ASTM D2274-94(1999)e1
(Test Method)Standard Test Method for Oxidation Stability of Distillate Fuel Oil (Accelerated Method)
Standard Test Method for Oxidation Stability of Distillate Fuel Oil (Accelerated Method)
SCOPE
1.1 This test method measures the inherent stability of middle distillate petroleum fuels under specified oxidizing conditions at 95°C.
Note 1—Fuels used in establishing the precision measures for this test method were described as gas oil, diesel fuel, No. 2 heating oil, and DFM, a Navy distillate fuel suitable for diesels, boilers, and gas turbines. While the test method may be used for fuels outside the range of these fuels, the precision measures may not apply.
1.2 This test method is not applicable to fuels containing residual oil or significant amounts of components derived from non-petroleum sources.
1.3 The values given in acceptable SI units are to be regarded as the standard. The values in parentheses are for information only.
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.
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e1
Designation: D 2274 – 94 (Reapproved 1999) An American National Standard
Designation: 388/97
Standard Test Method for
Oxidation Stability of Distillate Fuel Oil (Accelerated
Method)
This standard is issued under the fixed designation D 2274; 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.
This standard has been approved for use by agencies of the Department of Defense.
e NOTE—Warning statements were placed in the text in November 1999.
1. Scope 3. Terminology
1.1 This test method covers the measurement of inherent 3.1 Definitions of Terms Specific to This Standard:
stability of middle distillate petroleum fuel under accelerated 3.1.1 adherent insolubles (formerly adherent gum)—
oxidizing conditions. It is not applicable to fuels containing material which is produced in the course of stressing distillate
residual oil, or any significant component derived from a fuel under the conditions of this test and which adheres to the
nonpetroleum source. glassware after fuel has been flushed from the system.
1.2 The values given in acceptable SI units are to be 3.1.2 filterable insolubles—material, which is produced in
regarded as the standard. The values in parentheses are for the course of stressing distillate fuel under the conditions of
information only. this test, which is capable of being removed from the fuel by
1.3 This standard does not purport to address all of the filtration. This includes both material suspended in the fuel and
safety concerns, if any, associated with its use. It is the material easily removed from the oxidation cell and oxygen
responsibility of the user of this standard to establish appro- delivery tube with hydrocarbon solvent.
priate safety and health practices and determine the applica- 3.1.3 inherent stability—the resistance to change when
bility of regulatory limitations prior to use. exposed to air, but in the absence of other environmental
factors such as water, or reactive metallic surfaces and dirt.
2. Referenced Documents
3.1.4 total insolubles—sum of the adherent and filterable
2.1 ASTM Standards:
insolubles.
D 381 Test Method for Existent Gum in Fuels by Jet 3.1.5 trisolvent—(TAM), a solution of equal volumes of
Evaporation
toluene, acetone, and methanol.
D 943 Test Method for Oxidation Characteristics of Inhib- 3.1.6 zero time—the time the first of a batch of oxidation
ited Mineral Oils cells is placed in the heating bath.
D 2699 Test Method for Research Octane Number of
3.1.6.1 Discussion—This is the time taken as the start of the
Spark-Ignition Engine Fuel 16 h of residence in the heating bath.
D 2700 Test Method for Motor Octane Number of Spark-
4. Summary of Test Method
Ignition Engine Fuel
D 4057 Practice for Manual Sampling of Petroleum and 4.1 A 350-mL volume of filtered middle distillate fuel is
Petroleum Products aged at 95°C (203°F) for 16 h while oxygen is bubbled through
D 4625 Test Method for Distillate Fuel Storage Stability at the sample at a rate of 3 L/h. After aging, the sample is cooled
43°C (110°F) to approximately room temperature before filtering to obtain
the filterable insolubles quantity. Adherent insolubles are then
removed from the oxidation cell and associated glassware with
This test method is under the jurisdiction of Committee D-2 on Petroleum trisolvent. The trisolvent is evaporated to obtain the quantity of
Products and Lubricants and is the direct responsibility of Subcommittee D02.14 on
adherent insolubles. The sum of the filterable and adherent
Stability and Cleanliness of Liquid Fuels.
insolubles, expressed as milligrams per 100 mL, is reported as
Current edition approved July 15, 1994. Published September 1994. Originally
total insolubles.
published as D 2274 – 64 T. Last previous edition D 2274 – 88.
Annual Book of ASTM Standards, Vol 05.01.
Annual Book of ASTM Standards, Vol 05.05.
Annual Book of ASTM Standards, Vol 05.02.
Copyright © ASTM, 100 Barr Harbor Drive, West Conshohocken, PA 19428-2959, United States.
D 2274
5. Significance and Use laboratory personnel from potential harm, chromic acid shall
not be used for cleaning glassware in the practice of this
5.1 This test method provides a basis for the estimation of
method.
the storage stability of middle distillate fuels with an initial
6.2 It has been found that commercial grades of acetone, if
boiling point above about 175°C (347°F) and a 90 % recovery
used in the trisolvent, can have impurities which cause an
point below 370°C (698°F) such as No. 2 fuel oil. It is not
apparently greater level of adherent insolubles to be measured.
applicable to fuels containing residual oil, or any significant
It is, therefore, critical that only reagent (or higher) grade
component derived from a non-petroleum source.
materials be used in preparing the trisolvent mixture.
5.2 The test method may not provide a prediction of the
6.3 Ultraviolet light exposure has been found to increase the
quantity of insolubles that will form in field storage over any
amount of total insolubles. Therefore, the fuel being tested
given period of time. The amount of insolubles formed in such
shall be shielded from direct exposure to ultraviolet light
field storage is subject to the specific conditions which are too
(sunlight or fluorescent). Conduct all sampling, measuring,
variable for this test method to predict accurately.
filtration, and weighing away from direct sunlight and in as
5.3 Test Method D 2274 yields results more rapidly than
dark an area as would be compatible with other laboratory
Test Method D 4625, the 43°C bottle test. However, as a result
operations. Storage before stress, the stress period and cool-
of the significantly elavated temperature and the pure oxygen
down after stressing shall be in the dark.
atmosphere, the nature and amount of insolubles may deviate
to a greater extent than Test Method D 4625 from those formed
7. Apparatus
in field storage.
NOTE 1—It is suggested that all equipment be calibrated according to
6. Interferences
manufacturer’s instructions on a periodic basis to assure consistency of
results.
6.1 Oxidation is a major chemical process causing adherent
and filterable insolubles to form. Any substance such as copper 7.1 Oxidation Cell, of borosilicate glass, as shown in Fig. 1,
or chromium that catalyzes oxidation reactions will cause shall consist of a test tube, condenser, and oxygen delivery
greater quantities of insolubles to form. Since the apparatus tube. This cell is identical to that used in Test Method D 943.
used in this test can also be used in Test Method D 943, where 7.2 Heating Bath, with a thermostatically controlled liquid
coils of copper and steel are used, it is important that any medium, shall be capable of maintaining the bath temperature
residues that could contain these metals be eliminated from the at 95 6 0.2°C (203 6 0.4°F). It shall be fitted with a suitable
apparatus by thorough cleaning prior to use. Similarly, to
stirring device to provide a uniform temperature throughout the
preclude the presence of chromium ions, as well as to protect bath. It shall be large enough to hold the desired number of
FIG. 1 Oxidation Cell
D 2274
oxidation cells immersed to a depth of approximately 350 mm. sufficiently high purity to permit its use without lessening the
Further, the bath construction must permit shielding the fuel accuracy of the determination.
samples in the oxidation cells from light while they are 8.2 Isooctane, 99.75 % purity or better and containing no
undergoing oxidation. more than 0.10 % n-heptane (Test Methods D 2699 and
7.3 Flowmeters, shall have a capability of measuring 3 6 D 2700), prefiltered through filter media as described in 7.7
0.3 L/h of oxygen. One flowmeter shall be provided for each (Warning—Extremely flammable. Skin irritant on repeated
oxidation cell. contact. Aspiration hazard).
7.4 Filter Drying Oven, shall be capable of safely evapo- 8.3 Oxygen, 99.5 % purity or better. When the oxygen is
rating the solvent at 80°C 6 2°C (176°F 6 4°F) for the drying delivered through a plant system of piping, a filter shall be
of filter materials. provided adjacent to the constant temperature bath to prevent
7.5 Glassware Drying Oven, shall be capable of drying the introduction of line debris or moisture into the oxidation
glassware at 105°C 6 5°C (221 6 9°F). cells; a pressure regulator adequate to maintain a constant flow
7.6 Filter Assembly, see Fig. 2, shall be capable of holding of gas through the apparatus shall also be used. A tank of
the filters described in 7.7. oxygen of the specified purity can be used provided it is
7.7 Filter Media , 47 mm diameter cellulose ester mem- equipped with a two-stage pressure regulator. (Warning—
brane filters with a nominal pore size of 0.8 μm. Single, Oxygen vigorously accelerates combustion. Do not use equip-
surfactant-free 0.8-μm pore size filters will be used for prefil- ment having exposed surfaces containing oil or grease.)
tration, however, a matched weight pair, or preweighed control 8.4 Trisolvent, a mixture of equal volumes of acetone,
and sample, 0.8 μm filters must be used for determination of methanol, and toluene. See 8.1. (Warning—It is particularly
filterable particulates. important that technical, commercial, practical, or industrial
7.8 Evaporating Vessel, borosilicate glass beaker, 200-mL grades (however they are designated by the particular manu-
capacity, tall style. facturer) are not to be used, as their use may lead to apparently
7.9 Hot Plate, capable of heating a liquid in the evaporating increased levels of adherent insolubles. (Warning—Fire haz-
vessel (7.8) to 135°C (275°F). ard, toxic.)
8. Reagents and Materials 9. Samples and Sampling
8.1 Purity of Reagents—Reagent grade chemicals shall be 9.1 Analyze fuel samples as soon as possible after receipt.
used in all tests. Unless otherwise indicated, it is intended that When a fuel cannot be tested within one day blanket it with an
all reagents shall conform to the specifications of the Commit- inert gas such as oxygen-free nitrogen, argon, or helium and
tee on Analytical Reagents of the American Chemical Society, store at a temperature no higher than 10°C (50°F) but not lower
where such specifications are available. Other grades may be than the cloud point (see Appendix X1). (Warning—Plastic
used, provided it is first ascertained that the reagent is of containers are not acceptable for samples due to the potential
for leaching of plasticizers. Samples should be taken preferably
in metal cans previously cleaned according to Practice D 4057.
This apparatus is available from suppliers of specialty petroleum testin
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