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Astm D5853-24

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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: D5853 − 24

Designation: 441/17

Standard Test Method for


Pour Point of Crude Oils1,2
This standard is issued under the fixed designation D5853; 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.

1. Scope* 1.6 This international standard was developed in accor-


1.1 This test method covers two procedures for the deter- dance with internationally recognized principles on standard-
mination of the pour point temperatures of crude oils down to ization established in the Decision on Principles for the
−36 °C. Procedure A provides a measure of the maximum Development of International Standards, Guides and Recom-
(upper) pour point temperature and is described in 9.1. Proce- mendations issued by the World Trade Organization Technical
dure B provides a measure of the minimum (lower) pour point Barriers to Trade (TBT) Committee.
temperature and is described in 9.2.
2. Referenced Documents
1.2 The use of this test method is limited to use for crude
2.1 ASTM Standards:3
oils. Pour point temperatures of other petroleum products can
D97 Test Method for Pour Point of Petroleum Products
be determined by Test Method D97.
D130 Test Method for Corrosiveness to Copper from Petro-
1.3 The values stated in SI units are to be regarded as leum Products by Copper Strip Test
standard. No other units of measurement are included in this D323 Test Method for Vapor Pressure of Petroleum Products
standard. (Reid Method)
1.4 WARNING—Mercury has been designated by many D4057 Practice for Manual Sampling of Petroleum and
regulatory agencies as a hazardous substance that can cause Petroleum Products
serious medical issues. Mercury, or its vapor, has been dem- D4175 Terminology Relating to Petroleum Products, Liquid
onstrated to be hazardous to health and corrosive to materials. Fuels, and Lubricants
Use caution when handling mercury and mercury-containing D4177 Practice for Automatic Sampling of Petroleum and
products. See the applicable product Safety Data Sheet (SDS) Petroleum Products
for additional information. The potential exists that selling D7962 Practice for Determination of Minimum Immersion
mercury or mercury-containing products, or both, is prohibited Depth and Assessment of Temperature Sensor Measure-
by local or national law. Users must determine legality of sales ment Drift
in their location. E1 Specification for ASTM Liquid-in-Glass Thermometers
E77 Test Method for Inspection and Verification of Ther-
1.5 This standard does not purport to address all of the
mometers
safety concerns, if any, associated with its use. It is the
E644 Test Methods for Testing Industrial Resistance Ther-
responsibility of the user of this standard to establish appro-
mometers
priate safety, health, and environmental practices and deter-
E2251 Specification for Liquid-in-Glass ASTM Thermom-
mine the applicability of regulatory limitations prior to use.
eters with Low-Hazard Precision Liquids
For specific hazard statements, see Section 7.
E2877 Guide for Digital Contact Thermometers

3. Terminology
1
This test method is under the jurisdiction of ASTM International Committee
D02 on Petroleum Products, Liquid Fuels, and Lubricants and is the direct
3.1 Definitions:
responsibility of ASTM Subcommittee D02.07 on Flow Properties. The technically 3.1.1 For definitions of terms used in this test method, refer
equivalent standard as referenced is under the jurisdiction of the Energy Institute to Terminology D4175.
Subcommittee SC-B-7. 3.2 Definitions of Terms Specific to This Standard:
Current edition approved May 1, 2024. Published May 2024. Originally
approved in 1995. Last previous edition approved in 2017 as D5853 – 17a. DOI:
10.1520/D5853-24.
2 3
This test method has been developed through the cooperative effort between For referenced ASTM standards, visit the ASTM website, www.astm.org, or
ASTM and the Energy Institute, London. ASTM and IP standards were approved by contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
ASTM and EI technical committees as being technically equivalent but that does not Standards volume information, refer to the standard’s Document Summary page on
imply both standards are identical. the ASTM website.

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


Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States

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D5853 − 24
3.2.1 digital contact thermometer (DCT), n—an electronic characteristics. The lowest temperature at which movement of
device consisting of a digital display and associated tempera- the test specimen is observed is recorded as the pour point.
ture sensing probe.
5. Significance and Use
3.2.1.1 Discussion—This device consists of a temperature
sensor connected to a measuring instrument; this instrument 5.1 The pour point of a crude oil is an index of the lowest
measures the temperature-dependent quantity of the sensor, temperature of handleability for certain applications.
computes the temperature from the measured quantity, and
provides a digital output. This digital output goes to a digital 5.2 This is the only pour point method specifically designed
display and/or recording device that may be internal or external for crude oils.
to the device. These devices are sometimes referred to as a 5.3 The maximum and minimum pour point temperatures
“digital thermometer.” provide a temperature window where a crude oil, depending on
3.2.1.2 Discussion—PET is an acronym for portable elec- its thermal history, might appear in the liquid as well as the
tronic thermometers, a subset of digital contact thermometers solid state.
(DCT).
3.2.2 maximum (upper) pour point, n—the pour point ob- 5.4 The test method can be used to supplement other
tained after the test specimen has been subjected to a pre- measurements of cold flow behavior. It is especially useful for
scribed treatment designed to enhance gelation of wax crystals the screening of the effect of wax interaction modifiers on the
and solidification of the test specimen. flow behavior of crude oils.
3.2.3 minimum (lower) pour point, n—the pour point ob-
6. Apparatus
tained after the test specimen has been subjected to a pre-
scribed treatment designed to delay gelation of wax crystals 6.1 Pour Point Test Apparatus Assembly (see Fig. 1):
and solidification of the test specimen. 6.1.1 Test Jar, cylindrical, of clear glass, flat bottomed,
3.2.4 pour point, n—the lowest temperature at which move- outside diameter 33.2 mm to 34.8 mm, and height 115 mm to
ment of the test specimen is observed under the conditions of 125 mm. The inside diameter of the jar can range from
the test. 30.0 mm to 32.4 mm, within the constraint that the wall
thickness shall be no greater than 1.6 mm. The jar shall have a
4. Summary of Test Method line to indicate a sample height 54 mm 6 3 mm above the
4.1 After preliminary heating, the test specimen is cooled at inside bottom. The inside of the test jar (up to the mark) shall
a specified rate and examined at intervals of 3 °C for flow be visibly clean and free of scratches.

NOTE 1—All dimensions are stated in millimetres. Positioning of temperature sensing devices are shown in the figure.
FIG. 1 Apparatus for Pour Point Test

2
D5853 − 24
C
6.1.2 Temperature Measuring Device—Either liquid-in- Sensor sheath is the tube that holds the sensing element. The value is the
outside diameter of the sheath segment containing the sensor element.
glass thermometer as described in 6.1.2.1 or digital contact D
The physical length of the temperature sensing element.
thermometer (DCT) meeting the requirements described in E
As determined by Practice D7962 or an equivalent procedure.
F
6.1.2.3. Response Time—The time for a DCT to respond to a step change in tempera-
ture. The response time is 63.2 % of the step change time as determined per
6.1.2.1 Liquid-in-Glass Thermometers, having ranges Section 9 of Test Methods E644. The step change evaluation begins at 20 °C ±
shown in the following table and conforming to the require- 5 °C air to 77 °C ± 5 °C with water circulating at 0.9 m ⁄s ± 0.09 m ⁄s past the
ments prescribed in Specification E1 or Specification E2251 sensor.

for thermometers: NOTE 1—When making measurements below –40 °C with a PRT, it
Thermometer
may be necessary to use a 1000 Ω sensor in order to obtain accurate
Number measurements.
Thermometer Temperature Range NOTE 2—When the DCT display is mounted on the end to the probe’s
ASTM IP
sheath, the test jar with the probe inserted will be unstable. To resolve this,
High cloud and pour −38 °C to +50 °C 5C, S5C 1C it is recommended that the probe be between 15 cm and 30 cm in length.
Low cloud and pour −80 °C to +20 °C 6C 2C A 5 cm long stopper that has a low thermal conductivity with approxi-
Melting point +32 °C to +127 °C 61C 63C mately half of it inserted in the sample tube will improve stability.
6.1.2.2 Since separation of liquid column thermometers 6.1.2.4 The DCT calibration drift shall be checked at least
occasionally occurs and may escape detection, the ice point of annually by either measuring the ice point or against a
the thermometers shall be checked prior to the test and used reference thermometer in a constant temperature bath at the
only if they are accurate within 61 °C (see Test Method E77). prescribed immersion depth to ensure compliance with 6.1.2.3.
6.1.2.3 Digital Contact Thermometer Requirements for See Practice D7962.
Pour Point: 4
NOTE 3—When a DCT’s calibration drifts in one direction over several
Parameter Requirement calibration checks, it is an indication of a change in the DCT, thus a full
DCT Guide E2877 Class F or better recalibration is necessary.
Nominal temperature rangeA High Pour: –38 °C to 50 °C 6.1.3 Cork, to fit the test jar, center bored for the test
Low Pour: –80 °C to 20 °C thermometer.
Melt Point: 32 °C to 127 °C
6.1.4 Jacket, watertight, cylindrical, metal, flat bottomed,
Display resolution 0.1 °C minimum 115 mm 6 3 mm depth, with inside diameter of 44.2 mm to
45.8 mm. It shall be supported in a vertical position in the
AccuracyB ±500 mK (±0.5 °C)
cooling bath (6.1.7) so that no more than 25 mm projects out
Sensor type Platinum resistance thermometer (PRT) of the cooling medium. The jacket shall be capable of being
C
cleaned.
Sensor sheath 4.2 mm OD maximum
6.1.5 Disk, cork or felt, 6 mm thick to fit loosely inside the
Sensor lengthD Less than 10 mm jacket.
6.1.6 Gasket, to fit snugly around the outside of the test jar
Immersion depthE Less than 40 mm per Practice D7962
and loosely inside the jacket. The gasket shall be made of
Sample immersion depth Tip of sheath between 10 mm and 15 mm rubber, leather, or other material that is sufficiently elastic to
below sample meniscus
Fig. 1
cling to the test jar and hard enough to hold its shape. Its
purpose is to prevent the test jar from touching the jacket.
Measurement driftE Less than 500 mK (0.5 °C) per year 6.1.7 Cooling Bath or Baths, of a type suitable for obtaining
Response timeF Less than or equal to 4 s per footnote F
the required temperatures. The size and shape of the bath are
optional, but a support to hold the jacket firmly in a vertical
Calibration error Less than 500 mK (0.5 °C) over the range of position is essential. The bath temperature shall be monitored
intended use
by means of the appropriate thermometer (6.1.2) or any other
Calibration range Consistent with temperature range of use temperature measuring device capable of measuring and dis-
playing the designated temperature with the required precision
Calibration data Four data points evenly distributed over the cali-
bration range that is consistent with the range of
and accuracy. The required bath temperatures shall either be
use. The calibration data is to be included in the obtained by refrigeration or by suitable cooling mixtures and
calibration report. shall maintain the designated temperatures to within 61.5 °C.
Calibration report From a calibration laboratory with demonstrated
Cooling mixtures commonly used for bath temperatures are
competency in temperature calibration which is shown in Table 1.
traceable to a national calibration laboratory or
metrology standards body 6.2 Water Bath—The size and shape of the bath are optional,
but a support to hold the test jar immersed in the bath to above
A
The nominal temperature range may be different from the values shown provided the sample height in the test jar and in a firm vertical position
the calibration and accuracy criteria are met. is required. The required bath temperature may be maintained
B
Accuracy is the combined accuracy of the DCT unit, which is the display and
sensor. by any suitable means, provided the temperature can be
monitored and controlled to the designated temperature (61 °C
(9.1.4; 9.2.4)).
4
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1826. Contact ASTM Customer 6.3 Pressure Vessel, constructed of stainless steel according
Service at service@astm.org. to the dimensions given in Fig. 2, and capable of withstanding

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D5853 − 24
TABLE 1 Cooling Mixtures and Bath Temperatures
Bath Temperature
Ice and water 0 °C ± 1.5°C

Crushed ice and sodium chloride crystals or −18 °C ± 1.5°C


Acetone or petroleum naphtha or methanol or ethanol
(see Section 7) with solid carbon dioxide added to
give the desired temperature

Acetone or petroleum naphtha or methanol or ethanol –33 °C ± 1.5°C


(see Section 7) with solid carbon dioxide added to
give the desired temperature

Acetone or petroleum naphtha or methanol or ethanol –51 °C ± 1.5°C


(see Section 7) with solid carbon dioxide added to
give the desired temperature

Acetone or petroleum naphtha or methanol or ethanol –69 °C ± 1.5°C


(see Section 7) with solid carbon dioxide added to
give the desired temperature

a test pressure of 700 kPa. Alternative designs for the pressure of crude oil from which it was taken. Practices D4057 and
vessel cap and synthetic rubber gasket may be used provided D4177 provide guidance for obtaining such representative
that the internal dimensions of the pressure vessel are the same samples.
as those shown in Fig. 2. 8.2 Preparation of Test Samples—The pour point of crude
NOTE 4—This pressure vessel is identical to the pressure vessel oils is very sensitive to trace amounts of high melting waxes.
described in Test Method D130. Exercise meticulous care to ensure such waxes, if present, are
6.4 Timing Device, capable of measuring up to 30 s with a either completely melted or, if volatility constraints prevent
resolution of at least 0.1 s and an accuracy of 60.2 s or better. heating to complete melting, homogeneously suspended in the
sample (Appendix X1). Inspect the walls of the original
7. Reagents and Materials container to ensure that no high melting point material is left
sticking to the wall.
7.1 The following solvents of technical grade are appropri-
ate for low-temperature bath media. NOTE 7—It is not possible to define universal mandatory rules for the
7.1.1 Acetone, (Warning—Extremely flammable.) preparation of crude oil test samples. Guidelines for sample handling for
the most common situations are given in Appendix X1.
7.1.2 Petroleum Naphtha, (Warning—Combustible. Vapor
harmful.)
9. Procedure
NOTE 5—Typical petroleum naphtha used for cleaning purposes are VM
and P naphthas.
9.1 Procedure A for Maximum (Upper) Pour Point:
9.1.1 Pour the test sample into the test jar to the level mark.
7.2 Toluene, technical grade (Warning—Flammable. Vapor If necessary, reheat the test sample to a temperature at least
harmful.). 20 °C above the expected pour point (8.2 and Appendix X1)
7.3 Solid Carbon Dioxide, (Warning—Extremely cold but not higher than a temperature of 60 °C (Warning—The
(−78.5 °C).) vapor pressure of crude oils at temperatures higher than 60 °C
7.4 Sodium Chloride Crystals—Commercial or technical will usually exceed 100 kPa. Under these circumstances the
grade sodium chloride is suitable. sample container may rupture. Opening of the container may
induce foaming with resultant loss of sample and possible
7.5 Ethanol or Ethyl Alcohol—A commercial or technical injury to personnel.)
grade of dry ethanol is suitable for the cooling bath. 9.1.2 Immediately close the test jar with the cork carrying
(Warning—Flammable. Denatured. Cannot be made non- the high cloud and pour thermometer, or, if the expected pour
toxic.) point is above 36 °C, the melting point thermometer. Adjust the
7.6 Methanol or Methyl Alcohol—A commercial or techni- position of the cork and thermometer so the cork fits tightly, the
cal grade of dry methanol is suitable for the cooling bath. thermometer and the jar are coaxial, and the thermometer bulb
(Warning—Flammable. Vapor harmful.) is immersed to a depth that places the beginning of the
capillary 3 mm below the surface of the test specimen.
8. Sampling, Test Samples, and Test Specimens 9.1.3 Keep the test jar with the test specimen at room
NOTE 6—Sampling is defined as all steps required to obtain a portion of temperature (between 18 °C and 24 °C) for at least 24 h.
the contents of any pipe, tank, or other system and to place the sample into
the laboratory test container. NOTE 8—The pour point of a crude oil is dependent on the state of
crystallization of the wax in the test specimen. In crude oils, achieving
8.1 Laboratory Sample—It is essential that the sample equilibrium between crystallized wax and dissolved wax is a rather slow
received by the laboratory is representative of the batch or lot process. However, experience has shown that in a majority of cases, such

4
D5853 − 24

FIG. 2 Pressure Vessel

an equilibrium is reached within 24 h. Especially when a DCT is used, 9.1.4.1 As soon as the test specimen has reached the
additional care must be taken to ensure that the thermometer does not required temperature, remove the cork carrying the thermom-
move in the sample during the test, so additional support elements will
likely be needed. eter and stir the test specimen gently with a spatula or similar
device. Put the cork carrying the thermometer back in place
9.1.4 If the expected pour point is greater than 36 °C, heat
(see 9.1.2).
the sample to 9 °C above the expected pour point. If the
expected pour point is less than 36 °C, heat the sample to a 9.1.5 Ensure that the disk, gasket, and the inside of the
temperature of 45 °C 6 1 °C. Maintain the water bath (6.2) to jacket are clean and dry. Place the disk in the bottom of the
heat the sample at 48 °C 6 1 °C or at a temperature 12 °C jacket. Place the disk and jacket in the cooling medium a
higher than the expected pour point, whichever is higher. minimum of 10 min before the test jar is inserted. The use of

5
D5853 − 24
a jacket cover, while the empty jacket is cooling, is permitted. point. Continue observations at 3 °C intervals as described in 9.1.6 and
Remove the test jar from the water bath and dry with a tissue. 9.1.7 until the specification temperature is reached. Report the sample as
passing or failing the specification limit.
Place the gasket around the test jar, 25 mm from the bottom.
Insert the test jar into the jacket in the first bath maintained at 9.2 Procedure B for Minimum (Lower) Pour Point:
21 °C and commence observations for pour point. Never place 9.2.1 Pour 50 g of the test sample into a clean pressure
a test jar directly into the cooling medium. vessel (6.3 and Note 11). When necessary, reheat the test
9.1.6 Exercise care not to disturb the mass of test specimen sample to a temperature of at least 20 °C above the expected
nor permit the thermometer to shift in the test specimen; any pour point (8.2 and Appendix X1) but not higher than 60 °C
disturbance of the spongy network of wax crystals will lead to (Warning—The vapor pressure of crude oils at temperatures
a lower pour point and erroneous results (Note 8). higher than 60 °C will usually exceed 100 kPa. Under these
circumstances the sample container may rupture. Opening of
NOTE 9—With dark colored materials, such as crude oils, it is
impractical to observe, in the test jar, the onset of crystallization and the container may induce foaming with resultant loss of sample
network formation in the test specimen. Hence, it is presumed that and possible injury to personnel.) Check that the rubber ring is
network formation will begin at the very early stages of the cooling in place and screw the lid on tightly.
sequence.
NOTE 11—The pressure vessel may be cleaned by any appropriate
9.1.7 Pour points are expressed in temperatures which are solvent, provided the solvent is capable of dissolving remnants of high
positive or negative multiples of 3 °C. Begin to examine the melting wax and asphaltenes. Hot toluene (100 °C) has been found to be
appearance of the test specimen when the temperature of the an appropriate solvent for this purpose.
test specimen is 9 °C above the expected pour point (estimated 9.2.2 Heat the pressure vessel in an oil bath or by any other
as a multiple of 3 °C). At each test thermometer reading which suitable means to a temperature of 105 °C 6 2 °C and leave at
is a multiple of 3 °C below the starting temperature, remove that temperature for at least 30 min.
the test jar from the jacket. When necessary, remove moisture 9.2.3 Take the pressure vessel from the oil bath, wipe and
that limits visibility of the test specimen by wiping the surface dry the surface of the pressure vessel, swirl gently to homog-
of the test jar with a clean cloth moistened in alcohol at enize the contents, and leave the pressure vessel to cool at
approximately the temperature of the test specimen in the jar. room temperature for exactly 20 min 6 30 s.
Then tilt the jar just enough to ascertain whether there is 9.2.4 Carefully open the pressure vessel and transfer the
movement of the test specimen in the jar. When movement is sample into the test jar filling to the level mark of the test jar,
observed, immediately return the test jar into the jacket. If preheated in a water bath (6.2) kept at a temperature of 48 °C
movement of the specimen in the test jar is noted, then replace 6 1°C (Warning—After 20 min at ambient temperature, the
the test jar immediately in the jacket, and repeat a test for flow temperature of the test specimen will be approximately 50 °C.
at the next temperature, 3 °C lower. Typically the complete The vapor pressure at that temperature may still exceed
operation of removal, wiping, and replacement shall require 100 kPa. Under these circumstances, inattentive opening of the
not more than 3 s. pressure vessel may induce foaming with resultant loss of
9.1.7.1 If the test specimen has not ceased to flow when its sample and possible injury to personnel.)
temperature has reached 30 °C, transfer the test jar to the next 9.2.5 Immediately close the test jar with the cork carrying
lower temperature bath per the following schedule: the high cloud and pour thermometer, or, if the expected pour
(1) If the test specimen is at +30 °C, move to 0 °C bath; point is above 36 °C, the melting point thermometer. Adjust the
(2) If the test specimen is at +9 °C, move to −18 °C bath; position of the cork and thermometer so the cork fits tightly, the
(3) If the test specimen is at −9 °C, move to −33 °C bath; thermometer and the jar are coaxial, and the thermometer bulb
and is immersed to a depth which places the beginning of the
(4) If the test specimen is at −24 °C, move to −51 °C bath. capillary 3 mm below the surface of the test specimen.
9.1.7.2 If the test specimen in the jar does not show 9.2.6 Proceed as described in 9.1.5 – 9.1.8.
movement when tilted, hold the jar in a horizontal position for
5 s, as shown by an accurate timing device (6.4), and observe
10. Calculation and Report
the specimen carefully. If the test specimen shows any move-
ment before 5 s has passed, replace the test jar immediately in 10.1 Add 3 °C to the temperature recorded in 9.1.8 and
the jacket, and repeat a test for flow at the next temperature, report as Maximum Pour Point, ASTM D5853, Procedure A, or
3 °C lower. Minimum Pour Point, ASTM D5853, Procedure B, if the
9.1.8 Continue in this manner until a point is reached at procedure in 9.2 has been followed.
which the test specimen shows no movement when the test jar 10.2 If the test was discontinued (9.1.8.1), report the pour
is held in a horizontal position for 5 s. Record the observed point as ≤ −36 °C.
reading of the test temperature.
9.1.8.1 If the test specimen has reached −36 °C and still 11. Precision and Bias
shows movement, discontinue the test.
11.1 The following criteria are to be used for judging the
NOTE 10—To determine compliance with existing specifications having acceptability of results (95 % confidence):
pour point limits at temperatures not divisible by 3 °C, it is acceptable
practice to conduct the pour point measurement according to the following 11.1.1 Repeatability—The difference between successive
schedule. Begin to examine the appearance of the test specimen when the test results obtained by the same operator with the same
temperature of the test specimen is 9 °C above the specification pour apparatus under constant operating conditions on identical test

6
D5853 − 24
material would, in the long run, in the normal and correct NOTE 12—These precision values are derived from a 1994 cooperative
operation of the test method, exceed the following value only program5 and the current Committee D02 Statistical Method, RR:D02-
1007.6 The data in this study were obtained using liquid-in-glass ther-
in 1 case in 20. mometers.
Repeatability
Procedure °C (rounded) 11.2 Bias—The procedure in this test method has no bias
because the value of pour point is defined only in terms of this
A (max) 3.1 (3) (Note 12) test method.
B (min) 5.8 (6) (Note 12)
11.1.2 Reproducibility—The difference between two, single 12. Keywords
and independent results, obtained by different operators work-
12.1 cold flow; crude oil; pour point
ing in different laboratories on identical test material would, in
the long run, in the normal and correct operation of the test
method, exceed the following value only in 1 case in 20. 5
Supporting data have been filed at ASTM International Headquarters and may
Reproducibility be obtained by requesting Research Report RR:D02-1371. Contact ASTM Customer
Procedure °C (rounded) Service at service@astm.org.
6
Supporting data have been filed at ASTM International Headquarters and may
A (max) 18.0 (18) (Note 12) be obtained by requesting Research Report RR:D02-1007. Contact ASTM Customer
B (min) 22.0 (21) (Note 12) Service at service@astm.org.

ANNEX

(Mandatory Information)

A1. THERMOMETER SPECIFICATIONS

A1.1 See Table A1.1.

7
D5853 − 24
TABLE A1.1 Thermometer Specifications

NOTE 1—The emergent stem temperature is 21 C throughout the scale range


NOTE 2—Thermometers IP 1C/ASTM 5C (high cloud and pour), and IP 63C/ASTM 61C (melting point) conform to these requirements.
High cloud and pour Melting point
Range °C –38 to +50 32 to 127
Immersion mm 108 79
Graduation at each °C 1 0.2
Longer lines at each °C 5 1
Figured at each °C 10 2
Scale error, max °C 0.5 0.2
Expansion chamber to permit heating to °C 100 150
Overall length mm 230 ± 5 380 ± 5
Stem diameter mm 6 to 8 6 to 8
Bulb length mm 7 to 10 18 to 28
Distance from bottom of bulb to line at °C –38 32
mm 120 to 130 105 to 115
Length of scale mm 65 to 85 200 to 240

APPENDIX

(Nonmandatory Information)

X1. GUIDELINE FOR SAMPLE HANDLING

X1.1 Introduction X1.1.6 If crude oil samples are to be tested for vapor
X1.1.1 Sampling of crude oils from pipelines, tankers, pressure, density, or any other test in which retention of light
barges, or trucks is usually beyond control of the laboratory ends is essential, subsamples for these test methods shall be
and adequately covered by the appropriate sampling protocols taken first before any other sample handling procedures are
as specified in Practices D4057 and D4177. invoked for performing sampling for other tests such as pour
point.
X1.1.2 This guideline covers the sampling from containers
submitted to the analytical laboratory for analysis. It covers the X1.1.7 Never subsample crude oils in plastic containers or
handling of samples between the point at which they were any other container that will not retain gases or light materials
extracted or drawn, and the laboratory test bench or sample and cannot be heated without deformation.
storage. It is meant to ensure that the nature and integrity of the
samples are maintained as far as possible. X1.2 Heating of Samples
X1.1.3 The method of handling a sample will depend on the X1.2.1 Crude oils stored at temperatures below their cloud
purpose for which it was taken. The laboratory analytical point will show wax deposition on the walls of the (sample)
procedure to be used will often require a special handling containers. The wax coming out of the solution will be
procedure to be associated with it. For this reason, consult the preferentially the high melting wax. It is this type of wax that
appropriate methods of test so that any necessary instructions has the most pronounced influence on the crude oil pour point
as to sample handling can be given to the person drawing the and, at the same time, is the most difficult to redissolve or
sample. If the analytical procedures to be applied have con- disperse in the crude oil. Proper treatment of the samples
flicting requirements, as is often the case for crude oils, then before subsampling for pour point, therefore, is crucial for
draw separate samples and apply the appropriate procedure to obtaining reliable crude oil pour point results.
each sample.
X1.2.2 In order to achieve complete solubility of the wax,
X1.1.4 For crude oils, care in sampling is particularly heat crude oil samples to a temperature above the wax cloud
necessary because: point. This value is seldom known however. As a rule of
X1.1.4.1 They contain volatile material, hence loss by thumb, a temperature of 20 °C above the expected pour point
evaporation can occur. will usually satisfy the cloud point requirement, although
X1.1.4.2 They contain water or sediment, or both, which exceptions do occur.
tends to separate in the sample container.
X1.2.3 The vast majority of crude oils show a significant
X1.1.4.3 If not maintained at a sufficiently high vapor pressure even at ambient temperatures. Dead crude is
temperature, wax deposition at the walls of the container or usually stabilized at a vapor pressure of 50 kPa (Test Method
wax precipitation can occur. D323, RVP at 37.8 °C) or below. However, occasionally, high
X1.1.5 When making up composite samples, exercise care RVP crudes (80 kPa) are produced and marketed. Before
not to lose light ends and to ensure homogeneity of the testing, never subject a crude oil sample to a temperature
composing samples. higher than 60 °C or to a temperature above the bubble point

8
D5853 − 24
(vapor pressure ≥100 kPa). As a rule of thumb, the vapor (X1.2.3). Opening the container may induce foaming with
pressure doubles for every 20 °C increase in temperature. resultant spillage of sample and possible injury to personnel.)
Mixing can be accomplished by a mechanical shaker or by
X1.3 Homogenization of Samples vigorous manual shaking. Although the use of (high speed)
X1.3.1 The proper means and effectiveness of mixing in mixers or similar devices might be effective, it will require that
order to achieve homogeneity depend, in addition to the the container be open for some time, during which the escape
physical properties (for example, viscosity) of the crude oil, on of light ends can be excessive, and hence, this procedure is not
the capacity and shape of the container in which the crude oil recommended. (Warning—During this operation significant
arrives at the laboratory. It is virtually impossible to cater to amounts of highly flammable vapors might escape. Vent in a
every possibility and achieve optimum results under all cir- safe area.)
cumstances. Guidelines are provided which in actual practice X1.3.4 Bottles—Follow as described in X1.3.3. Exercise
have proven to achieve the best possible results for the most special care when heating bottles that are closed with a cork or
common situations. rubber stopper. The pressure buildup due to the heating will
X1.3.2 Drums, 15 L to 200 L—The most effective way of inevitably blow out the stopper. Take proper measures to
achieving homogenization is mixing the contents of the drum safeguard against such an event. (Warning—Before embark-
on a roller bank in a hot room kept at a temperature between ing on any heating or mixing procedure, or both, ensure that the
40 °C and 60 °C for 48 h (X1.2.3). Alternatively, keep the bottles and closures can withstand the expected pressure
drum at a temperature of 20 °C above the expected pour point buildup and can be handled safely without leakage.)
for 48 h (X1.2.3) and roll the drum for at least 15 min before (Warning—Exercise care when opening the container, as
taking a sample. If heating of the drum is not feasible, the only significant vapor pressure will have built up (X1.2.3). Opening
alternative is extensive rolling for at least 30 min to disperse the container may induce foaming with resultant spillage of
the wax and wax particles as effectively as possible. In order to sample and possible injury to personnel.)
avoid the cumbersome procedure of (re)mixing the contents of X1.3.5 Plastic Containers—The use of plastic containers
large sample containers, it is recommended to draw an ad- for crude oil samples is strongly discouraged for a number of
equate number of subsamples in smaller containers, using reasons (X1.1.7). If such a container is offered to the
Practice D4057 as a guide (X1.1.3 – X1.1.7). (Warning— laboratory, however, the only way to handle these containers is
Before embarking on any heating or mixing procedure, or both, by heating to a temperature 20 °C above the expected pour
ensure that the drum and plugs can withstand the expected point (X1.2.1 – X1.2.3) in a water bath kept at the appropriate
pressure build-up and can be handled safely without leakage.) temperature. The water bath prevents localized high tempera-
(Warning—Exercise care when opening the container, as tures in the container, which can create weak sections increas-
significant vapor pressure will have built up (X1.2.3). Opening ing the possibility of rupture. In any case, rupture of these
the container may induce foaming with resultant spillage of containers due to pressure buildup is a distinct possibility and
sample and possible injury to personnel.) adequate measures must be taken to ensure safety. (Warning—
X1.3.3 Tins, 1 L to 15 L—Store the container at a tempera- Exercise care when opening the container, as significant vapor
ture 20 °C above the expected pour point (X1.2.1) preferably in pressure will have built up (X1.2.3). Opening the container
a water bath kept at the appropriate temperature. Alternatively, may induce foaming with resultant spillage of sample and
store the container in an explosion-proof oven, bearing in mind possible injury to personnel.)
that local surface temperatures might be much higher than the X1.3.6 Sample Receivers (Practice D4177)—Follow the
oven temperature reading indicates. The time required to prescribed sample mixing and handling procedure as described
dissolve the wax will depend on the type of wax and the size in Practice D4177. It is recommended that a 1 L (tin)
of the container. For a 1 L tin, 2 h has been found to be subsample be taken concurrently with subsampling for density
adequate. For larger tins, longer times will be required. and water and sediment, provided that the sample receiver has
Although it is strongly recommended that the containers be not been below the crude oil cloud point for more than 6 h. If
closed when heated, it is advised that after approximately the container has been kept at a temperature below the cloud
30 min, the excess pressure is slowly released before continu- point for more then 6 h, reheat the container to a temperature
ing the heating. (Warning—Exercise care when opening the 20 °C above the expected pour point (X1.2.1 – X1.2.3) before
container, as significant vapor pressure will have built up mixing and subsampling.

9
D5853 − 24
SUMMARY OF CHANGES

Subcommittee D02.07 has identified the location of selected changes to this standard since the last issue
(D5853 – 17a) that may impact the use of this standard. (Approved May 1, 2024.)

(1) Added Terminology D4175 to Sections 2 and 3.

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