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ASTM D7397-07

(Test Method)

Standard Test Method for Cloud Point of Petroleum Products (Miniaturized Optical Method)

Standard Test Method for Cloud Point of Petroleum Products (Miniaturized Optical Method)

SCOPE
1.1 This test method covers the determination of the cloud point of petroleum products and biodiesel fuels that are transparent in layers 40 mm in thickness by an automatic instrument.
1.2 This test method covers the range of temperatures from -60 to +20°C with temperature resolution of 0.1C; however, the range of temperatures included in the 2006 interlaboratory cooperative test program only covered the temperature range of -35 to +12°C. See Section .
1.4 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.

General Information

Status
Historical
Publication Date
31-Oct-2007
ICS
75.080 - Petroleum products in general
Technical Committee
D02 - Petroleum Products, Liquid Fuels, and Lubricants
Drafting Committee
D02.07 - Flow Properties
Current Stage
Ref Project

Relations

Replaced By
ASTM D7397-08 - Standard Test Method for Cloud Point of Petroleum Products (Miniaturized Optical Method)
Effective Date
15-Oct-2008
Referred By
ASTM D6751-23a - Standard Specification for Biodiesel Fuel Blendstock (B100) for Middle Distillate Fuels
Effective Date
01-Nov-2007
Referred By
ASTM D7467-20a - Standard Specification for Diesel Fuel Oil, Biodiesel Blend (B6 to B20)
Effective Date
01-Nov-2007

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ASTM D7397-07 - Standard Test Method for Cloud Point of Petroleum Products (Miniaturized Optical Method)ASTM D7397-07 - Standard Test Method for Cloud Point of Petroleum Products (Miniaturized Optical Method)
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ASTM D7397-07 - Standard Test Method for Cloud Point of Petroleum Products (Miniaturized Optical Method)
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NOTICE: This standard has either been superseded and replaced by a new version or withdrawn.
Contact ASTM International (www.astm.org) for the latest information
An American National Standard
Designation: D 7397 – 07
Standard Test Method for
Cloud Point of Petroleum Products (Miniaturized Optical
Method)
This standard is issued under the fixed designation D 7397; 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.
1. Scope 3. Terminology
1.1 This test method covers the determination of the cloud 3.1 Definitions:
point of petroleum products and biodiesel fuels that are 3.1.1 biodiesel, n—fuel comprising mono-alkyl esters of
transparent in layers 40 mm in thickness by an automatic long-chain fatty acids derived from vegetable oils or animal
instrument. fats, designated B100.
1.2 This test method covers the range of temperatures from 3.1.1.1 Discussion—Biodiesel is typically produced by a
–60 to +20°C with temperature resolution of 0.1°C; however, reaction of vegetable oil or animal fat with an alcohol such as
the range of temperatures included in the 2006 interlaboratory methanol or ethanol in the presence of a catalyst to yield
cooperativetestprogramonlycoveredthetemperaturerangeof mono-esters and glycerin.The fuel typically may contain up to
–35 to +12°C. See Section 13. 14differenttypesoffattyacidsthatarechemicallytransformed
1.3 The values stated in SI units are to be regarded as the into fatty acid methyl esters (FAME).
standard. The values given in parentheses are for information 3.1.2 biodiesel blend (BXX), n—blendofbiodieselfuelwith
only. petroleum-based diesel fuel designated BXX, where XX is the
1.4 This standard does not purport to address all of the volume percentage (as a whole number without the percentage
safety concerns, if any, associated with its use. It is the sign) of biodiesel.
responsibility of the user of this standard to establish appro- 3.1.3 cloud point, n—in petroleum products and biodiesel
priate safety and health practices and determine the applica- fuels, the temperature of a liquid specimen when the smallest
bility of regulatory limitations prior to use. observable cluster of hydrocarbon crystals first occurs upon
cooling under prescribed conditions.
2. Referenced Documents
3.1.3.1 Discussion—The cloud point occurs when the tem-
2.1 ASTM Standards: perature of the specimen is low enough to cause hydrocarbon
D 2500 Test Method for Cloud Point of Petroleum Products
crystals to precipitate. In a homogeneous liquid, the cloud is
D 4057 Practice for Manual Sampling of Petroleum and always noted first at the location in the specimen where the
Petroleum Products
specimen temperature is the lowest. The cloud point is the
D 4177 Practice for Automatic Sampling of Petroleum and temperature at which the crystals first occur, regardless of their
Petroleum Products
location in the specimen, and not after extensive crystallization
D 5773 Test Method for Cloud Point of Petroleum Products has taken place. The hydrocarbon crystals that precipitate at
(Constant Cooling Rate Method)
lower temperatures are typically, but not excluded to, straight
2.2 Energy Institute Standards: chain hydrocarbons commonly called “wax crystals.”
IP 219 Test Method for Cloud Point of Petroleum Products
3.2 Definitions of Terms Specific to This Standard:
IP 446 Test Method for Cloud Point of Petroleum Products 3.2.1 miniaturized optical method, n—temperature of a
specimen, when the appearance of the cloud is determined
under the conditions of this test method.
This test method is under the jurisdiction of ASTM Committee D02 on
3.2.1.1 Discussion—The cloud point in this test method is
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
determined by an automatic instrument using a miniaturized
D02.07.0D on Wax-Related Viscometric Properties of Fuels and Oils.
test receptacle equipped with two optical fibers, one to bring
Current edition approved Nov. 1, 2007. Published December 2007.
light into the test receptacle and the other to receive light
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
scattered from the specimen.
Standards volume information, refer to the standard’s Document Summary page on
3.2.2 Peltier device, n—solid state thermoelectric device
the ASTM website.
3 constructed with dissimilar semiconductor materials and con-
Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR,
U.K., http://www.energyinst.org.uk. figured in such a way that it will transfer heat to or away from
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D7397–07
a test specimen dependent on the direction of electric current 6. Apparatus
4,5
applied to the device.
6.1 Automatic Apparatus —The automatic cloud point
apparatus described in this test method consists of a test
4. Summary of Test Method
chamber controlled by a microprocessor that is capable of
controlling the heating and cooling of the test specimen,
4.1 A specimen is cooled by a Peltier device at a rate of 30
optically observing the first appearance of a cloud of wax
6 5°C/min, while continuously being illuminated by a light
crystals and recording the temperature of the specimen de-
source. The specimen is continuously monitored by an optical
scribed in detail in Annex A1.
detector for the first appearance of a cloud of wax crystals.
6.2 The apparatus shall be equipped with a specimen
Once crystals are first detected, as manifested by an increase in
receptacle, optical detector, light source, optical fibers, digital
light level received by the optical detector, the specimen is
display, Peltier device, and a specimen temperature measuring
warmed at a rate of 15 6 5°C/min. As soon as all the crystals
device.
have re-dissolved into the liquid specimen, warming is halted
6.3 The Peltier device shall be capable of heating or cooling
and the specimen is cooled again; but this time at a slower rate
the test specimen at a rate of 3 to 35°C/min.
of 6 6 3°C/min. When crystals first appear under this slower
6.4 The temperature measuring device in the specimen
cooling rate, the temperature of the specimen is recorded to
receptacle shall be capable of measuring the temperature of the
0.1°C resolution as cloud point.
test specimen from –60 to +20°C at a resolution of 0.1°C.
NOTE 6—The apparatus described above is covered by patents. If you
5. Significance and Use
are aware of an alternative(s) to the patented items, please attach to your
ballot return a description of the alternative(s). All suggestions will be
5.1 The cloud point of petroleum products and biodiesel
considered by the committee.
fuels is an index of the lowest temperature of their utility for
certain applications. Wax crystals of sufficient quantity can
7. Reagents and Materials
plug filters used in some fuel systems.
7.1 Disposable syringe that is capable of dispensing at least
5.2 Petroleum blending operations require a precise mea-
10 6 0.5 mL per full discharge of sample into the specimen
surement of the cloud point.
receptacle.
5.3 This test method can determine the temperature of the
NOTE 7—The apparatus can also be connected to a sample supply line
test specimen at which wax crystals have formed sufficiently to
to receive new sample. The amount of sample required per analysis is the
be observed as a cloud with a resolution of 0.1°C.
same as that for the syringe injection procedure (that is, 20 6 1.0 mL per
analysis). In such cases, a disposable syringe would not be needed.
5.4 This test method provides results that are equivalent to
Test Method D 5773/IP 446. The temperature results of this
8. Sampling
test method have been found to be warmer than those of Test
8.1 Obtain a sample in accordance with Practices D 4057 or
Method D 2500/IP 219 by an average of 0.49°C; however, no
D 4177.
sample specific bias was observed.
8.2 Samples of very viscous materials may be warmed until
5.5 Similar to Test Method D 5773/IP 446, this test method
they are reasonably fluid before they are tested. However, no
determines cloud point in a shorter period of time than Test
sample should be heated more than absolutely necessary.
Method D 2500/IP 219.
8.3 The sample shall not be heated above 70°C. When the
sample is heated above 70 °C, allow the sample to cool below
NOTE 1—In cases of samples with cloud points near ambient tempera-
70°C before filtering or inserting into the apparatus.
tures, time savings may not be realized.
8.4 When moisture is present in the sample, remove the
NOTE 2—This test method eliminates most of the operator time
moisture by a method, such as filtration through dry lint-free
required of Test Method D 2500/IP 219.
filterpaper,untilthespecimenisperfectlyclear,butmakesuch
NOTE 3—The only utility required by the apparatus described in this
filtration at a temperature at least 14°C above the expected
test method is electricity with power consumption of approximately 20
watts. The electric power can come from an alternating current source cloud point.
(wall receptacle) or direct current source such as a battery or a cigarette
NOTE 8—Moisture will be noticed in the sample as a separate phase or
lighter plug in a vehicle.
as a haze throughout the entire sample. Generally, a slight haze will not
NOTE 4—The apparatus described by this test method can be made
interfere with the detection of the wax cloud.
much smaller and lighter than that of Test Methods D 5773/IP 446 and
D 2500/IP 219, allowing full portability.
9. Preparation of Apparatus
NOTE 5—The apparatus used in the 2006 interlaboratory study weighed
9.1 Prepare the instrument for operation in accordance with
approximately 1 kg and occupied the space of a small lunch box. See
the manufacturer
...

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5.1 The flash point temperature is one measure of the tendency of the test specimen to form a flammable mixture with air under controlled laboratory conditions. It is only one of a number of properties which must be considered in assessing the overall flammability hazard of a material.  
5.2 Flash point is used in shipping and safety regulations to define flammable and combustible materials and for classification purposes. This definition may vary from regulation to regulation. Consult the particular regulation involved for precise definitions of these classifications.  
5.3 This test method can be used to measure and describe the properties of materials in response to heat and an ignition source under controlled laboratory conditions and shall not be used to describe or appraise the fire hazard or fire risk of materials under actual fire conditions. However, results of this test method may be used as elements of a fire risk assessment, which takes into account all of the factors which are pertinent to an assessment of the fire hazard of a particular end use.  
5.4 Flash point can also indicate the possible presence of highly volatile and flammable materials in a relatively nonvolatile or nonflammable material, such as the contamination of lubricating oils by small amounts of diesel fuel or gasoline. This test method was designed to be more sensitive to potential contamination than Test Method D6450.
SCOPE
1.1 This test method covers the determination of the flash point of fuels including diesel/biodiesel blends, lube oils, solvents, and other liquids by a continuously closed cup tester utilizing a specimen size of 2 mL, cup size of 7 mL, with a heating rate of 2.5 °C per minute.  
1.1.1 Apparatus requiring a specimen size of 1 mL, cup size of 4 mL, and a heating rate of 5.5 °C per minute must be run according to Test Method D6450.  
1.2 This flash point test method is a dynamic method and depends on definite rates of temperature increase. It is one of the many flash point test methods available and every flash point test method, including this one, is an empirical method.
Note 1: Flash point values are not a constant physical chemical property of materials tested. They are a function of the apparatus design, the condition of the apparatus used, and the operational procedure carried out. Flash point can, therefore, only be defined in terms of a standard test method and no general valid correlation can be guaranteed between results obtained by different test methods or where different test apparatus is specified.  
1.3 This test method utilizes a closed but unsealed cup with air injected into the test chamber.  
1.4 The precision of this test method is applicable for testing samples with a flash point from 22.5 °C to 235.5 °C. Determinations below and above this range may be performed; however, the precision has not been established.  
1.5 If the user’s specification requires a defined flash point method other than this method, neither this method nor any other test method should be substituted for the prescribed test method without obtaining comparative data and an agreement from the specifier.  
1.6 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard. Temperatures are in degrees Celsius, pressure in kilo-Pascals.  
1.7 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific warning statements, see 7.2 and 8.5.  
1.8 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 th...

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ASTM
ASTM D665-23(Test Method)
Standard Test Method for Rust-Preventing Characteristics of Inhibited Mineral Oil in the Presence of Water

SIGNIFICANCE AND USE
5.1 In many instances, such as in the gears of a steam turbine, water can become mixed with the lubricant, and rusting of ferrous parts can occur. This test indicates how well inhibited mineral oils aid in preventing this type of rusting. This test method is also used for testing hydraulic and circulating oils, including heavier-than-water fluids. It is used for specification of new oils and monitoring of in-service oils.
Note 3: This test method was used as a basis for Test Method D3603. Test Method D3603 is used to test the oil on separate horizontal and vertical test rod surfaces, and can provide a more discriminating evaluation.
SCOPE
1.1 This test method covers the evaluation of the ability of inhibited mineral oils, particularly steam-turbine oils, to aid in preventing the rusting of ferrous parts should water become mixed with the oil. This test method is also used for testing other oils, such as hydraulic oils and circulating oils. Provision is made in the procedure for testing heavier-than-water fluids.
Note 1: For synthetic fluids, such as phosphate ester types, the plastic holder and beaker cover should be made of chemically resistant material suitable for the type of fluid tested.  
1.2 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.3 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For specific warning statements, see 7.4 – 7.6.  
1.4 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.

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ASTM
ASTM D2425-23(Test Method)
Standard Test Method for Hydrocarbon Types in Middle Distillates by Mass Spectrometry

SIGNIFICANCE AND USE
5.1 A knowledge of the hydrocarbon composition of process streams and petroleum products boiling within the range of 160 °C to 343 °C (320 °F to 650 °F) is useful in following the effect of changes in process variables, diagnosing the source of plant upsets, and in evaluating the effect of changes in composition on product performance properties.  
5.2 A test method to determine total cycloparafins and low level aromatic content is necessary to meet specifications for aviation turbine fuel containing synthesized hydrocarbons.
SCOPE
1.1 This test method covers an analytical scheme using the mass spectrometer to determine the hydrocarbon types present in conventional and synthesized hydrocarbons that have a boiling range of 160 °C to 343 °C (320 °F to 650 °F), 5 % to 95 % by volume as determined by Test Method D86. Samples with average carbon number value of paraffins between C12 and C16 and containing paraffins from C10 and C18 can be analyzed. Eleven hydrocarbon types are determined. These include: paraffins, noncondensed cycloparaffins, condensed dicycloparaffins, condensed tricycloparaffins, alkylbenzenes, indans or tetralins, or both, CnH 2n-10 (indenes, etc.), naphthalenes, CnH2n-14  (acenaphthenes, etc.), CnH 2n-16 (acenaphthylenes, etc.), and tricyclic aromatics.  
Note 1: This test method was developed on Consolidated Electrodynamics Corporation Type 103 Mass Spectrometers. Operating parameters for users with a Quadrupole Mass Spectrometer are provided.  
1.2 This test method is intended for use with full boiling range products that contain no significant olefin content.
Biodiesel (FAME components) could interfere with the separation of the sample and the characteristic mass fragments of FAME compounds are not defined in the procedure.
Hydrocarbons containing tertiary carbon fragments, sometimes found in synthetic aviation fuels, will interfere with the characteristic mass fragments of paraffins and result in a false, elevated cycloparaffin content.
Note 2: “No significant olefin content” for this method means D1319.  
1.3 The values stated in SI units are to be regarded as standard. The values given in parentheses after SI units are provided for information only and are not considered standard.  
1.4 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, health, and environmental practices and determine the applicability of regulatory limitations prior to use. For a specific warning statement, see 11.1.  
1.5 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.

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