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ASTM D6749-02(2012)

(Test Method)

Standard Test Method for Pour Point of Petroleum Products (Automatic Air Pressure Method)

Standard Test Method for Pour Point of Petroleum Products (Automatic Air Pressure Method)

SIGNIFICANCE AND USE
5.1 The pour point of a petroleum product is an index of the lowest temperature of its utility for certain applications. Flow characteristics, like pour point, can be critical for the correct operation of lubricating systems, fuel systems, and pipeline operations.  
5.2 Petroleum blending operations require precise measurement of the pour point.  
5.3 Test results from this test method can be determined at either 1 or 3°C intervals.  
5.4 This test method yields a pour point in a format similar to Test Method D97/IP 15 when the 3°C interval results are reported. However, when specification requires Test Method D97/IP 15, do not substitute this test method.Note 2—Since some users may wish to report their results in a format similar to Test Method D97/IP 15 (in 3°C intervals), the precision data were derived for the 3°C intervals. For statements on bias relative to Test Method D97/IP 15, see 13.3.1.  
5.5 This test method has better repeatability and reproducibility relative to Test Method D97/IP 15 as measured in the 1998 interlaboratory test program (see Section 13).
SCOPE
1.1 This test method covers the determination of pour point of petroleum products by an automatic apparatus that applies a slightly positive air pressure onto the specimen surface while the specimen is being cooled.  
1.2 This test method is designed to cover the range of temperatures from −57 to +51°C; however, the range of temperatures included in the (1998) interlaboratory test program only covered the temperature range from −51 to −11°C.  
1.3 Test results from this test method can be determined at either 1 or 3°C testing intervals.  
1.4 This test method is not intended for use with crude oils.Note 1—The applicability of this test method on residual fuel samples has not been verified. For further information on the applicability, refer to 13.4.  
1.5 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.  
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

General Information

Status
Historical
Publication Date
31-Oct-2012
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

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Replaced By
ASTM D6749-02(2018) - Standard Test Method for Pour Point of Petroleum Products (Automatic Air Pressure Method)
Effective Date
01-May-2018

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ASTM D6749-02(2012) - Standard Test Method for Pour Point of Petroleum Products (Automatic Air Pressure 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
Designation: D6749 − 02 (Reapproved 2012)
Standard Test Method for
Pour Point of Petroleum Products (Automatic Air Pressure
Method)
This standard is issued under the fixed designation D6749; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision.Anumber 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 D4057Practice for Manual Sampling of Petroleum and
Petroleum Products
1.1 This test method covers the determination of pour point
D4177Practice for Automatic Sampling of Petroleum and
of petroleum products by an automatic apparatus that applies a
Petroleum Products
slightly positive air pressure onto the specimen surface while
2.2 Energy Institute Standard:
the specimen is being cooled.
IP 15Test Method for Pour Point of Petroleum Products
1.2 This test method is designed to cover the range of
temperatures from −57 to +51°C; however, the range of
3. Terminology
temperatures included in the (1998) interlaboratory test pro-
3.1 Definitions:
gram only covered the temperature range from −51 to −11°C.
3.1.1 pour point, n—in petroleum products,lowesttempera-
1.3 Test results from this test method can be determined at
tureatwhichmovementofthetestspecimenisobservedunder
either 1 or 3°C testing intervals.
prescribed conditions of test.
1.4 This test method is not intended for use with crude oils.
3.2 Definitions of Terms Specific to This Standard:
NOTE 1—The applicability of this test method on residual fuel samples
3.2.1 air pressure, n—regulated slightly positive air pres-
has not been verified. For further information on the applicability, refer to
sure gently applied onto the specimen surface in the airtight
13.4.
test jar that causes upward movement of the specimen in the
1.5 The values stated in SI units are to be regarded as
communicating tube, which has one end inserted into the test
standard. No other units of measurement are included in this
specimen and the other end at atmospheric pressure.
standard.
3.2.2 no-flow point, n—in petroleum products, temperature
1.6 This standard does not purport to address all of the
ofthetestspecimenatwhichawaxcrystalstructureofthetest
safety concerns, if any, associated with its use. It is the
specimen or viscosity increase, or both, impedes movement of
responsibility of the user of this standard to establish appro-
thesurfaceofthetestspecimenundertheconditionsofthetest.
priate safety and health practices and determine the applica-
3.2.2.1 Discussion—The no-flow point occurs when, upon
bility of regulatory limitations prior to use.
cooling, the formation of wax crystal structures or viscosity
increase,orboth,hasprogressedtothepointwheretheapplied
2. Referenced Documents
observation device no longer detects movement under the
2.1 ASTM Standards:
conditions of the test. The preceding observation temperature,
D97Test Method for Pour Point of Petroleum Products
at which flow of the test specimen is last observed, is the pour
point.
This test method is under the jurisdiction of ASTM Committee D02 on
PetroleumProductsandLubricantsandisthedirectresponsibilityofSubcommittee
4. Summary of Test Method
D02.07 on Flow Properties.
Current edition approved Nov. 1, 2012. Published November 2012. Originally 4.1 After inserting the test jar containing the specimen into
approved in 2002. Last previous edition approved in 2007 as D6749–02 (2007).
the automatic pour point apparatus and initiating the test
DOI: 10.1520/D6749-02R12.
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
Standards volume information, refer to the standard’s Document Summary page on Available from Energy Institute, 61 New Cavendish St., London, WIG 7AR,
the ASTM website. U.K., http://www.energyinst.org.uk.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States
D6749 − 02 (2012)
program, the specimen is automatically heated to the desig- ing and reporting the pour point (see Fig. 1). The detail is
nated temperature and then cooled at a controlled rate. At described in Annex A1.
temperature intervals of 1 or 3°C, depending on the selection
6.2 Test Jar, clear cylindrical glass with a flat bottom with
made by the user prior to the test, a slightly positive air
an approximate capacity of 12 mL. Approximately 4.5 mL of
pressure is gently applied onto the surface of the specimen
sample specimen is contained when filled to the scribed line.
which is contained in an airtight test jar equipped with a
The test jar is fitted with a test jar cap assembly on its top to
communicatingtube.Sinceoneendofthecommunicatingtube
form an air chamber over the test specimen.
is inserted into the specimen while the other end is maintained
6.3 Test Jar Cap Assembly—Aplasticcapisinstalledontop
at atmospheric pressure, a small amount of downward move-
ofthetestjarwiththeprovisionofsealingair.Aglasstubewith
ment or deformation of the specimen surface, as a result of the
a metallic tip shall be inserted from underneath the plastic cap
application of air pressure, is observed by means of upward
intotheroundholeinthecenterofthetestjarcap.Thetopend
movement of the specimen in the communicating tube. This
oftheroundholeisconnectedtoanairpressuresensorbyway
upward movement of the specimen is detected by a pressure
of a vinyl tube. To supply air pressure to the specimen’s
sensor which is installed at the atmospheric end of the
surface, a vinyl tube connected to an air syringe is located
communicating tube. The lowest temperature at which defor-
adjacent to the glass tube through an orifice in the plastic cap.
mation of the specimen is observed upon application of air
When a specimen is to be tested, the test jar cap assembly is
pressure is recorded as the pour point in accordance with Test
installed on the test jar with the lower end of the glass tube
Method D6749.
insertedintothespecimeninthetestjar.Theglasstubeandthe
test jar form a communicating tube.Atemperature sensor in a
5. Significance and Use
smalldiametermetallicsheathshallbeinstalledinthecenterof
5.1 Thepourpointofapetroleumproductisanindexofthe
the glass tube.
lowest temperature of its utility for certain applications. Flow
6.4 Metallic Block Bath, a metallic block with a cylindrical
characteristics, like pour point, can be critical for the correct
hole to fit the test jar. The metallic block assembly shall have
operation of lubricating systems, fuel systems, and pipeline
operations.
5.2 Petroleum blending operations require precise measure-
ment of the pour point.
5.3 Test results from this test method can be determined at
either 1 or 3°C intervals.
5.4 This test method yields a pour point in a format similar
to Test Method D97/IP 15 when the 3°C interval results are
reported. However, when specification requires Test Method
D97/IP 15, do not substitute this test method.
NOTE 2—Since some users may wish to report their results in a format
similar to Test Method D97/IP 15 (in 3°C intervals), the precision data
were derived for the 3°C intervals. For statements on bias relative to Test
Method D97/IP 15, see 13.3.1.
5.5 This test method has better repeatability and reproduc-
ibility relative to Test Method D97/IP 15 as measured in the
1998 interlaboratory test program (see Section 13).
6. Apparatus
4,5
6.1 Automatic Apparatus —The automatic pour point ap-
paratus described in this test method is a microprocessor
controlled apparatus that is capable of heating and cooling a
specimen, applying air pressure onto the specimen’s surface,
detecting the specimen’s surface movement, and then comput-
Thesolesourceofsupplyoftheapparatusknowntothecommitteeatthistime
isTanaka model MPC series Pour PointAnalyzers available fromTanaka Scientific
Limited,Adachiku, Tokyo, Japan. Various models included in this model series are
differentiatedbytheircoolingcapacitiesornumberoftestheads,orboth.Ifyouare
aware of alternative suppliers, please provide this information to ASTM Interna-
tional Headquarters.Your comments will receive careful consideration at a meeting
of the responsible technical committee, which you may attend.
This pour point analyzer is covered by a patent. If you are aware of an
alternative(s) to the patented item, please attach to your ballot return a description
of the alternatives. All the suggestions will be considered by the committee. FIG. 1 Automatic Apparatus
D6749 − 02 (2012)
a provision for cooling/heating. A temperature sensor is em- thenentertheexpectedpourpoint(EPP).Whenthe3°Ctesting
bedded in the metallic block to monitor its temperature. interval is chosen, the EPP needs to be a multiple of 3°C.
11.4 Start the test program. The sample is automatically
7. Reagents and Materials
preheatedbytheautomaticapparatusto45°CortoEPP+9°C,
7.1 Cleaning Agents,capableofcleaninganddryingthetest
whichever is higher, but no higher than 70°C, by maintaining
jar,temperaturesensor,andglasstubeaftereachtest.Chemical
the bath temperature at 48°C or EPP + 12°C, whichever is
agents such as alcohol, petroleum-based solvents, and acetone
higher.
have been found suitable to use. ( Warning—Flammable.)
11.5 After the preheating is completed, the specimen is
(Warning—May be harmful by itself or when evaporated.)
cooled down automatically.
11.5.1 The metallic block bath is cooled down at a rate of 3
8. Sampling
to 4°C/min, to the EPP + 40°C.
8.1 Obtain a sample in accordance with Practice D4057 or
11.5.2 From the EPP + 40°C to the no-flow point, the
by Practice D4177.
metallic block bath is cooled at a rate of 0.8 to 1.1°C/min.
8.2 Samples of very viscous materials may be warmed until
11.6 As the specimen temperature reaches a predetermined
they are reasonably fluid before they are transferred; however,
temperature, which is dependent on the EPP, the automatic
no sample shall be heated more than is absolutely necessary.
apparatus starts testing for no-flow state by applying air
The sample shall not be heated and transferred into the test jar
pressure to the specimen surface at the programmed testing
unless its temperature is 70°C or lower.
interval. When the specimen is still in a fluid state, the
NOTE 3—In the event the sample has been heated above this
specimen level moves up in the glass tube as air pressure is
temp
...

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ASTM
ASTM D4175-23a(Terminology)
Standard Terminology Relating to Petroleum Products, Liquid Fuels, and Lubricants

SCOPE
1.1 This terminology standard covers the compilation of terminology developed by Committee D02 on Petroleum Products, Liquid Fuels, and Lubricants, except that it does not include terms/definitions specific only to the standards in which they appear.  
1.1.1 The terminology, mostly definitions, is unique to petroleum, petroleum products, lubricants, and certain products from biomass and chemical synthesis. Meanings of the same terms outside of applications to petroleum, petroleum products, and lubricants can be found in other compilations and in dictionaries of general usage.  
1.1.2 The terms/definitions exist in two places:  (1) in the standards in which they appear and (2) in this compilation.  
1.2 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 D86-23ae1(Test Method)
Standard Test Method for Distillation of Petroleum Products and Liquid Fuels at Atmospheric Pressure

SIGNIFICANCE AND USE
5.1 The basic test method of determining the boiling range of a petroleum product by performing a simple batch distillation has been in use as long as the petroleum industry has existed. It is one of the oldest test methods under the jurisdiction of ASTM Committee D02, dating from the time when it was still referred to as the Engler distillation. Since the test method has been in use for such an extended period, a tremendous number of historical data bases exist for estimating end-use sensitivity on products and processes.  
5.2 The distillation (volatility) characteristics of hydrocarbons have an important effect on their safety and performance, especially in the case of fuels and solvents. The boiling range gives information on the composition, the properties, and the behavior of the fuel during storage and use. Volatility is the major determinant of the tendency of a hydrocarbon mixture to produce potentially explosive vapors.  
5.3 The distillation characteristics are critically important for both automotive and aviation gasolines, affecting starting, warm-up, and tendency to vapor lock at high operating temperature or at high altitude, or both. The presence of high boiling point components in these and other fuels can significantly affect the degree of formation of solid combustion deposits.  
5.4 Volatility, as it affects rate of evaporation, is an important factor in the application of many solvents, particularly those used in paints.  
5.5 Distillation limits are often included in petroleum product specifications, in commercial contract agreements, process refinery/control applications, and for compliance to regulatory rules.
SCOPE
1.1 This test method covers the atmospheric distillation of petroleum products and liquid fuels using a laboratory batch distillation unit to determine quantitatively the boiling range characteristics of such products as light and middle distillates, automotive spark-ignition engine fuels with or without oxygenates (see Note 1), aviation gasolines, aviation turbine fuels, diesel fuels, biodiesel blends up to 30 % volume, marine fuels, special petroleum spirits, naphthas, white spirits, kerosines, and Grades 1 and 2 burner fuels.
Note 1: An interlaboratory study was conducted in 2008 involving 11 different laboratories submitting 15 data sets and 15 different samples of ethanol-fuel blends containing 25 % volume, 50 % volume, and 75 % volume ethanol. The results indicate that the repeatability limits of these samples are comparable or within the published repeatability of the method (with the exception of FBP of 75 % ethanol-fuel blends). On this basis, it can be concluded that Test Method D86 is applicable to ethanol-fuel blends such as Ed75 and Ed85 (Specification D5798) or other ethanol-fuel blends with greater than 10 % volume ethanol. See ASTM RR:D02-1694 for supporting data.2  
1.2 The test method is designed for the analysis of distillate fuels; it is not applicable to products containing appreciable quantities of residual material.  
1.3 This test method covers both manual and automated instruments.  
1.4 Unless otherwise noted, the values stated in SI units are to be regarded as the standard. The values given in parentheses are provided for information only.  
1.5 WARNING—Mercury has been designated by many regulatory agencies as a hazardous substance that can cause serious medical issues. Mercury, or its vapor, has been demonstrated to be hazardous to health and corrosive to materials. Use Caution when handling mercury and mercury-containing products. See the applicable product Safety Data Sheet (SDS) for additional information. The potential exists that selling mercury or mercury-containing products, or both, is prohibited by local or national law. Users must determine legality of sales in their location.  
1.6 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibilit...

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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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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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