An American National Standard

Designation: D 5773 – 03

Designation: 446/99

Standard Test Method for

Cloud Point of Petroleum Products (Constant Cooling Rate
Method)1
This standard is issued under the fixed designation D 5773; 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 describes an alternative procedure for the determination of cloud point of
petroleum products Test Method D 2500/IP219 using an automatic apparatus. The temperature results
from this test method have been found to be equivalent to Test Method D 2500/IP219. When
specification requires Test Method D 2500/IP219, do not substitute this test method or any other
method without obtaining comparative data and agreement from the specifier.

1. Scope* D 4177 Practice for Automatic Sampling of Petroleum and

1.1 This test method describes the determination of the Petroleum Products3
cloud point of petroleum products and biodiesel fuels that are 2.2 IP Standard:
transparent in layers 40 mm in thickness by an automatic IP219 Test Method for Cloud Point of Petroleum Products4
instrument using a constant cooling rate. 3. Terminology
1.2 This test method covers the range of temperatures from
−60 to +49°C with temperature resolution of 0.1°C, however, 3.1 Definitions:
the range of temperatures included in the 1997 interlaboratory 3.1.1 biodiesel, n—a fuel comprised of mono-alkyl esters of
cooperative test program only covered the temperature range of long-chain fatty acids derived from vegetable oils or animal
–56 to +34°C. fats, designated B100.
1.3 The values stated in SI units are to be regarded as the 3.1.1.1 Discussion—Biodiesel is typically produced by a
standard. The values given in parentheses are for information reaction of vegetable oil or animal fat with an alcohol such as
only. methanol or ethanol in the presence of a catalyst to yield
1.4 This standard does not purport to address all of the mono-esters and glycerin. The fuel typically may contain up to
safety concerns, if any, associated with its use. It is the 14 different types of fatty acids that are chemically transformed
responsibility of the user of this standard to establish appro- into fatty acid methyl esters (FAME).
priate safety and health practices and determine the applica- 3.1.2 biodiesel blend, n—a blend of biodiesel fuel with
bility of regulatory limitations prior to use. petroleum-based diesel fuel designated BXX, where XX is the
volume percentage of biodiesel.
2. Referenced Documents 3.1.3 cloud point, n—in petroleum products and biodiesel
2.1 ASTM Standards: fuels, the temperature of a liquid specimen when a wax crystal
D 2500 Test Method for Cloud Point of Petroleum Prod- structure that is similar in appearance to a cloud is formed upon
ucts2 cooling under prescribed conditions.
D 4057 Practice for Manual Sampling of Petroleum and 3.1.3.1 Discussion—The cloud point appears when the tem-
Petroleum Products3 perature of the specimen is low enough to cause wax crystals
to precipitate. In a homogeneous liquid, the cloud is always
noted first at the location in the specimen where the specimen
1
temperature is the lowest. This is typically at the lower portion
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
of the test jar when using the apparatus described in Test
D02.07 on Flow Properties. Method D 2500.
Current edition approved July 10, 2003. Published August 2003. Originally
approved in 1995. Last previous edition approved in 2002 as D 5773–02.
2 4
Annual Book of ASTM Standards, Vol 05.01. Available from the Institute of Petroleum, 61 New Cavendish Street, London,
3
Annual Book of ASTM Standards, Vol 05.02. England WIM 8AR.

*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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 D 5773 – 03
3.2 Definitions of Terms Specific to This Standard: 5.6 This test method eliminates most of the operator time
3.2.1 automatic cloud point, n—the temperature of a speci- required of Test Method D 2500.
men, when the appearance of the cloud is determined under the 5.7 This test method does not require the use of a mechani-
conditions of this test method. cal refrigeration apparatus.
3.2.1.1 Discussion—The cloud point in this test method is NOTE 3—In certain cases of high ambient temperature, a source of
determined by an automatic instrument using an optical device cooling water may be required to measure low temperature cloud points
for detection of the crystal formation. The apparatus and the (see 7.1).
conditions are different from those established for Test Method
D 2500, although according to interlaboratory examination, the 6. Apparatus
results have been determined to be equivalent to Test Method 6.1 Automatic Apparatus5—The automatic cloud point ap-
D 2500. paratus described in this test method consists of a test chamber
3.2.2 D 2500/IP219 equivalent cloud point, n—the tem- controlled by a microprocessor that is capable of controlling
perature of a specimen, in integers, calculated by rounding the the heating and cooling of the test specimen, optically observ-
results of this test method to the next lower integer. ing the first appearance of a cloud of wax crystals and
3.2.2.1 Discussion—This test method produces results with recording the temperature of the specimen described in detail
0.1°C resolution. Should the user wish to provide results with in Annex A1.
a similar format to Test Method D 2500, then this calculation 6.2 The apparatus shall be equipped with a specimen cup,
can be performed. Some apparatus can perform this calculation optical detector array, light source, digital display, Peltier
automatically. device, and a specimen temperature measuring device.
3.2.3 Peltier device, n—a solid state thermoelectric device 6.3 The Peltier device shall be capable of heating or cooling
constructed with dissimilar semiconductor materials and con- the test specimen at a constant rate of 1.5 6 0.1°C/min.
figured in such a way that it will transfer heat to or away from 6.4 The temperature measuring device in the specimen cup
a test specimen dependent on the direction of electric current shall be capable of measuring the temperature of the test
applied to the device. specimen from −40 to +70°C at a resolution of 0.1°C.
6.5 The apparatus shall be equipped with fittings to permit
4. Summary of Test Method the circulation of a liquid cooling medium, if required, to
4.1 A specimen is cooled by a Peltier device at a constant remove heat generated by the Peltier device and other elec-
rate of 1.5 6 0.1°C/min while continuously being illuminated tronic components of the apparatus.
by a light source. The specimen is continuously monitored by NOTE 4—Some apparatus are designed to use ambient air as a cooling
an array of optical detectors for the first appearance of a cloud medium. In such cases, a built-in fan is available to provide circulation of
of wax crystals. The detectors are sufficient in number to air and there is no need for fittings as described for a liquid cooling
ensure that any solid phase hydrocarbon crystals that may form medium. The function of the cooling medium is to remove heat from the
are detected. The temperature at which the appearance of a electronic components. The choice of the cooling medium has no impact
whatsoever on the test results.
cloud of wax crystals is first detected in the specimen is
recorded to 0.1°C resolution. When the recorded temperature is 6.6 The apparatus shall be equipped with fittings to permit
rounded to the next lower integer temperature, it is designated the circulation of purge gas to purge the test chamber contain-
as the D 2500/IP 219 equivalent cloud point per Test Method ing the specimen cup of any atmospheric moisture.
D 5773.
7. Reagents and Materials
5. Significance and Use 7.1 Cooling Medium—Air, tap water, or other liquid heat
5.1 The cloud point of petroleum products and biodiesel exchange medium sufficient to remove heat generated by the
fuels is an index of the lowest temperature of their utility for Peltier device and other electronic components from the
certain applications. Wax crystals of sufficient quantity can apparatus. To achieve specimen cooling to −40°C, supply
plug filters used in some fuel systems. circulation of liquid cooling medium at +25°C or lower to the
5.2 Petroleum blending operations require a precise mea- apparatus. For an apparatus which relies on air as cooling
surement of the cloud point. medium, the ambient air temperature has to be below +30°C to
5.3 This test method can determine the temperature of the achieve specimen cooling to −40°C.
test specimen at which wax crystals have formed sufficiently to 7.2 Purge Gas—A gas such as air, nitrogen, helium, or
be observed as a cloud with a resolution of 0.1°C. argon with a dew point below the lowest operating temperature
5.4 This test method provides results that are equivalent to
Test Method D 2500.
5
The sole source of supply of the Phase Technology Cloud Point Analyzer model
NOTE 1—This is based on the Test Method D 2500 equivalent cloud series 10, 30, and 70 known to the committee at this time is Phase Technology,
point in which the 0.1°C result is rounded to the next lower integer. #135-11960 Hammersmith Way, Richmond, B.C. Canada V7A 5C9. The various
model series mentioned above are differentiated by their cooling capacities;
5.5 This test method determines the cloud point in a shorter however, all of them are capable of covering the entire temperature range specified
period of time than Test Method D 2500. in the scope. If you are aware of alternative suppliers, please provide this
information to ASTM International Headquarters. Your comments will receive
NOTE 2—In cases of samples with cloud points near ambient tempera- careful consideration at a meeting of the responsible technical committee,1 which
tures, time savings may not be realized. you may attend.

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 D 5773 – 03
of the analyzer. (Warning—Compressed gas under high pres- 11.5 Close and lock the test chamber lid.
sure.) (Warning—Inert gas can be an asphyxiant when in- 11.6 Select the PRE-HEAT menu on the apparatus if the
haled.) expected cloud point is less than 14°C below the specimen
7.3 Adjustable Volume Pipette, capable of dispensing 0.15 ambient temperature. The specimen ambient temperature is
6 0.01 mL of sample. displayed on the front panel of the apparatus. With this
7.4 Cotton Swabs—Plastic or paper shaft cotton swabs used selection, the apparatus will automatically heat the specimen to
to clean the sample cup. (Warning—The use of swabs with a starting temperature of 50°C prior to cooling. If the PRE-
wooden shafts may damage the mirrored surface of the HEAT menu is not selected, the apparatus will cool the
specimen cup.) specimen from ambient temperature without any initial heat-
ing. When the cloud point is expected to be higher than 35°C,
8. Sampling select a higher starting temperature according to manufactur-
8.1 Obtain a sample in accordance with Practices D 4057 or er’s instructions. The highest starting temperature that can be
D 4177. programmed is 70°C.
8.2 Samples of very viscous materials may be warmed until 11.7 Push the RUN button located on the front panel of the
they are reasonably fluid before they are tested. However, no apparatus. With the push of this button, the apparatus will
sample should be heated more than absolutely necessary. allow the flow of liquid cooling medium, if required, (see Note
8.3 The sample shall not be heated above 70°C. When the 4) and the flow of purge gas through the apparatus.
sample is heated above 70°C, allow the sample to cool below (Warning—The apparatus will display appropriate warning
70°C before filtering or inserting into the apparatus. signals if any of these flows are not properly established. Refer
8.4 When moisture is present in the sample, remove the to manufacturer’s operating manual for corrective procedures.)
moisture by a method, such as filtration through dry lint-free 11.8 The specimen is heated if specified as described in
filter paper, until the oil is perfectly clear, but make such 11.6. It is then cooled by the Peltier device while the optical
filtration at a temperature at least 14°C above the expected detectors continuously monitor the specimen for the appear-
cloud point. ance of a cloud of wax crystals. The measurement is automati-
NOTE 5—Moisture will be noticed in the sample as a separate phase or cally terminated once the cloud point is detected.
as a haze throughout the entire sample. Generally, a slight haze will not 11.9 When the measurement is complete, the automatic
interfere with the detection of the wax cloud. cloud point value per Test Method D 5773 will be displayed on
the front panel of the apparatus.
9. Preparation of Apparatus 11.10 Unlock and open the test chamber lid and clean the
9.1 Prepare the instrument for operation in accordance with specimen out of the specimen cup with a cotton swab.
the manufacturer’s instructions.
9.2 Make liquid cooling medium connections if required 12. Report
(see Note 4) and ensure that they do not leak. 12.1 Report the temperature recorded in 11.9 as the auto-
9.3 Make purge gas connections and ensure that they do not matic cloud point Test Method D 5773.
leak. 12.2 When specified, round the temperature recorded in
9.4 Turn on the liquid cooling medium if required (see Note 11.9 to the next lower integer and report as the Test Method
4). D 2500 equivalent cloud point per Test Method D 5773.
9.5 Turn on the purge gas.
9.6 Turn on the main power switch of the analyzer. After the 13. Precision and Bias
automatic self diagnostics startup sequence is completed, the 13.1 Precision—The precision of this test method as deter-
instrument will display a READY message. mined by the statistical examination of the interlaboratory test
10. Calibration and Standardization results6,7 is as follows:
13.1.1 Repeatability—The difference between successive
10.1 Ensure that all of the manufacturer’s instructions for
test results, obtained by the same operator using the same
calibrating, checking, and operating the apparatus are fol-
apparatus under constant operating conditions on identical test
lowed.
material, would in the long run, in the normal and correct
10.2 A sample with a mutually agreed upon cloud point can
operation of this test method, exceed 1.3°C only in one case in
be used to verify performance of the apparatus.
twenty.
11. Procedure 13.1.2 Reproducibility—The difference between two single
11.1 Open the test chamber lid and clean the specimen cup and independent test results, obtained by different operators
inside the test chamber with a cotton swab. working in different laboratories on identical test material,
11.2 Use a pipet to deliver 0.15 6 0.01 mL of specimen into
the specimen cup. Clean the specimen out of the cup by using
a cotton swab. The cup must be cleaned to the point where no 6
Supporting data (the results of the 1990 interlaboratory cooperative test
visible droplets of specimen remain in the cup. program) have been filed at ASTM International Headquarters and may be obtained
by requesting Research Report RR: D02-1373.
11.3 Repeat step 11.2. 7
Supporting data (the results of the 1997 interlaboratory cooperative test
11.4 Carefully measure 0.15 6 0.01 mL of specimen into program) have been filed at ASTM International Headquarters and may be obtained
the specimen cup. by requesting Research Report RR: D02–1510.

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 D 5773 – 03
would in the long run, in normal and correct operation of this comprised cloud points from about −2 to +10°C.
test method, exceed 2.5°C only in one case in twenty. 13.4.3 The precision statements were derived from a 2001
13.1.3 The precision statements were derived from a 1997 interlaboratory cooperative test program.8 Participants ana-
interlaboratory cooperative test program.6 Participants ana- lyzed eleven sample sets comprised of two petroleum distillate
lyzed eleven sample sets as blind duplicates, comprised of fuels, diesel and kerosene, with various biodiesel fuels with a
various distillate fuels and lubricating oils, and with a cloud temperature range from +10 to −45°C. Fourteen laboratories
point range of +34 to −56°C. Ten laboratories participated with participated with the automatic machines and ten laboratories
the automatic apparatus and eight laboratories participated with participated with the manual Test Method D 2500/IP219.
the manual Test Method D 2500/IP219 test method. The Information on the type of samples and their average cloud
precision statistics were compiled and calculated based on the points are in the research report.8
0.1°C resolution offered by this automatic apparatus. Informa-
tion on the type of samples and their average cloud points are NOTE 7—One of the outcomes of the interlaboratory study was the
selection of the sample types used in the study contributed to a difficulty
in the research report. in determining the precision statement. Kerosene is a sufficiently different
13.2 Bias—Since there is no accepted reference material fuel type from biodiesel to cause some slight separation of phases upon
suitable for determining the bias for the procedure in this test cooling when in B20 blends. Also, the particular kerosene sample used
method, bias has not been determined. was atypical, which complicated the study further. Therefore data from the
13.3 Relative Bias—The results of the interlaboratory pro- blends of kerosene in biodiesel were not used in the precision statement.
gram were examined for bias relative to Test Method D 2500/ In addition, the diesel fuel used in the round-robin was high cloud point
material. Due to the cloud point of the base diesel material, this
IP219. A statistically insignificant bias of −0.03°C was ob- temperature range in the precision statement was limited.
served. NOTE 8—A future interlaboratory cloud study will be done including a
13.4 Precision of Biodiesel Fuels—The precision of this test wider range of base biodiesel fuels with various distillate blend stocks.
method, as determined by the statistical examination of the
13.5 Bias of Biodiesel Fuels—Since there is no accepted
interlaboratory test results, is as follows:
reference material suitable for determining the bias for the
13.4.1 Repeatability for Blends of Biodiesel in Diesel—The procedure in this test method, bias has not been determined.
difference between successive test results, obtained by the 13.6 Relative Bias—The statistical analysis for the inter-
same operator using the same apparatus under constant oper- laboratory test program for bias relative to Test Method
ating conditions on identical test material, would, in the long D 2500/IP219 has been determined for blends of biodiesel in
run, in the normal and correct operation of this test method, diesel samples.
exceed 0.7°C only in one case in twenty.
13.4.2 Reproducibility for Blends of Biodiesel in Diesel— 14. Keywords
The difference between two single and independent test results, 14.1 automatic cloud point; cloud point; constant cooling
obtained by different operators working in different laborato- rate; Peltier; petroleum products; thermoelectric; wax crystals
ries on identical test material, would in the long run, in the
normal and correct operation of this test method, exceed 0.9°C
8
only in one case in twenty. Supporting data (the results of the 2001 interlaboratory cooperative test
program) have been filed at ASTM International Headquarters and may be obtained
NOTE 6—The precision for blends of biodiesel in diesel samples by requesting Research Report RR: D02–1524.

ANNEX

(Mandatory Information)

A1. DETAILED DESCRIPTION OF APPARATUS

A1.1 Test Chamber, comprised of optical detectors, lens, A1.1.1 Specimen Cup, comprised of black plastic wall and a
light source, specimen cup, temperature sensor, Peltier device, highly polished metal bottom. The polished surface of the
and heat sink arranged in a configuration as shown in Fig. bottom serves as a reflective surface for light. The transfer of
A1.1. The lid of the test chamber can be opened to allow heat to and away from the specimen through the metal bottom
cleaning of specimen cup and introduction of new specimen. is controlled by the Peltier device.
Once closed and locked, the chamber becomes airtight. An A1.1.2 Temperature Sensor, reading to 0.1°C, permanently
O-ring is used to seal the mating surfaces between the lid and embedded into the bottom of the specimen cup and positioned
the rest of the chamber. The air trapped in the closed chamber
less than 0.1 mm below the top surface of the cup bottom. This
is purged by dry gas. The dry gas inlet and outlet are shown in
temperature sensor, which is made of a single strand platinum,
Fig. A1.1. The test chamber wall is made of black colored
provides accurate measurement of the specimen temperature.
metal and plastic components to minimize light reflection.

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 D 5773 – 03

FIG. A1.1 Schematic of Test Chamber

A1.1.3 Peltier Device, capable of controlling the specimen the displays and buttons may vary depending on the model
temperature over a wide range. The range varies depending on series).
the model series. During specimen cooling, heat is transferred
A1.2.1 Message Display, provides information on the status
from the top of the device to the bottom. Since the top is in
of the apparatus. It displays a READY message when the
thermal contact with the bottom of the specimen cup, the
apparatus is idle and no fault is found. At the end of a test, the
specimen will be chilled. The bottom of the Peltier device is in
result is displayed. It displays a diagnostic message if a fault is
thermal contact with the heat sink where heat is dissipated to
detected in any of the major components of the apparatus.
the cooling medium. During specimen warming, the reverse
Detailed explanation of the diagnostic messages is available in
process will take place.
the manufacturer’s service manual.
A1.1.4 Light Source, to provide a beam of light with a
wavelength of 660 6 10 nm. The light source is positioned A1.2.2 Specimen Temperature Display, gives an update of
such that it provides an incident beam (Fig. A1.1) impinging the specimen temperature, recorded to 0.1°C, every 2 s.
onto the specimen at an acute angle. The light is reflected from A1.2.3 Light Signal Display, gives an update of the scat-
the polished bottom of the specimen cup. When the specimen tered light level received by the optical detectors every 2 s.
is a homogeneous liquid, the reflected beam impinges onto the This information is used by service personnel for troubleshoot-
chamber lid, which is black in color. The reflected light is then ing purposes.
absorbed by the black surface. When wax crystals appear in the A1.2.4 Menu Buttons, allow the operator to specify the
specimen, the reflected beam is scattered by the solid-liquid pre-heat requirement for the specimen.
phase boundaries. A significant amount of scattered light A1.2.5 Run Button, allows the operator to start the measure-
impinges onto the lens (Fig. A1.2). ment sequence once the specimen is put inside the test
A1.1.5 Optical Detectors, positioned above the lens to chamber.
monitor the clarity of the specimen. The distance between the A1.2.6 Reset Button, allows the operator to stop the mea-
optical detectors and the lens is adjusted such that the image of surement sequence. Upon pressing this button, the apparatus
the specimen is projected onto the light sensitive surface of the will immediately stop the measurement sequence and warm the
optical detectors. Sufficient optical detectors are used to cover specimen to about 20°C.
the image area.
NOTE A1.1—A full description, installation, setup instructions, and
A1.2 Apparatus Exterior Interface, composed of several maintenance instructions are contained within the manufacturer’s manual
displays and buttons as shown in Fig. A1.3 (the exact layout of supplied with each instrument.

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 D 5773 – 03

FIG. A1.2 Detection of Crystal Formation

FIG. A1.3 Apparatus Exterior

SUMMARY OF CHANGES

Subcommittee D02.07 has identified the location of selected changes to this standard since the last issue
(D 5773–02) that may impact the use of this standard.

(1) Revised Scope to incorporate the 1997 round robin sample (4) Revised 13.1.3 to reflect wording pertaining to the 1997
temperature range. interlaboratory test program.
(2) Incorporated the 1997 round robin repeatability. (5) Deleted Note 6, because it was redundant with the
(3) Incorporated the 1997 round robin reproducibility. completion of the 1997 cloud round robin.

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 D 5773 – 03
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