicate hydraulic oils X = CPP97-6(2) Models predicted result in ºC, and
and automatic transmission fluid in the temperature range of Y = CPP 5Gs Models result in ºC.
−51 °C to −11 °C. Eight laboratories participated with the 13.5.2 The degree of agreement between the averages of
automatic apparatus, testing at 1 °C and 3 °C intervals, and 3 ºC interval results from Models CPP97-6(2) and Models
seven laboratories participated with the manual Test Method CPP-5Gs can be further improved by applying the bias-
D97 apparatus. correction outlined in Eq 2. No sample specific bias was
13.5 Relative Bias between Models CPP97-6(2) and CPP- observed.
5Gs7—The statistical analysis of the between method bias by X 5 Y11.21 (2)
Practice D6708 indicates that there is some statistical bias
between the average results of the models of instruments. See where:
research report RR:D02-1740 for further information. X = CPP97-6(2) Models predicted result in ºC, and
13.5.1 The degree of agreement between the averages of Y = CPP 5Gs Models result in ºC.
1 °C interval results from Models CPP97-6(2) and Models
14. Keywords

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7
Supporting data have been filed at ASTM International Headquarters and may 14.1 D97 equivalent; petroleum products; pour point; tilt
be obtained by requesting Research Report RR:D02-1740. method

SUMMARY OF CHANGES

Subcommittee D02.07 has identified the location of selected changes to this standard since the last issue
(D5950–12a) that may impact the use of this standard. (Approved May 1, 2014.)

(1) Added 6.8 and 8.3.

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 D5950 − 14
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