Renewable Energy 94 (2016) 466e473

Contents lists available at ScienceDirect

Renewable Energy
journal homepage: www.elsevier.com/locate/renene

The testing of the effects of cooking conditions on the quality of

biodiesel produced from waste cooking oils

an
Tuba Hatice Dog
Ataturk University, Department of Chemical Engineering, 25240, Erzurum, Turkey

a r t i c l e i n f o a b s t r a c t

Article history: In this study, the effects of cooking conditions on the cold ow properties and kinematic viscosity of
Received 9 March 2015 biodiesel produced from cooking oils were investigated. Sunower, corn and canola oils were used as
Received in revised form vegetable oils. Salt content, water content, cooking time and cooking temperature were selected as the
29 February 2016
experimental parameters. Some of the physical properties such as kinematic viscosity, density, cloud
Accepted 25 March 2016
point and pour point were examined. In addition, total polar material contents, heating values and acid
Available online 1 April 2016
values of biodiesel produced from waste cooking oils were analysed. The results of the study revealed
that increase in salt and water content, cooking time and temperature led to deterioration in the physical
Keywords:
Biodiesel
properties and cold ow properties of B100 biodiesel samples from waste cooking oils of sunower, corn
Waste cooking oils and canola oils. On the other hand, the heating values of all biodiesels were found to improve with the
Cooking conditions increasing salt content.
Physical properties 2016 Elsevier Ltd. All rights reserved.

1. Introduction properties of biodiesel. Yaakob et al. suggested that waste cooking

Biodiesel is a fuel produced from the reaction of vegetable or
animal oils in the presence of a catalyst with a short chain alcohol
like methanol or ethanol. The world energy need is increasing,
while the available sources of fossil fuels such as coal and petro-
leum are reducing. Moreover, the utilization of fossil fuels causes
global warming by increasing the effects of greenhouse gases,
signicantly. Biodiesel is biodegradable, non-toxic and environ-
mentally friendly due to low emission proles. Contrary to these
advantages, the most important disadvantage of biodiesel is its
high cost [1,2]. Since vegetable oils are important raw materials in
food industry, their utilization in biodiesel production is not
economical and practical. Waste cooking oils are accumulated in
very large quantities each year in all countries and releasing these
oils into the environment can cause environmental problems and
clogs inside drainage pipes. Therefore, the use of waste cooking oils
for biodiesel production is one of the promising ways.
Important review studies were performed related with biodiesel
production from waste cooking oils. Kulkarni and Dalai [3] said that
undesired products such as free fatty acids and some polymerized
triglycerides formed in vegetable oil during frying could affect
negatively both transesterication reaction and the physical
E-mail address: hatice@atauni.edu.tr.
oil was a promising raw material of biodiesel production [4].
Knothe and Steidley, examined the acid values, viscosities and
fatty acid proles of used frying oils they obtained from 16 local
restaurants. According to the obtained results researchers decided
that used cooking oils are very heterogenous raw material source
for biodiesel production [5].
Zhang et al. developed 4 different process ow charts for bio-
diesel production from waste cooking oil at commercial scale.
Operation conditions and equipment design were obtained in
detail for each process. In the research it was determined that a
system with acid catalyst is technically more convenient compared
to basic one [6].
Studies were also made where optimum conditions of biodiesel
production from waste frying oils were researched. In these studies
the conditions for reaching highest methyl ester product were
determined [7e9].
In some studies various physical and chemical properties of
biodiesel produced from waste frying oil were measured. In these
studies the fuel quality of produced biodiesel was researched
[10e14].
In the present study, the effects of cooking conditions of cooking
oils on the quality of biodiesel produced from waste cooking oils
were investigated. The cloud point (CP), pour point (PP), density,
viscosity, heating value, acid value and total polar materials (TPM)
contents were used as determining parameters of the biodiesel

http://dx.doi.org/10.1016/j.renene.2016.03.088
0960-1481/ 2016 Elsevier Ltd. All rights reserved.
 T.H. Dog
an / Renewable Energy 94 (2016) 466e473 467

quality. Majority of the studies made examines the properties of Table 2

biodiesel produced. However this study focuses on the effects of Experimental parameters during cooking experiments.

waste oil cooking conditions on biodiesel properties. Parameters Values

Salt amount (wt %) 0.22 0.44a 0.88

2. Materials and methods Water amount (v %) 2a 4 8
Time (h) 5a 10 15

Temperature ( C) 100a 160 230
2.1. Materials
a
Constant parameters used when the effects of other parameters were tested.
Sunower, corn and canola oils used in this study were obtained
from a local market in Erzurum, Turkey. The fatty acid composition
transferred to a reactor for biodiesel production. The operations
of these oils was obtained by GS and given in Table 1. The methanol
were repeated for other values determined for effect of salt. Same
and potassium hydroxide catalyst used for biodiesel production
method was followed while examining the effect of each param-
had 99.9% purity. They were provided from Merck and Flake,
eter. Namely while the parameter aimed to be examined was
respectively. Edible salt used in the experiments was supplied from
changed the parameters stated to be constant on Table 2 were not
a local market.
changed.

2.2. Equipment
Cooking experiments were carried out in a 1000 mL at-
bottomed glass balloon. Hot plate magnetic stirrer was used for
stirring and heating. The balloon was placed in boiling stones and a
magnet to prevent the oil explosion. In addition, it was tted with a
condenser to prevent water losses and a digital thermometer was
used for temperature measurement. Experimental parameters
during the cooking experiments were given in Table 2.
Transesterication experiments were performed in a 1000 mL
jacketed glass reactor. A mechanical stirrer, a constant temperature
circulator and a condenser were utilized in order to keep the
methanol amount inside the reactor constant. Experiments were
carried out at atmospheric pressure. Constant parameters, reaction
temperature, reaction time, oil to alcohol ratio and catalyst amount
were dened as 60  C, 1 h, 1:6 (in weight) and 1% KOH (in weight),
respectively.
3. Experimental procedure
Experiments were repeated three times at different times. Av-
erages of standard deviations (ASD) and R2 values were calculated.
R2 values were displayed on gures and ASD were given along with
the labels of gures.
3.1. Cooking experiments
The glass balloon was initially lled with vegetable oil. Water
and edible salt were added in the certain amount. The balloon
contents were heated to the desired temperature and kept at that
temperature for the desired time. For example while examining the
effect of salt content, 500 mL of vegetable oil was placed in a glass
balloon with at bottom surface. After that 2% water by volume and
0.22% salt by weight (initial value of salt amount) were added. On
top of them condenser was added for preventing water loss and a
thermometer for temperature control. The oil was heated at 100  C
for 5 h. The oil which is exposed to cooking conditions was
3.2. Transesterication reaction
The vegetable oil exposed to cooking conditions was placed into
the reactor and heated to 60  C. KOH catalyst dissolved in methanol
was added to the stirred reactor and the reaction started. At the end
of the reaction, the reactor content was taken to a separator funnel
and glycerol phase was separated from the bottom. After three
times washing with deionized water, mixture in the separator
funnel was placed on a rotary evaporator and kept there under
vacuum at 80  C in order to remove residual methanol.
3.3. Analytical methods
Physical properties of the biodiesel products obtained from
waste cooking oil were determined according to related European
standards (EN). After each experiment, pour point (PP), cloud point
(CP) and density (at 15  C) were measured. Kinematic viscosity (at
40  C) and heating value of each sample were determined by using
Koehler kV4000 series viscosimeter and calorimetric bomb IKA C
200, respectively. The acid values of samples were measured
through the titration method using a KOH-ethanol solution and
given Table 3. Additionally, the amount of total polar materials (%
TPM) of each biodiesel sample (B100) at 50  C was analysed by
Testo 270 cooking oil tester. In order to achieve this the biodiesel
sample in which TPM content will be determined, was heated to
50  C. In the sample Testo 270 e the cooking oil determination
device was immersed and directly the TPM percentage was read
from digital screen.
Fatty acid composition of vegetable oils and Fatty acid methyl
ester contents of biodiesel samples were analysed using a Gas
Chromatograph system equipped with an auto-injector (Perkin
Elmer Clarus 680, USA). The BPX-70 capillary column (SGE, Mel-
bourne, Australia, 60 m  0.25 mm i.d., 0.25) was used for the
analysis of FAME. The initial oven temperature was 50  C for 4 min,
and was increased to 230  C at a rate of 4  C/min, then maintained
for 10 min.

Table 1
Fatty acid composition (mass%) of canola, sunower and corn oils.

Fatty acid Canola oil Sunower oil Corn oil

Palmitic C16:0 4.85 27.35 31.72

Stearic C18:0 1.93 60.95 52.42
Oleic C18:1 64.38 0.50 1.17
Linoleic C18:2 19,74 6.54 11.80
Linolenic C18:3 7.05 3.61 2.18
Arachidic C20:0 1.14 0.15 0.27
Behenic C22:0 0.28 0.64 0.15
468 T.H. Dog
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Table 3
The effects on acid value of the cooking conditions.
Acid Value (mgKOH/g)
Salt amount Water amount
(wt%) (V%)
0.22 0.44 0.88 2 4
Canola 0.07 0.10 0.90 0.10 0.29
Sunower 0.13 0.28 0.56 0.28 0.50
Corn 0.13 0.15 0.41 0.15 0.18
4. Results and discussion
In this study, biodiesel (B100) was produced from vegetable oils
exposed to different cooking conditions. Cooking time, cooking
temperature, salt content and water content of sunower, corn and
canola oils were dened as the cooking conditions. Changes in the
physical and cold ow properties of each biodiesel sample were
examined. In this way, the effect of cooking conditions on the
quality of biodiesel was determined. Viscosity, density, CP, PP,
heating value, acid value and TPM contents were used to identify
the quality of biodiesel.
Since high viscosity causes poor combustion and plugging of the
injectors, it is one of the undesired properties for fuels [15]. Similar
to high viscosity, high density is also undesirable due to its negative
impact on fuel consumption and heating value during combustion
process [16].
Cloud point (CP) and pour point (PP) are the most important
cold ow properties of fuels. Cloud point is the temperature at
which the rst wax crystal cloud is observed, while pour point is
dened as the lowest temperature at which fuel starts to ow
under cold storage conditions. Since poor cold ow properties of
fuel generally cause performance problems at cold temperatures,
high CP and PP values affect the quality of biodiesel negatively [17].
The heating value is an important property for vehicles espe-
cially with weight restrictions. In this type of vehicles, high heating
value provides more efcient fuel consumption by using lower
amount of fuel [18].
Acid value is a measurement of free fatty acid content in bio-
diesel. The free fatty acids (FFA) within the oil indicate the
incomplete transesterication or oxidative degradation. Acid value
is one of the important properties effecting biodiesel quality.
Because high acid value speeds up degradation during storage of
biodiesel and decreases the life time of vehicle fuel pump and lters
[7,19].
Due to ongoing reactions during frying some physical and
chemical changed occur in vegetable oil. Basically 3 degradation
reactions are realized in oil; hydrolysis caused by water, oxidation
caused by oxygen and thermal degradation caused by heat [20]. As
a result of all these reactions that may occur at different degrees
and through different mechanisms according to frying conditions,
hundreds of degradation products all of which are in different
structure but all of which have polar character, are formed in frying
oil. Free fatty acids and total polar materials are decomposition
products formed during frying process [21]. Increase in cooking
time and cooking temperature leads to an increase in the amounts
of these products. As a result, this increase in degradation products
deteriorates the physical properties of biodiesel.
The results of the experiments are presented in the following
part.
4.1. The effects of salt content
Salt is usually added on the foods before frying in order to
Cooking time Cooking

(h) Temperature ( C)
8 5 10 15 100 160 230
0.45 0.10 0.16 0.28 0.10 0.30 0.55
1.88 0.28 0.45 0.76 0.28 0.34 0.47
0.36 0.15 0.18 0.26 0.15 0.41 0.61
enhance the avour. Since the salt on food passes through the oil
during frying, the effect of the salt content in the cooking oil on the
physical properties, such as kinematic viscosity, density, CP, PP,
heating value, acid value and TPM contents were investigated. The
results are given as corresponding property versus salt content
(Fig. 1 and Table 3).
It was observed that kinematic viscosity and density of three
samples increased with the increasing salt content in Fig. 1-a and b,
respectively. Similarly, cold ow properties (CP and PP) also
increased (Fig. 1-c, d). An increase of salt would increase the water
activity in the reaction medium. An increase of water increases
hydrolysis, hence FFA production (and decreased yield). This situ-
ation deteriorates the physical and cold ow properties of biodiesel
samples.
As seen in Fig. 1-e, approximately 50 cal/g increase in the
heating value was recorded for three samples with increasing salt
content. It was interesting that the heat value increased with the
increasing salt content. The increase in heat value is considered to
be originated from increase of salt content and polymerized sub-
stances formed as a result of various reactions occurring due to salt
addition. The hydrogen content of these polymerized substances
are considered to cause a higher thermal value to be obtained.
During frying viscosity, density and FFA content of oil increases.
At the same time polar materials and polymeric compounds also
increase in the oil [22]. For this reason, the TPM content provides
healthy evaluations related with amount of occurring degradation
reactions. As shown in Fig. 1-f, TPM values of the three biodiesel
increased nearly at the same ratio. At the same time increase in salt
content caused acid value of all biodiesel samples to increase
(Table 3). As well-known increase in acid value increases the hy-
drolysis of free fatty acids and therefore decreases ester product.
Since the acid value increases with increasing FFAs, it can be said
that the rise in FFA, depending upon the increase in the salt, causes
to increase the acid value of biodiesel. The fatty acid methyl ester
(FAME) composition of the canola biodiesel sample with highest
salt content (0.88 wt%) was analysed in gas chromatograph and
found to be 61.80%.
4.2. The effects of water content
Food is fried after washing. The water in food passes into the oil
during frying. If the frying process is done in a closed vessel, a few
amount of water remains in the oil and the water passes into bio-
diesel produced from this oil. Water can be present in the biodiesel
as dissolved or suspended droplets. Since the presence of water
causes the corrosion in the parts of injection system, biodiesel
should not contain water. Furthermore, the presence of water leads
to sludge formation and acidication of the biodiesel due to the
microbiological formation [23,24].
The effects of water content in the cooking oil on the kinematic
viscosity, density, CP, PP, heating value, acid value and TPM contents
of biodiesel produced from these oils were tested. The results are
given as corresponding property versus water content in Fig. 2 and
 T.H. Dog
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Fig. 1. The effects of salt content on viscosity, 0.15 ASD (a), density, 1.5 ASD (b), CP, 1 ASD (c), PP, 1 ASD (d), heating value, 30 ASD (e) and TPM%, 0.5 ASD (f) of cooking oil
biodiesels.

Table 3.
Kinematic viscosity (Fig. 2-a) and density (Fig. 2-b) of all bio-
diesel samples increased with the increasing water content.
Maximum increase in kinematic viscosity was recorded for corn oil
from 4.8 mm2/s to 12 mm2/s.
Similar results obtained from experiments were indicated for CP
and PP values of the three biodiesel in Fig. 2-c,d. Heating value of
the biodiesel decreased with the increasing amount of water in
cooking oils. Minimum decrease was found for sunower oil from
9409 cal/g to 9364 (Fig. 2-e). Similarly, the slight increase in TPM of
the three biodiesels with the increasing water content is shown in
Fig. 2-f.
In the study performed by Park et al. it was observed that FAME
content decreased by increasing water in oil increases the hydro-
lysis of oil and accordingly free fatty acids also increase. FFA and
water signicantly and negatively affect transesterication reaction
and decreases FAME content [25]. When Table 3 was examined it
was observed that increasing water amount increased the acid
value of all biodiesel samples. FFAs, which are the products of hy-
drolysis reaction, increase with increasing amount of water in oil.
As a result, the higher FFAs are responsible for the higher acid value
of biodiesel. It should be realized that increase in free fatty acids
within biodiesel increases both acid and viscosity values. Because
viscosity of FFA is signicantly higher than esters [19,26]. Besides
formation of polymeric and dimeric acids and glycerin in waste
cooking oils increases the density of the oil while increasing the
viscosity [23].
As a result, minimum change in the kinematic viscosity, density,
CP, PP, heating value and TPM values were obtained for sunower
oil (Fig. 2-a, b, c, d, e, and f). The result reveals that the properties of
the waste sunower biodiesel have minimal deterioration.
470 T.H. Dog
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Fig. 2. The effects of water content on viscosity, 0.15 ASD (a), density, 1.5 ASD (b), CP, 1 ASD (c), PP, 1 ASD (d), heating value, 30 ASD (e) and TPM%, 0.5 ASD (f) of cooking oil
biodiesels.
4.3. The effects of cooking time
In this part of the study, the effects of cooking time on the
physical properties of biodiesel produced from vegetable oils were
examined. Duration of the cooking time was considered as 5 h.
Repeated cooking increases the deterioration of sunower, corn
and canola oils. The results given as corresponding property versus
cooking time are presented in Fig. 3 and Table 3.
Kinematic viscosity and density of all biodiesel samples
increased with the increasing cooking time and the highest in-
crease was recorded for waste canola biodiesel in Fig. 3-a and b.
Similarly, the CP and PP values of the three biodiesels also increased
with the increasing cooking time. Maximum increase was found for
sunower biodiesel. PP value increased from 10.3  C to 5.5  C,
while CP value of sunower biodiesel increased from 6  C
to 1.2  C (Fig. 3-c and d).
Fig. 3e indicates that the heating value of all biodiesels
decreased slightly with the increasing cooking time. As cooking
period increases free fatty acids, polar and polymer materials in-
creases [22,27,28]. For this reason, while increase in cooking period
decreases methyl ester product, it may also cause heat value to
decrease a bit. Besides it was demonstrated in the studies per-
formed that length of the carbon chain of the fatty acids increases
the heat value. Increase of oxygen amount in oil decreases heat
value [11,29,30]. In addition, the increase in TPM values of three
biodiesel samples with the increasing cooking time is shown in
Fig. 3-f. As expected increase in cooking period, increased acid
values (Table 3). The concentration of polar and polymeric mate-
rials with high molecular weights in oil increases with increasing
cooking time. Since this increase causes to increase in FFAs, the acid
value of biodiesel also increases.
 T.H. Dog
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Fig. 3. The effects of cooking time on viscosity, 0.15 ASD (a), density, 1.5 ASD (b), CP, 1 ASD (c), PP, 1 ASD (d), heating value, 30 ASD (e) and TPM%, 0.5 ASD (f) of cooking oil
biodiesels.

4.4. The effects of cooking temperature
The effects of the cooking temperature of the cooking oil on the
kinematic viscosity, density, CP, PP, heating value, acid value and
TPM contents of biodiesels produced from sunower, corn, and
canola oils were studied. The results are given as corresponding
property versus cooking temperature in Fig. 4 and Table 3.
An undesirable increase in the kinematic viscosity of the three
samples with the increasing cooking temperature is presented in
Fig. 4-a. Similarly, as seen in Fig. 4b, c, and d, the density, CP and PP
values of the three biodiesels also increased with the increasing
cooking temperature. The highest increase in density, CP and PP
values was found for sunower biodiesel. The density of sunower
biodiesel increased from 902 kg/m3 to 920 kg/m3 (Fig. 4-b, c and d).
It was observed that the heating value of all biodiesels decreased
with the increasing cooking temperature. Maximum decrease was
obtained for canola biodiesel from 9371 cal/g to 9300 cal/g (Fig. 4-
e). High frying temperature speeds up the thermal oxidation and
polymerization of the oil [31]. The studies performed demonstrated
that increase in cooking temperature increased the polymer
amount as well [32,33]. Increase in cooking temperature causes FFA
amount to increase and also product amount to decrease at the
same time. This degradation occurring in oil decreases biodiesel
quality and may negatively effect the heat value. As shown in Fig. 4-
f, the TPM amount of the three biodiesel samples increased with
the increasing cooking temperature and the highest increase was
recorded for sunower biodiesel from 22% to 29%. Besides as the
cooking temperature increased, acid value of all three biodiesel
samples increased as well (Table 3). High cooking temperature is
one of the parameters increasing FFAs formation. These thermal
degradation products (FFAs) increase the acid value of biodiesel.
The FAME composition of the canola biodiesel sample with highest
472 T.H. Dog
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Fig. 4. The effects of cooking temperature on viscosity, 0.15 ASD (a), density, 1.5 ASD (b), CP, 1 ASD (c), PP, 1 ASD (d), heating value, 30 ASD (e) and TPM%, 0.5 ASD (f) of
cooking oil biodiesels.

cooking temperature (23O C) was analysed in gas chromatograph
and found to be 76.39%.
As a result, maximum deterioration in density, CP, PP, and TPM
values was found for sunower biodiesel with the increasing
cooking temperature.
5. Conclusions
Physical properties such as kinematic viscosity, density, CP, PP
and heating value, and TPM contents and acid values of biodiesels
produced from wastes frying of canola, sunower and corn oils
signicantly deteriorate when salt content, water content, cooking
time and cooking temperature of cooking oils are increased. On the
other hand, a small increase in the heating value with the
increasing amount of salt is another important nding of the study.
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