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INVESTIGATION OF BIODIESEL THERMAL STABILITY

UNDER SIMULATED IN-USE CONDITIONS
A. Monyem, M. Canakci, J. H. Van Gerpen

ABSTRACT. Biodiesel is an alternative diesel fuel produced by transesterification of vegetable oils or animal fats. While
biodiesel provides numerous environmental benefits such as reduced exhaust emissions, it is more prone to oxidation than
petroleum-based diesel fuel and this can alter its properties. When oxidation occurs at ordinary temperatures, the initial
products are hydroperoxides. As the oxidation continues, the peroxides may split and form aldehydes, ketones, and short
chain acids that produce unpleasant odors. Sediment and gums are formed through polymerization of the peroxides and
can cause fuel filter plugging. The objective of this study was to relate the chemical and physical processes associated
with biodiesel oxidation to the conditions that affect diesel fuel system performance. A relationship was sought between
the test that is used by the engine industry to define engine fuel stability requirements (ASTM D2274) and the tests used by
the fats and oils industry to characterize oxidation (Peroxide Value and Acid Value). It was found during the course of this
study that the ASTM fuel stability method is not suitable for biodiesel. While oxidation causes the fuel viscosity to
increase, fuel filter plugging was not necessarily a natural consequence of biodiesel oxidation even when the fuel was
oxidized to a level beyond what would be observed in practice. The effect of fuel temperature and blending with diesel fuel
on the oxidation was investigated and the interrelationship between the fuel’s acid value and viscosity is shown.
Keywords. Diesel, Energy, Engines, Fuel, Oil, Oilseed, Soybean oil.

M
any researchers have investigated vegetable cold flow properties. Saturated compounds are less prone
oils as an alternative fuel for diesel engines to oxidation than unsaturated compounds but they
(Goering et al., 1982; Bagby et al., 1987; crystallize at unacceptably high temperatures. Vegetable
Engelman et al., 1978; Hawkins et al., 1983). oils are oxidized through contact with molecular oxygen in
Most of this research has shown that using raw vegetable the air. Oxidation reactions that occur without any outside
oils for diesel engines can cause numerous problems influence are called autoxidation. Autoxidation is initiated
(Korus et al., 1982; Lague et al., 1988). The increased and propagated by free radicals reacting with methylene -
viscosity, low volatility, and poor cold flow properties of CH2- groups that are adjacent to double bonds (Stauffer,
vegetable oils lead to severe engine deposits, injector 1996). This is why the rate of oxidation is so strongly
coking, and piston ring sticking (Perkins et al., 1991; affected by the degree of saturation of the oil. Some
Pestes and Stanislao, 1984; Clark et al., 1984; Vellguth, vegetable oils contain natural antioxidants, such as
1983). However, these effects can be reduced or eliminated vitamin E (tocopherol). These antioxidants react with the
through transesterification of the vegetable oil to form active free radicals producing a species of low reactivity
monoesters (Perkins et al., 1991; Zhang et al., 1988). The that does not initiate new reaction chains. However, as free
process of transesterification removes glycerol from the radicals continue to form, eventually all the antioxidant
triglycerides and replaces it with radicals from the alcohol will be consumed, and then oxidation will proceed rapidly.
used for the conversion process (Kusy, 1982). This process Hydroperoxides are the initial products of oxidation at
decreases the fuel’s viscosity but maintains its cetane ordinary temperatures. They are very unstable and have a
number and heating value. These alkyl monoesters of tendency to attack elastomers. In addition, hydroperoxides
vegetable oils or animal fats have come to be known as can polymerize and form insoluble gums and sediments
biodiesel. The most common form of biodiesel in the that increase viscosity and plug fuel filters (Clark et al.,
United States is made with methanol and soybean oil and is 1984). These peroxides split and form aldehydes, ketones,
known as soy methyl ester, or methyl soyate. and finally shorter chain acids. The level of these acids is
One drawback of biodiesel is that there is an inverse measured by the acid value. However, no research has yet
relationship between biodiesel’s tendency to oxidize and its been conducted to determine the maximum degree of
oxidation allowable for fuel to be used in diesel engines.
The objective of this study was to monitor the oxidation
Article has been reviewed and approved for publication by the Power of biodiesel under conditions that are similar to those
& Machinery Division of ASAE. encountered in use. Then the chemical and physical
The authors are Abdul Monyem, Design Engineer, Caterpillar Inc., processes associated with biodiesel oxidation were related
Peoria, Ill.; Mustafa Canakci, Research Assistant, and Jon H. Van to the conditions that affect fuel system performance. To
Gerpen, ASAE Member Engineer, Associate Professor, Department of
Mechanical Engineering, Iowa State University, Ames, Iowa.
support this objective a connection was sought between the
Corresponding author: Jon Van Gerpen, Iowa State University, ASTM (American Society for Testing and Materials)
Department of Mechanical Engineering, Ames, IA 50011, phone: D 2274 fuel stability tests (ASTM, 1998) and the AOCS
515.294.5563, fax: 515.294.3261, e-mail: <[email protected]>. (American Oil Chemists’ Society) tests for peroxides and

Applied Engineering in Agriculture

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acids. ASTM D2274 measures sediment and gum barrel. The biodiesel fuel was pumped from the barrel and
formation in diesel fuels, and AOCS Cd 8-53 and Cd 3a-63 pushed through the fuel filter before returning to the barrel.
measure the peroxides and acids formed by fuel oxidation A three-way valve was used to take fuel samples at a point
(AOCS, 1998a,b). The Peroxide Value is expressed as downstream of the filter. An electric heating tape was
milliequivalents of peroxide per kilogram of sample. The wrapped around the barrel to control the fuel temperature.
Acid Value characterizes the amount of organic acids In this experiment, a total of four test rigs using 208 L
produced by oxidation and is expressed as the amount of (55 gal) barrels and a single test rig with a 19 L (5 gal)
potassium hydroxide required to neutralize the acids. stainless steel container were used. Two of the barrels were
During the course of this project it was found that maintained at a controlled temperature at 60°C (140°F) and
ASTM D2274 was not appropriate for use with biodiesel. the other two were at room temperature. The 19-L test rig
As will be described later, the technique used to isolate was maintained at 60°C. The flow rate was kept constant
gums and sediment in this method does not adequately for all of the tests at 5 kg/min (11 lb/min), a typical flow
distinguish between these compounds and biodiesel. It was rate for an engine circulating pump. The fuel flow rate was
also found that fuel filter plugging is not an inevitable measured periodically by switching the three-way valve
consequence of biodiesel oxidation. In contrast to an earlier following the filter to direct the flow into a graduated
project by other researchers (Clark et al., 1984), no cylinder rather than returning it to the barrel. A stop watch
tendency to fuel filter plugging was found in this project, was used to determine the average flow rate.
even with highly oxidized biodiesel. The conditions in the test rig were intended to simulate
This article describes the chemical changes that were the conditions that fuel would be exposed to while
observed in the biodiesel as it oxidized under simulated in- circulating through a diesel fuel system. The temperature of
use conditions. The effect of temperature and blending with 60°C was chosen because this is a reasonable value for fuel
diesel fuel is also discussed. Since ASTM D2274 is not circulating through a diesel engine fuel system. The test
able to characterize the stability of biodiesel a new test should be considered as severe because the fuel is
procedure is needed. The data presented here will support recirculated for a longer time than would normally be
efforts to develop this procedure. A companion article encountered in practice. Originally, the test duration was
presents the results of biodiesel oxidation under controlled intended to correspond to the actual length of time that fuel
laboratory conditions where phenomena occur that were could be expected to recirculate before being injected and
not observed during the simulated in-use testing burned in the engine. However, when no indication of fuel
(Canakci et al., 1999). filter plugging was found, the tests were extended in an
attempt to identify conditions that might cause filter
plugging.
EQUIPMENT AND PROCEDURE A data logging system was used to measure the time,
To simulate the in-use conditions experienced by fuel in temperature, and differential pressure across the filter every
a diesel fuel system, a test stand following Society of five minutes for each test rig. Fuel samples were initially
Automotive Engineers (SAE) standard J905 (SAE, 1995) taken every day, however, after a few days, the samples
for fuel filter testing was constructed. A schematic of the were taken every two days.
test stand is shown in figure 1. A Holley model 12-802 The biodiesel used for these tests was purchased from
electric fuel pump followed by a Fleetguard model FS1001 NOPEC Corporation of Lakeland, Florida. The diesel fuel
fuel filter was attached to the top of a 208 L (55 gallon) was a commercial No. 2 low sulfur diesel fuel. The
laboratory analysis of these two fuels is shown in tables 1
and 2. As mentioned earlier, the peroxide value was
measured with AOCS method Cd 8-53 and the acid value
was measured with AOCS method Cd 3a-63. These
methods are both based on titration and were assumed to be
applicable to petroleum-based fuels. Since similar ASTM

Table 1. Analysis of the biodiesel fuel*

Fatty Acid Composition
Palmitic (16:0) 10.76%
Stearic (18:0) 4.37%
Oleic (18:1) 24.13%
Linoleic (18:2) 51.83%
Linolenic (18:3) 6.81%
Free glycerin (%) 0.004
Monoglycerides (%) 0.352
Diglycerides (%) 0.132
Triglycerides (%) 0.152
Total glycerin (%) 0.131
Cetane number (D613) 51.1
Lower heating value (kJ/kg) 37272
% Sulfur 0.005
% Carbon 76.14
% Hydrogen 11.75
Viscosity (cSt) 4.63
Figure 1–Schematic diagram of the fuel filter test rig. * All percentages are by weight.

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Table 2. Analysis of no. 2 diesel fuel*

% Carbon 86.23%
% Hydrogen 13.14%
% Sulfur 0.034%
Heat of combustion
Gross (kJ/kg) 45504
Net (kJ/kg) 42715
Hydrocarbon types
Saturates (%) 64.1
Olefins (%) 4.9
Aromatics (%) 31.0
* All percentages are by weight.

methods are available for petroleum fuels (D664, D3703)

this assumption should be valid.
In order to understand the effect of oxidation on the
Figure 2–Pressure drop across the fuel filter for 100% biodiesel at
properties of biodiesel fuel, five tests were conducted using 60°C.
the fuel filter test apparatus. Two of them were with 20%
and 50% biodiesel in No. 2 diesel fuel (by weight) at 60°C
(140°F). Two other tests were conducted with 20% and
50% biodiesel at room temperature (23°C, 73°F). These
four tests were conducted in 208 L (55 gal) barrels each
containing 125 L (33 gal) of fuel. The final test was 100%
biodiesel at 60°C in the 19 L (5 gal) stainless steel
container with 5 kg (11 kg) of biodiesel. In general, all of
the tests were continued until the fuel pump failed, usually
by seizure. The duration varied from 38 days for the 60°C
test of 100% biodiesel to 190 days for the room
temperature test of 20% biodiesel. The failure of these
pumps should not be interpreted as an indication of the
quality of the pumps or any incompatibility between the
pumps and biodiesel. During the test the flow rate was
monitored and as it dropped due to increased fuel viscosity,
the voltage applied to the pump was raised to compensate.
Generally, by the end of the test, the voltage applied to the Figure 3–Effect of oxidation on the peroxide value (PV) of biodiesel.
pump was above the manufacturers recommendations and
this was the probable cause of failure.
initial rise in PV and the subsequent decline. The total test
duration here is clearly beyond what would occur in actual
RESULTS AND DISCUSSION practice. The test was continued to gain a complete
In this section, the effect of oxidation on the peroxide understanding of the processes that may occur in the fuel as
value, acid value, and viscosity of biodiesel are presented. it progresses from unoxidized to highly oxidized fuel. The
These properties characterize the chemical changes oxidation process in an engine fuel system may be
occurring in the biodiesel as it oxidizes. One expected accelerated compared with this experiment if there is a
product of the fuel oxidation was the production of higher degree of aeration. Other test results have shown
sediment and gum. This sediment and gum should be that with a high level of aeration, the fuel can oxidize in a
collected by the fuel filter and cause the pressure drop few hours at 60°C. Another reason for the extended testing
across the filter to rise. A sample case of 100% biodiesel at was to determine whether fuel filter plugging would occur.
60°C (140°F) is shown in figure 2. The increase in the No instances of plugged fuel filters were observed in this
pressure drop across the filter was relatively small for all of test program.
the cases studied in this project. Miyashita et al. (1988) investigated the autoxidation
rates of various esters of safflower oil. They found that the
EFFECT OF OXIDATION ON THE PEROXIDE VALUE OF peroxide value increased rapidly after the induction period,
BIODIESEL but then decreased as was found in this study. However,
The peroxide values measured for all five tests are they found the maximum peroxide value to be about
shown in figure 3. In all cases, the peroxide value (PV) 2000 meq/kg ester. The reason for the higher PV is not
rises to a level between 300 and 400 meq/kg ester and then known but they did use a different method, the
drops off. The three cases at 60°C went through this Calorimetric Iodine method (Takagi et al., 1978), to
process of rise and fall of PV within the first 1000 h with measure the peroxide value. Gan et al. (1995) investigated
the rise in PV for the 50% and 100% biodiesel occurring the effects of oxidation on the methyl ester of palm olein.
within the first 50 h. The 20% blend rose more slowly but They recorded the maximum peroxide value to be about
followed the same general process. The two runs at room 300 meq/kg ester after 288 h, which was close to that
temperature were similar but much slower, both for the observed in this experiment.

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The reason the PV reaches a maximum and then drops EFFECT OF OXIDATION ON THE VISCOSITY OF BIODIESEL
off may be due to the solubility of oxygen in the fuel. Figure 5 shows that the viscosity of all the blends
When the induction period is over, the oxidation proceeds increased with time. The blends containing higher fractions
rapidly consuming all of the oxygen that is dissolved in the of biodiesel and at higher temperatures increased more
ester. The peroxides formed are subsequently converted to rapidly. The 50% and 100% biodiesel at 60°C had rapid
aldehydes, ketones, and acids. When the dissolved oxygen increases in viscosity until the time where the rate of
is consumed, the peroxide formation rate drops off to the increase of acid value was a maximum. Then the viscosity
rate that can be sustained by diffusion of O2 into the ester increased more slowly. The data for the 50% blend at room
from the air surface. If this rate is below the rate at which temperature demonstrated the unusual behavior of having a
peroxides are converted to aldehydes and ketones, the peak at about 1300 h and then leveling off. This anomalous
concentration of peroxides will remain low. behavior has not been explained.

EFFECT OF OXIDATION ON THE ACID VALUE OF BIODIESEL INTERRELATIONSHIP BETWEEN ACID VALUE AND
The results of the acid value measurements for the tests VISCOSITY
described earlier are shown in figure 4. The acid value for Figure 6 shows the correlation between acid value and
all the blends increased with time, but the rates of increase viscosity. For the 20% biodiesel at 60°C (140°F) and at
were different. It can be seen in figures 3 and 4 that the room temperature, the viscosity versus acid value curves
acid value starts to increase at a slightly later time than coincide, but the acid value did not increase to as high a
when the peroxide value starts to rise. The rate of increase value for the room temperature case by the time the test
of the acid value is higher until the point where the was terminated. The coincidence of the 20% blend lines
peroxide value returns to a low value. Beyond this point supports the hypothesis that there is a coupling between the
the acid value increases more slowly indicating a slower reactions that form the acid compounds and the
rate of oxidation. This behavior supports the hypothesis polymerization reactions that increase the viscosity. The
proposed earlier for an oxidation rate controlled by oxygen 50% blend lines also coincide for the initial portion of the
diffusion. oxidation process but when the anomaly mentioned earlier
occurred, and the viscosity decreased, the curves diverged.

ASTM D2274-94 TEST METHOD FOR OXIDATIVE

STABILITY TEST
The standard method to measure the thermal and
oxidative stability of diesel fuels is ASTM (American
Society for Testing and Materials) D2274 (ASTM, 1998).
The method uses accelerated oxidizing conditions to
determine the mass of insoluble material formed by the
fuel oxidation. A 300 mL (0.079 gal) sample of fuel is held
at 95°C (203°F) for 16 h while pure oxygen is bubbled
through it at the rate of 3 L/h. Then the sample is cooled to
approximately room temperature before filtering to collect
insoluble material. Adherent insolubles are removed from
the oxidation cell and associated glassware with a solvent
that is evaporated to obtain the quantity of adherent
insolubles. The sum of the filterable and adherent
insolubles is the total insolubles and is expressed as
milligrams per 100 mL of fuel. The prescribed filter media
Figure 4–The effect of oxidation on the acid value (AV) of biodiesel.

Figure 6–The relation between viscosity and acid value (AV) for
Figure 5–The effect of oxidation on the viscosity of biodiesel. biodiesel blends.

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are 47 mm (1.85 in.) diameter cellulose ester membranes Additional testing was performed to determine whether
with a pore size of 0.8 µm (3.15 × 10 –5 in.). The method the filter weight gain with the biodiesel could have been
requires two filters with one stacked on top of the other. caused by contaminants. The amount of biodiesel was
The bottom filter is used as a blank and the difference varied, and different techniques were used to filter and
between the top and bottom filters is the filterable preclean the biodiesel before it entered the filters. Different
insoluble. The ASTM procedure needed to be modified for solvents, including hexane and toluene were tried with the
this test because finding a matched pair of filters is very same results. Other, more polar, solvents might be more
difficult. This problem was accommodated by weighing the effective at removing the biodiesel but they would also
top (sample) and bottom (blank) filters before and after tend to remove the gums and sediments the test is used to
filtration of the sample. measure.
ASTM D2274 was never fully applied to biodiesel in Another approach was to increase the number of times
this study because preliminary testing showed that the filter the filters were washed with isooctane from 3 to 10. When
washing procedures were not effective. In an effort to this was performed the weight change of the filters was
validate the method, 300 mL of previously filtered much smaller, although it was still positive. This further
biodiesel from a newly opened barrel of methyl soyate was confirmed that inadequate filter washing was the problem.
poured through the filters. This was clean fuel that should Washing the filters with this much isooctane was not
have contained no insoluble material. After filtration, three considered to be an acceptable method because it was a
separate 50 mL volumes of isooctane were used to rinse the significant departure from the ASTM procedure and this
filter assembly. The two filters were dried at 80°C for amount of isooctane could also remove a portion of the
30 min and then cooled at room temperature for another gums and sediments that are to be measured. The type of
30 min before weighing. The results of this initial filter used was also changed. Gelman type AE glass fiber
validation test are shown as Test No. 1 in table 3. The top filters were used and retained even more biodiesel than the
and bottom filters had weight gains of 0.01478 g and membrane filters specified in the ASTM method. At this
0.01501 g, respectively. The total filterable insoluble for point it was determined that ASTM D2274 was not
this test would be the difference between these two weights appropriate for use with biodiesel and further testing was
and was – 0.00023 g or – 0.00008 g/100 mL fuel which terminated.
could be taken as an indication of little or no sediment
formation. However, the large increase in weight for the
blank filter is suspicious because it indicates that the CONCLUSIONS
biodiesel was not removed from the filters. Subsequent The original objective of this project was to relate the
repetitions with biodiesel gave approximately the same ASTM test procedures for fuel oxidation and stability to
results. the AOCS test procedures and to the needs of the engine.
Test No. 2 shown in table 3, used the same procedure as During the course of the project it was found that the
Test No. 1 except that the sample was clean No. 2 diesel standard ASTM procedure for characterizing the oxidative
fuel. Instead of gaining weight as occurred during the stability of diesel fuel (ASTM D2274) is not appropriate
methyl soyate test, both the top and bottom filters lost a for biodiesel. The original expectation that the primary
small amount of weight. This expected result was probably obstacle to using oxidized biodiesel in an engine would be
caused by the isooctane washing a small amount of organic fuel filter plugging was also found to be incorrect. Long-
material from the filter medium. It was the primary purpose term testing with biodiesel that had been oxidized well
for including the blank. The weight change of the top filter beyond what would be encountered in practice showed no
was –0.00051 g and for the bottom was –0.00023 g so the instances of fuel filter plugging.
filterable insoluble was –0.00009 g/100 mL fuel. These Quantitative results showing the chemical and physical
results indicate that the isooctane washing procedure was changes that occur in the fuel when it oxidizes were
effective in removing the diesel fuel from the filters. This presented. The following conclusions can be drawn about
positive result with diesel fuel also showed that the the oxidation process of biodiesel.
laboratory techniques used for the test were valid. 1. The oxidation of biodiesel (SME) occurs more
rapidly at higher temperatures. Dilution with diesel
fuel slows the biodiesel oxidation rate.
Table 3. Filterable insoluble for different fuels* 2. The maximum peroxide value observed for any of
Test No. 1 Test No. 2 the fuels was between 300 and 400 meq/kg ester.
The peroxide value rose to the maximum level and
Fuel Biodiesel No. 2 Diesel
then dropped off.
Amount of fuel filtered (mL) 300 300 3. The induction period varies for different blend levels
After filtering 1.09388 1.07566 with 100% biodiesel having a shorter induction
Top filter weight (g) Before 1.07910 1.07617 period than the blends.
Difference 0.01478 –0.00051 4. The initial rate of increase of acid value was higher
After filtering 1.09335 1.08359 until the point where the peroxide value dropped off,
Bottom filter weight (g) Before 1.07834 1.08382 then the rate of increase of the acid value was lower.
Difference 0.01501 –0.00023 5. A strong correlation was found between acid value
Total filterable insoluble (g) –0.00023 –0.00028 and viscosity. The viscosity increased with time for
Filterable insoluble (g/100mL) –0.00008 –0.00009 all blends of biodiesel and diesel fuel.
* Filters washed three times each with 50 mL of isooctane and 83 kPa of
vacuum.

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378 APPLIED ENGINEERING IN AGRICULTURE