ASTM D4625-92(1998)
(Test Method)Standard Test Method for Distillate Fuel Storage Stability at 43°C (110°F)
Standard Test Method for Distillate Fuel Storage Stability at 43°C (110°F)
SCOPE
1.1 This test method covers a method for evaluating the inherent storage stability of distillate fuels having flash points above 38°C (100°F) and 90% distilled points below 340°C (644°F). Note 1-ASTM specification fuels falling within the scope of this test method are D396 grade Nos. 1 and 2, D975 grades 1-D and 2-D, and D2880 grades 1-GT and 2-GT.
1.2 This test method is not suitable for quality control testing but, rather it is intended for research use to shorten storage time relative to that required at ambient storage temperatures.
1.3 Appendix X1 presents additional information about storage stability and the correlation of D4625 results with sediment formation in actual field storage.
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. For specific hazard information, see Notes 2 through 6.
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An American National Standard
Designation: D 4625 – 92 (Reapprved 1998)
Designation: 378/87
Standard Test Method for
Distillate Fuel Storage Stability at 43°C (110°F)
This standard is issued under the fixed designation D 4625; 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 test method was adopted as a joint ASTM/IP standard in 1986.
This standard has been approved for use by agencies of the Department of Defense.
1. Scope Petroleum Products
1.1 This test method covers a method for evaluating the
3. Terminology
inherent storage stability of distillate fuels having flash points
3.1 Definitions of Terms Specific to This Standard:
above 38°C (100°F) and 90 % distilled points below 340°C
3.1.1 adherent insolubles, n—gums formed during storage
(644°F).
which remain tightly attached to the walls of the vessel.
NOTE 1—ASTM specification fuels falling within the scope of this test
3.1.2 filterable insolubles, n—solids formed during storage
method are Specification D 396 grade Nos. 1 and 2, Specification D 975
which can be removed from the fuel by filtration.
grades 1-D and 2-D, and Specification D 2880 grades 1-GT and 2-GT.
3.1.3 inherent storage stability, n—of mid-distillate fuel—
1.2 This test method is not suitable for quality control
the resistance to change in storage in contact with air, but in the
testing but, rather it is intended for research use to shorten
absence of other environmental factors such as water, or
storage time relative to that required at ambient storage
reactive metallic surfaces and dirt.
temperatures.
3.1.4 total insolubles, n—sum of the filterable insolubles
1.3 Appendix X1 presents additional information about
plus the adherent insolubles.
storage stability and the correlation of Test Method D 4625
4. Summary of Test Method
results with sediment formation in actual field storage.
1.4 This standard does not purport to address all of the
4.1 Four-hundred millilitre volumes of filtered fuel are aged
safety concerns, if any, associated with its use. It is the
by storage in borosilicate glass containers at 43°C (110°F) for
responsibility of the user of this standard to establish appro-
periods of 0, 4, 8, 12, 18, and 24 weeks. After aging for a
priate safety and health practices and determine the applica-
selected time period, a sample is removed from storage, cooled
bility of regulatory limitations prior to use. For specific hazard
to room temperature, and analyzed for filterable insolubles and
information, see Notes 2-6.
for adherent insolubles.
2. Referenced Documents
5. Significance and Use
2.1 ASTM Standards:
5.1 Fuel oxidation and other degradative reactions leading
D 381 Test Method for Existent Gum in Fuels by Jet
to formation of sediment (and color) are mildly accelerated by
Evaporation
the test conditions, compared to typical storage conditions. Test
D 396 Specification for Fuel Oils
results have been shown to predict storage stability more
D 975 Specification for Diesel Fuel Oils
reliably than other more accelerated tests. See Appendix X1 for
D 2880 Specification for Gas Turbine Fuel Oils
information on the correlation of test results with actual field
D 4057 Practice for Manual Sampling of Petroleum and
storage.
5.2 Because the storage periods are long (4 to 24 weeks), the
test method is not suitable for quality control testing, but does
This test method is under the jurisdiction of ASTM Committee D02 on
provide a tool for research on storage properties of fuels.
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.14 on Stability and Cleanliness of Liquid Fuels.
Current edition approved Aug. 15, 1992. Published October 1992. Originally
published as D 4625 – 86. Last previous edition D 4625 – 86.
Annual Book of ASTM Standards, Vol 05.01.
Annual Book of ASTM Standards, Vol 05.02.
Copyright © ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.
D 4625
5.3 Because environmental effects and the materials and provided it is first ascertained that the reagent is of sufficiently
nature of tank construction affect storage stability, the results high purity to permit its use without lessening the accuracy of
obtained by this test are not necessarily the same as those the determination.
obtained during storage in a specific field storage situation. 7.2 Glass Fiber Filter, 2.4-cm circle, 1.5-μm nominal pore
size.
6. Apparatus
7.3 Hydrocarbon Solvent, iso—octane, ASTM knock test
reference fuel grade, prefiltered through two glass-fiber filters.
6.1 Sample Containers, borosilicate glass bottles. The con-
tainers must have a lid or cover, preferably with a polytet-
NOTE 2—Warning: Extremely flammable. Harmful if inhaled. Vapors
rafluoroethylene (PTFE) insert and a hole for a borosilicate
may cause flash fire.
glass vent. The total capacity of the containers is 500 mL.
7.4 Adherent Insolubles Solvent (Note 3)—Mix equal parts
6.2 Storage Oven, large enough to contain all of the sample
of reagent grade acetone (Note 4), methanol (Note 5), and
bottles. The oven shall be thermostatically controlled to main-
toluene (Note 6).
tain a temperature of 43 6 1°C (110 6 2°F). It shall be as dark
as possible to prevent degradation due to photolytic reactions NOTE 3—Warning: Extremely flammable. Vapors harmful. May cause
flash fire.
and shall also be explosion proof.
NOTE 4—Warning: Extremely flammable. Vapors may cause flash fire.
6.3 Drying Oven, maintained at 99 6 1°C (210 6 2°F).
NOTE 5—Warning: Flammable. Vapor harmful. May be fatal or cause
6.4 Gooch Crucible, porcelain, No. 4 and Walter crucible
blindness if swallowed or inhaled. Cannot be made nonpoisonous.
holder.
NOTE 6—Warning: Flammable. Vapor harmful.
6.5 Filter Flask assembly, as shown in Fig. 1.
8. Sampling Procedure
7. Reagents and Materials
8.1 Samples for testing shall be obtained by an appropriate
7.1 Purity of Reagents—Reagent grade chemicals shall be
method outlined in Test Method D 4057. Sample containers
used in all tests. Unless otherwise indicated, it is intended that
should be 1 gal (3.78 L) or larger, epoxy-lined cans. Fill sample
all reagents conform to the specifications of the Committee on
cans almost to the top to avoid a significant air space. Purge the
Analytical Reagents of the American Chemical Society where
void space with nitrogen. Store the samples at reduced tem-
such specifications are available. Other grades may be used,
perature, − 7 to 4°C (20 to 40°F), prior to use, where possible.
9. Preparation and Apparatus
9.1 Sample Storage Bottles—Scrub each bottle with a de-
“Reagent Chemicals, American Chemical Society Specifications,” Am. Chemi-
cal Soc., Washington, DC. For suggestions on the testing of reagents not listed by tergent solution and rinse it with water. Soak the bottle
the American Chemical Society, see Analar Standards for Laboratory Chemicals-
overnight in a mildly alkaline laboratory glassware cleaning
,BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia and National
solution. Rinse the bottle with tap-water, then invert it and
Formulary,U.S. Pharmacopeial Convention, Inc., (USPC), Rockville, MD.
flush it with a stream of distilled water. Allow the bottles to dry
and rinse the bottles with 50 mL of the fuel sample. Vent the
bottles during storage, using a glass tube bent in an upside
down “U,” (see Fig. 2), to prevent contamination of the sample
from airborne particulates. Insert the glass tube through a
cover, preferably equipped with a polytetrafluoroethylene
(PTFE) insert (see Fig. 2).
9.2 Filter Preparation—Insert two glass-fiber filter disks
into the clean Gooch crucible (Note 7). Wash the filters by
pouring 200 mL of knock-grade isooctane through the Gooch
crucible. After removing the excess solvent with suction, dry
the crucible and filters for1hinan oven maintained at 99 6
1°C (210 6 2°F).
9.3 Cooling and Weighing—After drying, place the crucible
and filters in a desiccator without desiccant for at least 30 min
to protect the crucible and filters from airborne particulates and
to allow the crucible to cool in an environment similar to the
surrounding environment and thereby prevent possible errors
due to sudden absorption of moisture from the atmosphere
when the crucible is removed from the desiccator. Use the
weight of the moisture blank crucible to correct for atmo-
spheric moisture. Weigh the crucibles with the filters to the
nearest 0.1 mg and retain for sample analysis. This must be
The glass fiber filter paper available from Whatman as Catalog No. 1827 024
FIG. 1 Self-Feeding Filtering Assembly (934-AH), has been found satisfactory for this purpose.
D 4625
11.1.4 Perform zero-week analyses on the same day as the
other samples are placed in storage. Zero-week data are
necessary to provide base data and assure satisfactory tech-
nique.
11.2 Determination of Filterable Insolubles:
11.2.1 At the end of each prescribed period of time, remove
two bottles from the storage oven and allow them to cool to 21
to 27°C (70 to 80°F) in a dark environment. This may take
from4to24h.
11.2.2 After cooling, pour the sample from one bottle into a
clean separatory funnel, using a glass funnel (10.2), and using
a self-feeding system as pictured in Fig. 1, filter through a tared
Gooch crucible containing two glass-fiber filters (Note 9).
11.2.3 Rinse the bottles used during aging with filtere
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