Designation: D6468 − 08

Standard Test Method for

High Temperature Stability of Middle Distillate Fuels1
This standard is issued under the fixed designation D6468; 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.

1. Scope* D2880 Specification for Gas Turbine Fuel Oils

1.1 This test method covers relative stability of middle D3699 Specification for Kerosine
distillate fuels under high temperature aging conditions with D3828 Test Methods for Flash Point by Small Scale Closed
limited air exposure. This test method is suitable for all No. 1 Cup Tester
and No. 2 grades in Specifications D396, D975, D2880, and D4057 Practice for Manual Sampling of Petroleum and
D3699. It is also suitable for similar fuels meeting other Petroleum Products
specifications. D4625 Test Method for Middle Distillate Fuel Storage
Stability at 43°C (110°F)
1.2 This test method is not suitable for fuels whose flash D5452 Test Method for Particulate Contamination in Avia-
point, as determined by Test Methods D56, D93, or D3828, is tion Fuels by Laboratory Filtration
less than 38°C. This test method is not suitable for fuels
containing residual oil. 3. Terminology
1.3 The values stated in SI units are to be regarded as 3.1 Definitions of Terms Specific to This Standard:
standard. No other units of measurement are included in this 3.1.1 adherent insolubles—material that is produced in the
standard. course of stressing distillate fuel and that adheres to the
1.3.1 Exception—The maximum vacuum includes inch- glassware after fuel has been flushed from the system.
pound units in 6.5 and 11.2. 3.1.2 filterable insolubles—material that is produced in the
1.4 This standard does not purport to address all of the course of stressing distillate fuel and that is capable of being
safety concerns, if any, associated with its use. It is the removed from the fuel by filtration.
responsibility of the user of this standard to establish appro- 3.1.3 inherent stability—the resistance to change when ex-
priate safety and health practices and determine the applica- posed to air, but in the absence of other environmental factors
bility of regulatory limitations prior to use. such as water, reactive metal surfaces, and dirt.
3.1.4 storage stability—the resistance of fuel to formation
2. Referenced Documents
of degradation products when stored at ambient temperatures.
2.1 ASTM Standards:2
3.1.5 thermal stability—the resistance of fuel to formation
D56 Test Method for Flash Point by Tag Closed Cup Tester
of degradation products when thermally stressed.
D93 Test Methods for Flash Point by Pensky-Martens
Closed Cup Tester 4. Summary of Test Method
D396 Specification for Fuel Oils 4.1 Two 50-mL volumes of filtered middle distillate fuel are
D975 Specification for Diesel Fuel Oils aged for 90 or 180 min at 150°C in open tubes with air
D1500 Test Method for ASTM Color of Petroleum Products exposure. After aging and cooling, the fuel samples are filtered
(ASTM Color Scale) and the average amount of filterable insolubles is estimated by
D2274 Test Method for Oxidation Stability of Distillate Fuel measuring the light reflectance of the filter pads. The 100 and
Oil (Accelerated Method) 0 % extremes of the reflectance rating range are defined by an
unused filter pad and a commercial black standard, respec-
1
tively.
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee 5. Significance and Use3
D02.14 on Stability and Cleanliness of Liquid Fuels.
Current edition approved July 1, 2008. Published August 2008. Originally 5.1 This test method provides an indication of thermal
approved in 1999. Last previous edition approved in 2006 as D6468–06. DOI: oxidative stability of distillate fuels when heated to high
10.1520/D6468-08.
2
For referenced ASTM standards, visit the ASTM website, [Link], or
3
contact ASTM Customer Service at service@[Link]. For Annual Book of ASTM Henry, C. P., “The du Pont F21 149°C (300°F) Accelerated Stability Test,”
Standards volume information, refer to the standard’s Document Summary page on Distillate Fuel Stability and Cleanliness, ASTM STP 751, Stavinoha, L. L. and
the ASTM website. Henry, C. P., Eds., ASTM International, 1981, pp. 22-33.

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

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 D6468 − 08
temperatures that simulate those that may occur in some types obtained. Glass filter holders that use a 75-µm (200-mesh) screen to
of recirculating engine or burner fuel delivery systems. Results support the filter are available; however, since the screen can be an
unbonded electrostatic charge collector, these are not recommended for
have not been substantially correlated to engine or burner use with flammable liquids.
operation. The test method can be useful for investigation of
operational problems related to fuel thermal stability. 6.5 Vacuum Source, that limits the maximum vacuum to 27
kPa (200 mm Hg) below atmospheric pressure. The vacuum
5.2 When the test method is used to monitor manufacture or should rise to 27 kPa within 10 to 15 s after the sample is added
storage of fuels, changes in filter rating values can indicate a to the filtration funnel.
relative change in inherent stability. Storage stability predic-
tions are more reliable when correlated to longer-term storage NOTE 2—Use of reduced vacuum improves retention of particulate on
the relatively porous filter media.
tests, for example, Test Method D4625, or other lower tem-
perature, long-term tests. When fuel samples are freshly 6.6 Reflection meter, Photovolt Model 577 Digital Reflec-
produced, aging for 180 min, instead of the traditional 90-min tion Meter, complete with search unit Y with a green filter and
interval, tends to give a result correlating more satisfactorily polished black glass standard.5
with the above methods (see Appendix X2). NOTE 3—Other reflection meters or search units, or both, can be used,
5.3 The test method uses a filter paper with a nominal but they are likely to provide only similar (not identical) results. For
example, Photovolt Model 577 digital reflection meter equipped with
porosity of 11 µm, which will not capture all of the sediment search unit W usually gives somewhat lower percent reflectance values.
formed during aging but allows differentiation over a broad Correlation of these values is discussed in Appendix X1.
range. Reflectance ratings are also affected by the color of
filterable insolubles, which may not correlate to the mass of the 7. Reagents and Materials
material filtered from the aged fuel sample. Therefore, no 7.1 Purity of Reagents—Reagent grade chemicals shall be
quantitative relationship exists between the pad rating and the used in all tests. Unless otherwise indicated, it is intended that
gravimetric mass of filterable insolubles. all reagents conform to the specifications of the Committee on
Analytical Reagents of the American Chemical Society where
6. Apparatus such specifications are available.6 Other grades may be used,
6.1 Aging Tubes, 25× 200 mm, heavy wall test tubes made provided it is first ascertained that the reagent is of sufficiently
of borosilicate glass. high purity to permit its use without lessening the accuracy of
6.2 Heating Bath, with liquid heating medium, thermostati- the determination.
cally controlled to maintain the sample in the aging tube within 7.2 Acetone, (Warning—Extremely flammable.)
1.5°C of 150°C. It must be large enough to hold aging tubes 7.3 Adherent Insolubles Solvent (Trisolvent or TAM), a
immersed in the heating liquid to a depth above the level of mixture of equal parts by volume of reagent grade toluene
samples in the tubes. The bath and its location shall be such to (Warning—Flammable. Vapor harmful), acetone (Warning—
enable shielding of the samples from direct light during aging. see 7.2), and methanol (Warning—Flammable. Vapor harm-
The volume of bath and its heat recovery rate shall be such that ful. May be fatal or cause blindness if swallowed or inhaled.
the temperature of the medium does not drop more than 5°C Cannot be made nonpoisonous).
when the maximum number of aging tubes are inserted, and
recovery to 150°C shall not require more than 15 min. 7.4 Hydrocarbon Solvent, 2,2,4-trimethylpentane (iso-
(Warning—The flash point of the liquid heating medium must octane), 99.75 % purity minimum (Warning—see 7.2).
be at least 180°C. Bath vapors and oil sample vapors shall be NOTE 4—Heptane is a satisfactory alternative hydrocarbon solvent.
properly vented. Exposed hot surfaces on the apparatus and hot However, small differences may be seen due to slightly different solubility
heating medium can cause severe burns.) characteristics. Iso-octane is specified to be in agreement with the
hydrocarbon solvent used in other middle distillate stability test methods
6.3 Bath Thermometer, either glass or digital measuring such as Test Methods D2274 and D4625.
temperature measuring device, whose accuracy in the 140 to 7.5 Filter Paper (Filter Pad), Whatman No. 1, 47-mm
160°C range is certified or traceable to a certified thermometer. diameter, or equivalent.
6.4 Membrane Filter Holder, to fit 47-mm membrane filters,
NOTE 5—Filter papers of 42.5 or 55-mm diameter are technically
fitted to a heavy-walled 500-mL or 1-L vacuum flask. satisfactory. Filters with a diameter of 47 mm permit a small unused
NOTE 1—Several types of membrane filter holders are available. To margin for identifying the sample and fit all filtration apparatuses.
reduce electrostatic hazards, an all metal filter holder equipped with
grounding cables is recommended.4 Such an apparatus and correct 5
The sole source of supply of the apparatus known to the committee at this time
grounding practices are described in Test Method D5452. A fritted glass is available from UMM Electronics Inc., Photovolt Instruments, 6911 Hillsdale
filter holder is less preferred because of a tendency to become partially Court, Indianapolis, IN 46250-2062. If you are aware of alternative suppliers, please
clogged during use so that filter pads that do not have uniform deposits are provide this information to ASTM International Headquarters. Your comments will
receive careful consideration at a meeting of the responsible technical committee,1
which you may attend.
4 6
The sole source of supply of the apparatus known to the committee at this time Reagent Chemicals, American Chemical Society Specifications , American
is a suitable filter holder available from Millipore Corporation, 80 Ashby Rd., Chemical Society, Washington, DC. For suggestions on the testing of reagents not
Bedford, MA 01730; Catalog No. XX20 047 20. If you are aware of alternative listed by the American Chemical Society, see Analar Standards for Laboratory
suppliers, please provide this information to ASTM International Headquarters. Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
Your comments will receive careful consideration at a meeting of the responsible and National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,
technical committee,1 which you may attend. MD.

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 D6468 − 08
8. Sampling NOTE 8—The calibration procedure ensures that the instrument is
working properly. It also indirectly sets a nominal 100 % reflectance
8.1 When samples of a fuel batch are obtained to determine setting that is subsequently reset in 10.3.
stability, obtain samples in accordance with Practice D4057. 10.3 Place a new filter paper on top of a stack of at least ten
Use only epoxy-lined cans or borosilicate glass bottles. Shield unused Whatman No. 1 filters of the same size. Place the
clear glass bottles from sunlight to prevent photochemical search unit on the center of the filter, and adjust the meter
reactions. reading to 100 %, using the sensitivity control.
8.2 When samples are from a fuel or component rundown NOTE 9—Such adjustment, which sets the test method 100 % reflec-
line, exercise care to ensure that the sampling line and valving tance point, alters the reflectance scale; as a result, the reflection meter will
are thoroughly flushed with current mainstream sample. no longer read the recited reflectance of the standard plaque.

8.3 Because stability of some fuels, as determined in this 10.4 Place the search unit on the center of the black glass
test method, changes over time, the sampling date shall be standard, and adjust the meter reading to 0 %, using the ZERO
recorded; record time and date if sample is from a fuel or control. Recheck the 100 % adjustment against the new filter
component rundown line. Samples should be stored at tem- paper, and continue adjustment until the meter reads both 0 %
peratures below 5°C. If storage for more than a few days is with the black glass standard and 100 % with the new filter
expected, oxygen should be removed from the fuel by subsur- pad.
face purging with a stream of nitrogen; for example, by 11. Procedure
bubbling nitrogen for 1 min/L of sample.
8.3.1 If samples are taken out of cold storage, warm them to 11.1 Adjust the heating bath to a temperature of 1506 1.5°C
ambient temperature and thoroughly mix prior to aliquot (see 6.3).
sampling. 11.2 Assemble the filter apparatus with a new filter paper.
NOTE 6—If multiple analyses are to be performed on a sample, it is not Filter at least 100 mL of the fuel sample through the paper. Use
a good practice to warm the whole sample repeatedly for this purpose. the inline vacuum regulator so that the maximum vacuum is 27
One way of doing this would be to pour an aliquot of the cold sample into kPa (200 mm Hg). Measure two 50 6 2-mL volumes of filtered
a graduated cylinder, cap, allow to warm, and then dispense into the aging
tube for analysis. If the cloud point of the fuel is above 5ºC, warm to a
fuel and decant into each of two aging tubes (see Appendix
temperature 5ºC higher than the cloud point before dispensing. X3).
NOTE 10—Where practical, filter a fuel sample larger than 100 mL. This
9. Preparation of Apparatus will reduce the possibility that the paper may absorb trace materials that
affect stability.
9.1 Cleaning Aging Tubes—Clean new tubes using adherent
insolubles solvent, then with a mildly alkaline or neutral 11.3 Place the uncapped sample tubes in the heating bath,
laboratory detergent, followed by copious rinsing with deion- making sure the level of the fluid in the test tube is below the
ized or distilled water to remove all traces of detergent. Then surface of the oil in the heating bath. Age the fuel samples for
rinse with acetone and air dry. Rinse used tubes with trisolvent, 90 6 3 min, or 180 6 5 min. Place the tubes in the bath in the
dry, then clean as above for new tubes. Visually inspect tubes same order in which they are to be removed. (Warning—Fuels
before use, and reclean or reject if there is the slightest trace of will be heated above their flash points. There is a possibility
contamination. that certain light fuels such as kerosine will boil under
conditions of the test. Both situations raise the risk of fire when
9.1.1 Because of the small sample size and the high surface
an ignition source is present. Fuel samples that may contain
to volume ratio in this test method, carefully avoid carryover
gasoline or other volatile components should not be tested.)
from past tests or from cleaning agents. There are especially
strong effects from traces of copper, strong acids, and strong NOTE 11—The severity of the test is increased by aging for longer times
bases. at 150°C. The selection of the aging time depends on application and
should be established by correlation with other tests or with application
NOTE 7—Clean test tubes carefully to avoid carryover from past tests or requirements.
from cleaning agents. As a result of the small sample size evaluated and 11.4 Remove the samples from the heating bath and allow to
the high surface to volume ratio inherent to the test method, the results
obtained can be greatly influenced by the presence of trace contaminants
cool gradually in air to 20 to 25°C over a period of 90 min to
such as copper, strong acids, or strong bases. 4 h. Cool in the dark to prevent photochemical reactions. Do
not accelerate cooling by immersing in a cooling bath as this
9.2 Cleaning Membrane Filter Holder —Rinse with trisol- can result in small particle size and a lower pad rating. If
vent, then with acetone, and air dry. samples are allowed to stand more than 4 h before filtering,
insoluble gum may adhere to the aging tubes, resulting in
10. Calibration and Standardization erratic data. (Warning—The hot samples can cause severe
10.1 Turn on the reflection meter and allow at least 30 min burns. Use protective equipment.)
for warm-up. Set the gain to LO position for search unit Y with 11.5 Prepare a filtration assembly with a new filter paper,
green filter. and attach all grounding clips to ground. Filter one of the two
10.2 Follow the manufacturer’s instructions to carry out a aged fuel samples.
two point calibration of the reflection meter, using the black 11.6 While maintaining vacuum, wash the aging tube with
standard and standard plaque supplied with the search unit. three small portions, about 15 mL each, of iso-octane and filter

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 D6468 − 08
through the filter paper. Wash the inside of the filter assembly 15 laboratories. A separate program also verified that properly
with iso-octane, and remove the funnel portion of the assembly. calibrated reflection meters in different laboratories were in
While still maintaining vacuum, use a gentle stream of iso- excellent agreement. See the interlaboratory report (RR:D02-
octane from a squeeze bottle to wash the filter clean of any 1463).7 The precision of this test method as determined by
traces of fuel oil, and allow to dry under vacuum for 1 or 2 min statistical examination of interlaboratory results is as follows:
(see Note 13). Shut off vacuum, and remove the filter from the 13.1.1 Repeatability—The difference between two test re-
assembly with forceps. If the deposit on the filter pad is not sults, obtained by the same operator with the same apparatus
evenly distributed, reject the pad and rerun the test after under constant operating conditions on identical test material,
cleaning the membrane filter holder (see 9.2). would in the long run, in normal and correct operation of the
NOTE 12—When multiple tests are carried out, the margin of the pad test method, exceed the following values in only one case in
may be used for sample identification. twenty:
NOTE 13—Some laboratories may contain sufficient airborne contami- Aging Time Repeatability
nation to change results if the air drying period is prolonged. 90 min 22.42 - 0.2130x
11.7 If the deposit on the filter pad is not evenly distributed, 180 min 22.55 - 0.2145x
reject the pad and rerun the test (see 9.2). where:
11.8 Place the test filter on the stack of at least ten unused x = the average of two results in percent reflectance.
filter pads, center the search unit on the filter, and record the
meter value as percent reflectance filter pad rating to one 13.1.2 Reproducibility—The difference between two inde-
decimal place. pendent test results, obtained by different operators working in
different laboratories on identical test material, would in the
11.9 Repeat 11.5-11.8, using the second of two aged fuel long run, in normal and correct operation of the test method,
samples. exceed the following values in only one case in twenty:
12. Report Aging Time Reproducibility
90 min 44.04 - 0.4281x
12.1 Report the following information: 180 min 34.11 - 0.3034x
12.1.1 Sampling date and date of test (see 8.3).
where:
12.1.2 Aging time at 150°C.
12.1.3 Percent reflectance filter pad rating as the average of x = the average of two results in percent reflectance.
duplicate determinations, to the nearest whole percent. 13.2 Bias—Since there is no accepted reference material for
13. Precision and Bias 7 determining the bias for this test method, bias cannot be
determined.
13.1 Precision—The precision statement is based on analy-
sis of five D975 S5000 and five samples of D975 S500 fuels in
14. Keywords
7
Supporting data have been filed at ASTM International Headquarters and may 14.1 fuel insolubles; high temperature stability; middle
be obtained by requesting Research Report RR:D02-1463. distillate fuels; storage stability; thermal stability

APPENDIXES

(Nonmandatory Information)

X1. INTERPRETATION OF RESULTS

X1.1 Test results should be correlated to actual storage or TABLE X1.1 Interpretation of Results
use conditions, or equipment operation, to have maximum Y Search Unit
W Search Unit
utility. In the case of storage stability, results should be checked Relative Stability with Green Filter
% Reflectance
% Reflectance
against longer term, less accelerated test methods.
100-90 100-85
89-80 84-71
X1.2 For internal, contractual, or industry specification | 79-70 70-62
purposes, satisfactory results are partly defined by age of the Decreasing 69-60 61-53
sample at time of testing, by anticipated storage needs, or by Stability 59-50 52-32
↓ 49-0 31-0
equipment needs; all of these vary and may reflect more or less
conservative approaches.
X1.3 Table X1.1 shows an interpretation of test results, X1.4 The Y search unit with green filter has a different
which appears to be generally accepted. Rankings are with spectral response than the W search unit, and on average, gives
respect to relative performance in the test; relevance to use a higher result. Because the sediments on filter pads vary in
applications requires interpretation and judgment. color, the difference between results varies.

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 D6468 − 08
X1.4.1 During the precision program on this test method, solubilizing properties (for example, when a dark light cycle
some laboratories used the W search unit, and a precision oil is commingled with a paraffinic fuel). Staining alone will
statement for its use was developed (see RR:D02-14637). typically not give filter pad ratings with less than 50 %
However, because the result and difference between results reflectance.
over the percent reflectance range varies when obtained with
the two search units, it was agreed that only one should be X1.6 The test method can be used to determine the relative
specified in the test method, to enable generation of compa- performance of additives under conditions of the test. Because
rable results, especially comparable laboratory-to-laboratory results depend on the history of the fuel sample, relative
results. Further, the data suggest that the bias between the two performance is best determined by carrying out comparison
search units is not uniform, so a bias correction cannot be tests in a single batch of samples, prepared and aged together.
recommended. Other reflection meters can be used, but in that X1.7 The test temperature may simulate conditions that
case, the use of a different instrument should be reported, and exist in some equipment where fuel is exposed to temperatures
it should also be reported that a modified test method was used. from 100 to 150°C, or higher, then recycled back to a storage
It would also be appropriate to generate a new table, such as tank.
Table X1.1, which establishes the relevance of the results.
X1.8 This test method is effective to monitor the relative
X1.5 When the fuel is very dark, the filter pad may be thermal stability and possible change in storage stability at a
stained a dark color, yet microscopic examination shows little production site where crude source and process conditions vary
or no particulate matter is present. Fuel color does not over time. Substantial changes can signal a fuel quality
necessarily correlate with performance; however, dark-colored excursion. The test method can also be used to verify that
fuels frequently have oxidation sediment associated with them stabilizing additives have been appropriately added to distillate
and may form sediment if commingled with fuels having poor fuels with marginal stability.

X2. FACTORS WHICH AFFECT THE TEST METHOD

X2.1 Due to the high test temperature and the lack of X2.2 Additives can have positive or negative effects in this
oxygen feed to the test specimen during aging, there is a test, which may or may not be observed in actual storage or
tendency of the test method to give better results with fresh fuel use.
than with the same fuel after it has aged at ambient temperature X2.2.1 The test method tends to give results that amplify the
with oxygen exposure. When tests are carried out on freshly benefits of some stabilizer additives. The benefit of metal
produced fuel, the aging period can be increased to 180 min, or deactivator additive, when fuel contains dissolved copper,
more stringent standards can be imposed on the pad rating to correlates well with less accelerated tests. Effects of dispersant
better reflect change in properties that may result from distri- additives are also well correlated.
bution and storage.
X2.2.2 Some additives exhibit effects on samples aged in
X2.1.1 The choice of fuel stressing (90 min or 180 min) is accordance with this test method, which are not found in other
directed by the specification for which the fuel is evaluated or tests where samples are aged at 100°C or lower. For example,
by the specific requirements of the evaluator. Generally, many fuels will give worse results if alkyl nitrate cetane
stressing for 180 min is a more stringent evaluation of fuel number improver is present. The relevance of these findings is
thermal stability. not entirely clear.

X3. FUEL COLOR

X3.1 Diesel fuel natural color ranges from water white temperatures, is not a reliable measure of fuel quality. None-
(colorless) to dark amber, reflecting the crude oil or the refinery theless, some fuel technologists believe that measurement of
process streams from which the fuel is produced, or both. Color fuel color before and after aging provides useful information.
per se, as determined by Test Method D1500, does not
necessarily reflect suitability of the fuel for its intended use. X3.3 Practitioners of this test method who insist on mea-
There is also no agreement on how to measure fuel color when suring Test Method D1500 color before and after aging should
dye is present. measure unaged fuel color (initial color) after filtration in 11.2
and carry out aged fuel color measurement on the filtrate
X3.2 Change in fuel color (darkening) alone, during storage generated in 11.5 that has been decanted from the vacuum flask
at ambient temperatures or upon accelerated aging at elevated before use of any iso-octane.

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 D6468 − 08
SUMMARY OF CHANGES

Subcommittee D02.14 has identified the location of selected changes to this standard since the last issue
(D6468–06) that may impact the use of this standard.

(1) Revised 6.3, 7.2, 8.3, 9.1, 9.2, 10.1, 10.4, 11.3, and 13.1. (3) Added 8.3.1, X2.1.1, and Note 7.
(2) Deleted original Note 4. (4) Added “Middle” to title (“Middle Distillate Fuels”).

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