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.

Designation: D4625 − 16´1

Standard Test Method for

Middle Distillate Fuel Storage Stability at 43 °C (110 °F)1
This standard is issued under the fixed designation D4625; 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 (´) indicates an editorial change since the last revision or reapproval.
This standard has been approved for use by agencies of the U.S. Department of Defense.

ε1 NOTE—The IP designation was removed and footnote 1 was revised editorially in February 2018.

1. Scope* 2. Referenced Documents

1.1 This test method covers a method for evaluating the 2.1 ASTM Standards:2
inherent storage stability of distillate fuels having flash points D86 Test Method for Distillation of Petroleum Products and
above 38 °C (100 °F), by Test Methods D93, and 90 % distilled Liquid Fuels at Atmospheric Pressure
points below 340 °C (644 °F), by Test Method D86. D93 Test Methods for Flash Point by Pensky-Martens
Closed Cup Tester
NOTE 1—ASTM specification fuels falling within the scope of this test D381 Test Method for Gum Content in Fuels by Jet Evapo-
method are Specification D396, Grade Nos. 1 and 2; Specification D975, ration
Grades 1-D and 2-D; and Specification D2880, Grades 1-GT and 2-GT.
D396 Specification for Fuel Oils
1.2 This test method is not suitable for quality control D975 Specification for Diesel Fuel Oils
testing but, rather it is intended for research use to shorten D1193 Specification for Reagent Water
storage time relative to that required at ambient storage D2880 Specification for Gas Turbine Fuel Oils
temperatures. D4057 Practice for Manual Sampling of Petroleum and
Petroleum Products
1.3 Appendix X1 presents additional information about
D4177 Practice for Automatic Sampling of Petroleum and
storage stability and the correlation of Test Method D4625
Petroleum Products
results with sediment formation in actual field storage.
1.4 The values given in SI units are to be regarded as the 3. Terminology
standard. 3.1 Definitions of Terms Specific to This Standard:
1.4.1 Exception—The values in parentheses are for informa- 3.1.1 adherent insolubles, n—gums formed during storage
tion only. that remain tightly attached to the walls of the vessel after fuel
has been flushed from the container.
1.5 This standard does not purport to address all of the
safety concerns, if any, associated with its use. It is the 3.1.2 filterable insolubles, n—solids formed during storage
responsibility of the user of this standard to establish appro- that can be removed from the fuel by filtration.
priate safety, health, and environmental practices and deter- 3.1.3 inherent storage stability, n—of middle distillate
mine the applicability of regulatory limitations prior to use. fuel—the resistance of the fuel to change during storage in
1.6 This international standard was developed in accor- contact with air, but in the absence of other environmental
dance with internationally recognized principles on standard- factors such as water, or reactive metals and dirt.
ization established in the Decision on Principles for the 3.1.4 total insolubles, n—the arithmetic sum of the filterable
Development of International Standards, Guides and Recom- insolubles plus the adherent insolubles.
mendations issued by the World Trade Organization Technical
Barriers to Trade (TBT) Committee. 4. Summary of Test Method
4.1 Four-hundred (400) mL volumes of filtered fuel are aged
by storage in borosilicate glass containers at 43 °C (110 °F) for
1
This test method is under the jurisdiction of ASTM Committee D02 on periods of 4, 8, 12, 18, and 24 weeks. If desired, perform
Petroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility of
Subcommittee D02.14 on on Stability, Cleanliness and Compatibility of Liquid
2
Fuels. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved Dec. 1, 2016. Published January 2017. Originally contact ASTM Customer Service at [email protected]. For Annual Book of ASTM
approved in 1986. Last previous edition approved in 2014 as D4625 – 14. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D4625-16E01. the ASTM website.

*A Summary of Changes section appears at the end of this standard

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 D4625 − 16´1
6.3 Filter Drying Oven, shall be capable of safely evapo-
rating the solvent at 90 °C 6 5 °C for the drying of filters.
6.4 Filtration System—Arrange the following components
as shown in Fig. 2.
6.4.1 Funnel and Funnel Base, with filter support for a
47 mm diameter membrane and a locking ring or spring action
clip.
6.4.2 Ground/Bond Wire, 0.912 mm to 2.59 mm (No. 10 to
No. 19) bare-stranded, flexible stainless steel or copper in-
stalled in the flasks and grounded as shown in Fig. 2.
6.4.3 Receiving Flask, 1.5 L, or larger, borosilicate glass
vacuum filter flask, into which the filtration apparatus fits,
equipped with a sidearm to connect to the safety flask.
6.4.4 Safety Flask, 1.5 L, or larger, borosilicate glass
vacuum filter flask equipped with a sidearm to connect the
vacuum system. A fuel and solvent resistant rubber hose,
through which the grounding wire passes, shall connect the
sidearm of the receiving flask to the tube passing through the
rubber stopper in the top of the safety flask.
6.4.5 Vacuum System, either a water-aspirated, or a
mechanical, vacuum pump may be used if capable of produc-
FIG. 1 Sample Storage Container ing a vacuum of 80 kPa to 100 kPa below atmospheric pressure
when measured at the receiving flask.
zero-week analyses on the same day as the other samples are
placed in storage. Zero-week data are used to provide base data 7. Reagents and Materials
and ensure satisfactory technique. After aging for a selected 7.1 Purity of Reagents—Reagent grade chemicals shall be
time period, a sample is removed from storage, cooled to room used in all tests. Unless otherwise indicated, it is intended that
temperature, and analyzed for filterable insolubles and for all reagents conform to the specifications of the Committee on
adherent insolubles. Analytical Reagents of the American Chemical Society where
such specifications are available.3 Other grades may be used,
5. Significance and Use provided it is first ascertained that the reagent is of sufficiently
5.1 Fuel oxidation and other degradative reactions leading high purity to permit its use without lessening the accuracy of
to formation of sediment (and color) are mildly accelerated by the determination.
the test conditions compared with typical storage conditions. 7.2 Nylon Test and Control Membrane Filters—plain,
Test results have been shown to predict storage stability more 47 mm diameter, nominal pore size 0.8 µm. (Membrane filters
reliably than other more accelerated tests. See Appendix X1 for with a grid imprinted on their surface may be used as control
information on the correlation of test results with actual field membrane filters for identification.)
storage.
7.3 Hydrocarbon Solvent, 2,2,4-trimethylpentane (iso-
5.2 Because the storage periods are long (4 weeks to octane)—ASTM knock test reference fuel grade or equivalent,
24 weeks), the test method is not suitable for quality control prefiltered through two glass-fiber or nylon membrane filters,
testing, but does provide a tool for research on storage nominal pore size 0.8 µm. (Warning—Extremely flammable.
properties of fuels. Harmful if inhaled. Vapors may cause flash fire.)
5.3 Because environmental effects and the materials and 7.4 Adherent Insolubles Solvent (Warning—Extremely
nature of tank construction affect storage stability, the results flammable. Vapors harmful. May cause flash fire)—Mix equal
obtained by this test are not necessarily the same as those volumes of reagent grade acetone (Warning—Extremely flam-
obtained during storage in a specific field storage situation. mable. Vapors may cause flash fire), methyl alcohol
6. Apparatus (Warning—Flammable. Vapor harmful. May be fatal or cause
blindness if swallowed or inhaled. Cannot be made
6.1 Sample Containers, borosilicate glass bottles, nominal nonpoisonous), and toluene (Warning—Flammable. Vapor
capacity 500 mL (Fig. 1). The containers shall have a cap, lid, harmful.).
or cover, preferably with a polytetrafluoroethylene (PTFE)
insert and a hole for a borosilicate glass vent.
6.2 Storage Oven, large enough to contain all of the sample 3
Reagent Chemicals, American Chemical Society Specifications, American
bottles. The oven shall be thermostatically controlled to main- Chemical Society, Washington, DC. For Suggestions on the testing of reagents not
listed by the American Chemical Society, see Annual Standards for Laboratory
tain a temperature of 43 °C 6 1 °C (110 °F 6 2 °F). It shall be
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
as dark as possible to prevent degradation due to photolytic and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
reactions and shall also be explosion proof. MD.

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 D4625 − 16´1

FIG. 2 Schematic of Filtration System

7.5 Purity of Water—Unless otherwise indicated, references 9.3 Preparation of Membrane Filters:
to water mean reagent water as defined by Type III of 9.3.1 Each set of test filters consists of one test membrane
Specification D1193. filter and one control membrane filter. For fuels containing
7.6 Liquid or Powder Detergent, water-soluble, for cleaning little particulate materials, only one set of filters is required. If
glassware. the fuel is highly contaminated, more than one set of filters
may be required. The two membrane filters used for each
8. Sampling Procedure individual test shall be identified by marking the petri dishes
8.1 Samples for testing shall be obtained by an appropriate used to hold and transport the filters. Clean all glassware used
method outlined in Practice D4057 or D4177. Sample contain- in preparation of membrane filters as described in 9.2.
ers should be 1 gal (3.78 L) or larger, epoxy-lined cans. Fill 9.3.1.1 Using forceps, place the test and control membrane
sample cans almost to the top to avoid a significant air space. filters side by side in a clean petri dish. To facilitate handling,
Purge the void space with nitrogen. Store the samples at the membrane filters should rest on clean glass support rods, or
reduced temperature, –7 °C to 4 °C (20 °F to 40 °F), prior to watch glasses, in the petri dish.
use, where possible. 9.3.1.2 Place the petri dish, with its lid slightly ajar, in a
drying oven at 90 °C 6 5 °C and leave it for 30 min.
9. Preparation of Apparatus and Sample Bottles 9.3.1.3 Remove the petri dish from the drying oven, and
place it near the balance. Keep the petri dish cover ajar, but
9.1 Sample Storage Bottles—Scrub each bottle and cap with
keep it such that the membrane filters are still protected from
a detergent solution and rinse it with water. Soak the bottle and
contamination from the atmosphere. Allow 30 min for the
cap overnight in an alkaline laboratory glassware cleaning
membrane filters to come to equilibrium with room air tem-
solution. Rinse the bottle and cap with tap water, then invert
perature and humidity.
them and flush them with a stream of distilled water. Allow the
bottles and caps to dry. Prior to introducing the sample, rinse 9.3.1.4 Remove the control membrane filter from the petri
the bottles with 50 mL of the fuel sample. Vent the bottles dish with forceps, handling by the edge only, and place it
during storage, using a glass tube bent in an upside down “U,” centrally on the weighing pan of the balance. Weigh it, record
(see Fig. 1), to prevent contamination of the sample from the initial mass to the nearest 0.1 mg, and return it to the petri
airborne particulates. Insert the glass tube through a cover, dish.
preferably equipped with a polytetrafluoroethylene (PTFE) 9.3.1.5 Repeat 9.3.1.4 for the test membrane filter.
insert (see Fig. 1). 9.3.1.6 Using clean forceps, place the weighed control
membrane filter centrally on the membrane filter support of the
9.2 Clean all components of the filtration apparatus as filtration apparatus (see Fig. 2). Place the weighed test mem-
described in 9.2.1 – 9.2.7. brane filter on top of the control membrane filter. Install the
9.2.1 Remove any labels, tags, and so forth. funnel and secure with locking ring or spring clip. Do not
9.2.2 Wash with warm tap water containing detergent. remove the plastic film from the funnel opening until ready to
9.2.3 Rinse thoroughly with warm tap water. start filtration.
9.2.4 Rinse thoroughly with deionized water.
9.2.5 Rinse thoroughly with propan-2-ol that has been 10. Preparation of Sample
filtered through a 0.45 µm membrane filter.
9.2.6 Rinse thoroughly with filtered flushing fluid and dry. 10.1 If the fuel has been stored at reduced temperature,
9.2.7 Keep a clean protective cover (the cover may be rinsed allow the sample to come to ambient temperature. To dissolve
with filtered flushing fluid) over the top of the sample container any separated wax, be certain that the entire fuel sample is at
until the cap is installed. Similarly, protect the funnel opening least 5 °C above its cloud point before proceeding.
of the assembled filtration apparatus with a clean protective 10.2 The test fuel shall be filtered prior to placing it in
cover until ready for use. storage. Assemble a filtration system, as shown in Fig. 2, to

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 D4625 − 16´1
filter the fuel. Use a single membrane filter for this filtration tain vacuum after the final washing for 10 s to 15 s to remove
step. This membrane filter need not be preweighed. excess filtered flushing fluid from the membrane filter.
10.3 Using this filtration assembly, filter sufficient fuel to 11.2.2.3 Using clean forceps, carefully remove the test and
put 400 mL of fuel in each storage bottle. For a typical test, this control membrane filters from the filter base and place them
is 4 L of fuel. It is prudent to filter a small amount of extra fuel. side by side on clean glass support rods or watch glasses in a
It may be necessary to replace the filter membrane (7.2) clean, covered petri dish. Dry and reweigh the membrane filters
throughout this step, depending on the cleanliness of the test as described in 9.3, taking care not to disturb the particulate on
fuel. the surface of the test membrane filter. Record the final control
membrane filter mass and the final test membrane filter mass to
11. Procedure the nearest 0.1 mg for each filtration.
11.1 Sample Aging: NOTE 2—Do not mix rinsings and filtrate if filtrate color changes are
11.1.1 Adjust the storage oven for sample storage to a being measured.
NOTE 3—If severe filter plugging is encountered so that filtration is not
temperature of 43 °C 6 1 °C (110 °F 6 2 °F). complete in 3 h, discontinue the test with the notation that filter plugging
11.1.2 Place 400 mL of filtered fuel into each bottle. Use occurred.
two bottles for each sampling period. (Commonly used sam-
11.2.3 Repeat the procedure in 11.2.2 – 11.2.2.3 for the
pling periods are 4, 8, 12, 18, and 24 weeks). Extra bottles may
second bottle.
be placed in storage to be used in case of accidents, for further
tests at other times of storage, or to extend the overall test 11.3 Determination of Adherent Insolubles on Sample
duration. Bottle—After the final washing with the hydrocarbon solvent,
11.1.2.1 Some operators have found it useful to conduct a dissolve any adherent gum on the sample container walls with
zero-week test as a demonstration of proper technique. Since two washings of 30 mL to 35 mL of the adherent insolubles
the fuel is prefiltered, zero-week results should be nil. A solvent. Pour each washing into previously weighed 100 mL
zero-week analysis is not a mandatory part of the analysis. beakers. Evaporate the solvent at 160 °C (320 °F) by the air jet
11.1.3 Label each storage bottle with the time and date the method in accordance with Test Method D381. After the
test is started, sample identification, and the time and date solvent is completely evaporated, place the beakers in a
when the bottle is to be removed from storage. Place the bottles desiccator without desiccant and allow to cool to room
in the oven in random order as a means to reduce the possible temperature. Weigh the beakers to the nearest 0.1 mg. Use a
effects of hot zones in the oven. tare beaker (moisture blank) in accordance with Test Method
D381.
11.2 Determination of Filterable Insolubles:
11.2.1 At the end of each prescribed period of time, remove
12. Calculation
two bottles from the storage oven and allow them to cool to
21 °C to 27 °C (70 °F to 80 °F) in a dark environment. This 12.1 Calculate the total insolubles (Ti) in milligrams per
may take from 4 h to 24 h. 100 mL of fuel after aging, as follows:
11.2.2 Assemble the filtration apparatus with a preweighed ~ F i 1A i !
sample and control filter. After the fuel has cooled, pour fuel Ti 5 (1)
4
from the sample container to the graduated cylinder, start the
vacuum, and then transfer 100 mL of fuel to the filter funnel. where:
11.2.2.1 Continue transferring 100 mL increments of fuel to Ti = total insolubles, mg/100 mL,
the filter funnel. When all the fuel from the sample container Fi = mass of filterable insolubles, mg, as determined in 11.2,
has been filtered, or if filtration slows so that 100 mL of sample and
requires greater than 10 min for complete filtration, then Ai = moisture corrected mass of adherent insolubles, mg, as
remove the filter support/filter funnel from the receiving flask, determined in 11.3.
pour the filtered fuel into a clean graduated cylinder, and record
the volume of fuel that was filtered in millilitres. Keep the fuel 13. Report
sample filtrate separate from the solvent washings filtrate. This 13.1 Report Ti, Fi, and Ai from 12.1 for both bottles to show
allows the fuel to be used for additional analyses (if desired). repeatability of tests at each aging period.
If all the fuel has been filtered, thoroughly rinse the sample
container and the graduated cylinder with one or more portions 14. Precision and Bias4
of filtered flushing fluid, pour the rinses into the funnel, and 14.1 The precision of this test method as determined by the
proceed to 11.2.2.2. If all the fuel has not been filtered, proceed statistical examination of the interlaboratory test results is as
to 11.2.2.2 and 11.2.2.3, and then repeat from 11.2.2.1. follows.
11.2.2.2 Wash down the inside of the funnel and the outside NOTE 4—The precision of this method was determined in a cooperative
of the joint between the funnel and filter base filtered with test involving ten laboratories and eight different fuels. The results ranged
flushing fluid. With the vacuum applied, carefully separate the from 0.1 mg ⁄100 mL to 11.8 mg ⁄100 mL.
funnel from the filter base. Wash the periphery of the mem-
brane filter by directing a gentle stream of filtered flushing fluid
from the edge to the center, exercising care not to wash any of 4
Supporting data have been filed at ASTM International Headquarters and may
the particulate from the surface of the membrane filter. Main- be obtained by requesting Research Report RR:D02-1203.

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 D4625 − 16´1

Repeatability 5 0.62 =X (2)

where:
X = the average of two results, reported in mg/100 mL.
14.3 Reproducibility—The difference between two single
and independent results obtained by different operators work-
ing in different laboratories on identical test material would, in
the long run, exceed the following values only in one case in
twenty (see Fig. 3).
Reproducibility 5 2.20 =X (3)

where:
FIG. 3 Repeatability and Reproducibility for Total Insolubles X = the average value of two results, reported in mg/100 mL.
Measurements
14.4 Bias—The nature of this test and the parameters being
measured are such that a true bias statement cannot be written.
14.2 Repeatability—The difference between successive re- 14.5 These precision data were obtained by statistical ex-
sults obtained by the same operator with the same apparatus amination in interlaboratory tests.
under constant operating conditions on identical test material
would, in the long run, in the normal and correct operation of 15. Keywords
the test method exceed the following values only in one case in 15.1 accelerated test; adherent insolubles; distillate fuel;
twenty (see Fig. 3). filterable insolubles; prediction; storage stability

APPENDIX

(Nonmandatory Information)

X1. CORRELATION OF 43 °C STABILITY TEST RESULTS WITH ACTUAL FIELD STORAGE

X1.1 Introduction—The storage stability properties of dis- X1.3 Correlation Effects—The consequence of variation in
tillate fuels depend on complex oxidative and non-oxidative the chemical reactions leading to degradation during storage is
interactions of olefins, dienes, nitrogen-containing compounds, that some fuels show consistent effects from temperature
sulfur-containing compounds, and oxygen-containing com- acceleration; others do not. The reliability of correlations of
pounds which are present in fuel. These reactions may be accelerated test results with actual storage stability is enhanced
promoted by other contaminants, such as dissolved metal salts. when fuels tested are from the same feedstock source, or are
Storage stability varies enormously due to refinery feedstock similarly processed.
source (crude oil or otherwise) and the type of processing used
to produce components in the finished fuel. Because the X1.4 Correlation of Ambient and 43 °C Storage—For most
chemical reactions leading to formation of sediment (and practical purposes, it has been shown that aging fuel at 43 °C
color) vary depending on the type and amount of unstable results in an approximately fourfold acceleration of the degra-
materials present, the effects of degradation-accelerating con- dation for an ambient temperature of 21 °C, that is, a week of
ditions will also vary. 43 °C storage is roughly equivalent to a month of storage at
normal (environmental) ambient temperatures.5,6 Depending
X1.2 Effect of Aging Temperature—Fuel degradation is on fuel composition and actual storage conditions, this corre-
accelerated in the 43 °C test by aging at a higher than ambient lation may vary substantially in either direction.
temperature. The rate of degradation for various fuel types does
not change uniformly as temperature is increased. The rela-
tionship between temperature and rate depends on the activa- 5
“Navy-CRC Barge Storage Program,” Report No. 341, Project CG-1-58,
tion energies of the rate-controlling steps in the chemical Coordination Research Council, Inc., September 1959.
6
degradation reactions. These will vary from fuel to fuel; Stavinoha, L. L. and Westbrook, S. R., “Accelerated Stability Test Techniques
for Middle Distillate Fuels,” and Garner, M. Q. and White, E. W., “Correlation of
indeed, the chemical reactions may change under accelerated Long-Term Storage and Accelerated Stability Tests,” Distillate Fuel Stability and
conditions to give a sediment with a different composition. Cleanliness, ASTM STP 751, L. L. Stavinoha and C. P. Henry, Eds., ASTM
This effect is minimized in the 43 °C test. International, 1981, pp. 3 and 34 respectively.

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 D4625 − 16´1
SUMMARY OF CHANGES

Subcommittee D02.14 has identified the location of selected changes to this standard since the last issue
(D4625 – 14) that may impact the use of this standard. (Approved Dec. 1, 2016.)

(1) Revised subsections 4.1, 6.1, 6.3, 6.4, 6.4.2, 6.4.3, 6.4.4, (2) Added new subsections 10.3 and 11.1.2.1.
6.4.5, 7.3, 9.1, 9.2.4, 9.3.1.4, 9.3.1.6, 10.2, 11.1.2, 11.1.3, (3) Deleted former subsection 11.1.4.
11.2.2, 11.2.2.1, and 11.2.2.3; swapped positions of Fig. 1 and
Fig. 2.

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