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Procedia - Social and Behavioral Sciences 195 (2015) 2492 – 2500

World Conference on Technology, Innovation and Entrepreneurship

Determination of transesterification reaction parameters giving the

lowest viscosity waste cooking oil biodiesel
Atilla Bilgina, Mert Gülümb*, İhsan Koyuncuogluc, Elif Nacd, Abdülvahap Cakmake
a, b ,c, d ,e Karadeniz Technical University, Faculty of Engineering, Department of Mechanical Engineering, Trabzon 61080, Turkey

Abstract

This study aims determination of transesterification reaction parameters to produce the lowest kinematic viscosity waste
cooking oil biodiesel by using sodium hydroxide (NaOH) as catalyst and ethanol (C 2H5OH) as alcohol. For this purpose, the
individual effects of main reaction parameters such as catalyst concentration (0.50-1.75 ), reaction temperature (60-90 ),
reaction time (60-150 min.) and alcohol/oil molar ratio (6:1-15:1) on the kinematic viscosities of produced biodiesels were
investigated, respectively. According to results, reaction parameters giving the lowest kinematic viscosity of 4.387 were
determined as 1.25 catalyst concentration, 70 reaction temperature, 120 minutes reaction time and 12:1 alcohol/oil molar
ratio.

©
© 2015
2015TheTheAuthors. Published
Authors. by by
Published Elsevier Ltd. Ltd.
Elsevier This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
Peer-review under responsibility of Istanbul University.
Peer-review under responsibility of Istanbul Univeristy.

Keywords: Waste cooking oil biodiesel, transesterification, viscosity, ethanol, sodium hydroxide

1. Introduction

Increasing prices and diminishing known supplies of fossil fuels, and global warming have lead to international
interest in developing alternative fuel for engines (Salvi and Panwar, 2012; Alberici et al., 2012). Biodiesel, which is
a substitute fuel made up of mono-alkyl esters of long-chain fatty acids prepared from renewable vegetable oils or
animal fats as per the American Society for Testing and Materials (ASTM), has fascinated considerable interest as a
renewable alternative fuel for diesel engines (Shah et al., 2013). Biodiesel has the following general advantages:

*Corresponding author. Tel.: +90 462 377 41 30; fax: +90 462 377 33 36.
E-mail address: gulum@ktu.edu.tr

1877-0428 © 2015 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY-NC-ND license
(http://creativecommons.org/licenses/by-nc-nd/4.0/).
Peer-review under responsibility of Istanbul Univeristy.
doi:10.1016/j.sbspro.2015.06.318
 Atilla Bilgin et al. / Procedia - Social and Behavioral Sciences 195 (2015) 2492 – 2500 2493

(1) It is an oxygenated fuel which contains about 10-12 oxygen by weight in molecular structure, and has higher
cetane number than petro-diesel fuel (here after referred as diesel fuel). These facts lead to better ignition quality and
complete combustion. Thus the use of biodiesel instead of the diesel fuel significantly reduces the exhaust emissions
such as carbon dioxide (CO), unburned hydrocarbons (HC) and smoke. Also, being a free-sulfur fuel, biodiesel leads
to zero sulfur oxide (SOx) emissions (Salvi and Panwar, 2012; Alberici et al., 2012; Basha and Gopal, 2012; Borges
and Diaz, 2013). (2) It is clean, biodegradable and non-toxic fuel, being beneficial for reservoirs, lakes, marine life
and other environmentally sensitive places (Vicente et al., 2008). (3) It displays lubricating properties superior to
diesel fuel, reducing premature wearing of fuel pumps (Alberici et al., 2012; Joshi and Pegg, 2007). (4) It has the
potential to relieve the country’s dependence on foreign energy sources since it can be produced renewable and
domestic feedstock (Yuan et al., 2003). (5) The flash point temperature of biodiesel is higher than that of diesel fuel
which makes it safer regarding to the storage and transport (Alptekin and Canakci, 2008). (6) Biodiesel-diesel fuel
blends or even pure biodiesel can be used in diesel engines with small modifications. Taking these advantages into
consideration, it can be said that biodiesel is ideal fuel for diesel engines. However, biodiesel has some
disadvantages such as poor low-temperature flow properties, higher viscosity and nitrogen-oxides (NOx) emissions
and lower energy content (Yusuf et al., 2011). Also, the biodiesel produced from oils, no matter if it is neat vegetable
oil or animal fat, is usually more expensive than diesel fuel from 10 to 50 . Therefore, the high cost of biodiesel
is the major obstacle for its commercialization (Leung and Guo, 2006).
Homogeneous catalyzed transesterification reaction has been commonly used to produce biodiesel. Sodium
(NaOH) and potassium hydroxide (KOH) are generally preferred for this reaction in literature. Some studies in this
type are summarized as following.
In the study performed by Encinar and his colleagues (2002), production of biodiesel from Cynara cardunculus L
was carried out by using ethanol as alcohol and different catalysts (sodium and potassium hydroxide). The operation
variables for reaction temperature, catalyst concentration and ethanol/oil molar ratio were ranged as 25-75 , 0.25-
1.50 wt and 3:1-15:1, respectively. The optimum parameters giving maximum biodiesel yield were found as
ethanol/oil molar ratio 12:1, sodium hydroxide as catalyst (1.00 wt ) and 75 temperature. Zhang and his
colleagues (2008) investigated the optimum conditions of two stage biodiesel production from Zanthoxylum
bungeanum seed oil having high free fatty acids. The acid value of the oil was reduced from 45.51 mg KOH/g to
1.16 mg KOH/g by first stage acid catalyzed esterification reaction, performed with methyl alcohol/oil molar ratio of
24:1, sulfuric acid/oil weight ratio of 2.00 , reaction temperature of 60 and reaction time of 80 min. In the second
stage, the pretreated oil was used for alkali-catalyzed transesterification and then the biodiesel having yield of higher
than 98 was produced at the end of the reaction. El-Sabagh and his colleagues (2011) determined the optimum
conditions of biodiesel production from waste frying oil. The transesterification process was carried out by using
four types alcohol (methanol, ethanol, 1-propanol and 1-butanol). According to experimental results, when
methanol/oil molar ratio of 6:1 and sodium hydroxide/oil weight ratio of 0.40 were used, maximum ester yield
was obtained as 87 wt . Also, the researchers blended the produced optimum biodiesel and diesel fuel at different
volume ratios (10, 15 and 20 ) to improve fuel properties of the biodiesel. Gülüm and Bilgin (2014) determined the
production parameters for the producible lowest viscosity corn oil biodiesel by using sodium hydroxide (NaOH) as
catalyst and methanol (CH3OH) as alcohol. The effects of main production parameters that influence the
transesterification reaction such as catalyst amount, reaction temperature, reaction time, alcohol/oil molar ratio on
the dynamic and kinematic viscosity of produced corn oil biodiesel was investigated. From the results obtained,
production parameters that give the lowest viscosity was determined as 0.90 catalyst amount, 50 reaction
temperature, 60 minute reaction time and 9:1 alcohol/oil molar ratio. Gülüm and Bilgin (2015) investigated densities
of commercially available petro-diesel fuel and its blends with corn oil biodiesel. The corn oil biodiesel was
produced according to previously determined optimum parameters such as 0.90 0 catalyst concentration, 9:1 methyl
alcohol/oil molar ratio, 50 reaction temperature and 60 minute reaction time. The effects of temperature ( ) and
biodiesel percentage in blend ( ) on the densities of blends were examined. The blends (B5, B10, B15, B20, B50
and B75) were prepared on a volume basis and their densities were measured by following ISO test method at
temperatures of 10, 15, 20, 30 and 40 . New one- and two-dimensional equations were fitted to the measurements
for identifying of variations of densities with respect to and ; and these equations were compared with other
equations published in literature.
2494 Atilla Bilgin et al. / Procedia - Social and Behavioral Sciences 195 (2015) 2492 – 2500

The objective of the present work is to (1) investigate the individual effects of main transesterification reaction
parameters such as catalyst concentration, reaction temperature, reaction time and alcohol/oil molar ratio on the
kinematic viscosities of produced waste cooking oil biodiesels, (2) determine the values giving minimum kinematic
viscosities for each reaction parameters.

2. Materials and Methods

x Materials

To produce biodiesel by basic catalyzed transesterification, waste cooking oil was provided from the university
canteen. Ethanol of 99.8 purity and sodium hydroxide of pure grade were of Merck.

x Production parameters and biodiesel production

Physical and chemical properties of produced biodiesel are significantly affected by various reaction parameters.
In this study, the effects of the following parameters on the kinematic viscosities of produced waste cooking oil
biodiesels were investigated.

. Catalyst concentrations, (mass of NaOH/mass of waste cooking oil): 0.50, 0.75, 1.00, 1.25, 1.50, 1.75
. Reaction temperatures, : 60, 70, 80, 90
. Reaction times, minute: 60, 90, 120, 150
. Alcohol/oil molar ratios: 6:1, 9:1, 12:1, 15:1

The above parameter values were selected as including the ranges in the literature (Karonis et al., 2009; Ginting
et al., 2012; Barbosa et al., 2010; Issariyakul et al., 2008; Meneghetti et al., 2006). The transesterification reaction
was carried out in a 1 L flat-bottomed flask, equipped with a magnetic stirrer heater, thermometer and spiral reflux
condenser. Haake Falling Ball Viscometer, Isolab pycnometer, top loading balance with an accuracy of 0.01 ,
Haake Water Bath and stopwatch with an accuracy of 0.01 were used to measure dynamic viscosity and density.
Before starting the reaction, a certain amount of sodium hydroxide (NaOH) according to chosen catalyst
concentration was dissolved in a certain amount of ethyl alcohol (C2H5OH) depending on alcohol/oil molar ratio in a
narrow-neck flask to make alcoholic solution of catalyst. In the flat bottomed flask, this alcoholic solution was
added to the 200 waste cooking oil that was formerly warmed to about 80 in a beaker. Until a certain time, these
reactants were mixed at a certain reaction temperature with stirring speed of 500 rpm by means of the magnetic
stirrer heater. Transesterification reaction was carried out with the spiral reflux condenser for avoiding loss of
alcohol. Also, reaction temperature was controlled by using the thermometer to remain at a constant temperature
during the reaction. At the end of reaction, the resulting product mixture was transferred to a separating funnel.
After a day, two phases occurred in the separating funnel. The upper phase consists of ethyl esters (biodiesel) while
the lower one consists of glycerol, excess ethanol and the remaining catalyst together with soap. After separation of
the two layers by gravity with gliserol, the upper layer (biodiesel) was washed with warm distilled water. Washed
biodiesel was heated up to about 100 to remove ethyl alcohol and water residuals.

x Density measurement

The density of the produced biodiesel was determined by means of Eq. (1) and measurements in accordance with
ISO 4787 standard:

m total mpycnometer
pycnomete
ycnometer
biodiesel water
(1)
m water
 Atilla Bilgin et al. / Procedia - Social and Behavioral Sciences 195 (2015) 2492 – 2500 2495

where is density of biodiesel at intended temperature, is mass of the pycnometer

filled with biodiesel, is mass of the empty pycnometer, is mass of water (empty
pycnometer mass subtracted), is density of distilled water at intended temperature. and
were experimentally determined as 43.00 and 50.02 , respectively. In order to minimize measurement
errors, all the measurements were conducted three times for each sample and the results were averaged. Also
uncertainty analysis was carried out depending on the sensitivities of measurement devices.

x Dynamic and kinematic viscosity measurement

The dynamic viscosity at 40 was determined in accordance with DIN 53015 standard by using Eq. (2) and
making measurements by means of the Haake Falling Ball Viscometer, Haake Water Bath and stopwatch:

biodiesel Kball
bal ( ball biodiesel )t (2)

where is dynamic viscosity of produced biodiesel, is coefficient of the viscometer ball, and is
falling time of the ball moving between two horizontal line marked on viscometer tube at limit velocity. and
are 0.057 and 2.2 , respectively. The viscosity measurements were also conducted
three times for each sample and the results were averaged.
The kinematic viscosity was determined from Eq. (3) by dividing dynamic viscosity to density at same
temperature:

biodiesel biodiesel / biodiesel (3)

In Eq. (3), if and are in the unit of and , respectively, then is obtained in
unit of .

x Uncertainty analysis

The results obtained from experimental studies are generally calculated from measured physical quantities. These
quantities have some uncertainties due to uncertainties of measuring tools and measurement systems. Therefore,
uncertainty analysis should be applied for proving reliability of the calculated results. In this study, uncertainties of
the measured and calculated physical quantities such as dynamic and kinematic viscosities and densities were
determined by the method proposed by (Kline and McClintock, 2012 ). According to this method, if the result is a
given function of the independent variables , , , and are the uncertainties of each
independent variables, then the uncertainty of the result is calculated by using the equation:

2 2 2
R R R
wR w1 w2 ... wn (4)
x1 x2 xn

By using the method (4), the highest uncertainty was determined as 0.0946 , which show that the results have
fairly high reliability.

3. Results and Discussion

Parametric study was started by varying catalyst concentration. After determination of the optimum catalyst
concentration, the effects of reaction temperature, reaction time and ethyl alcohol/oil molar ratio on kinematic
2496 Atilla Bilgin et al. / Procedia - Social and Behavioral Sciences 195 (2015) 2492 – 2500

viscosities of produced biodiesels were investigated, respectively.

3.1. Effects of catalyst concentration

In order to research the effect of catalyst concentration on kinematic viscosity of biodiesel,

. the alcohol/oil molar ratio: 9:1

. reaction temperature: 70
. reaction time: 90 minutes

were kept constant throughout this set of the experiments and catalyst concentration was changed as 0.50, 0.75,
1.00, 1.25, 1.50 and 1.75 . The change of kinematic viscosity of produced biodiesel with respect to catalyst
concentration is shown in Fig. 1. In this figure, as catalyst concentration is increased, kinematic viscosity of
produced biodiesel gradually decreases until the catalyst concentration of 1.25 . At this point, the kinematic
viscosity takes a minimum value of 4.441 . Then, when the catalyst concentration is continued to increase, the
viscosity gradually increases. This variation can be attributed to the yield of the transesterification reaction. It is
known that the viscosity of the produced biodiesel decreases with increasing reaction yield (Ghanei et al., 2011;
Moradi et al., 2012). Because there is not enough amount of catalyst in reaction medium for low catalyst
concentrations (e.g., 0.50 of sodium hydroxide), much of the triglycerides in the oil cannot be converted
sufficiently to ethyl esters throughout the reaction period (90 minutes). This situation reduces yield of the
transesterification reaction and increases kinematic viscosity of produced biodiesel. If higher catalyst concentration
is used, the yield of the transesterification reaction improves and thus the viscosity of the produced biodiesel
decreases. But, when excess catalyst concentration is used, the yield of the transesterification reaction decreases
(Uzun et al., 2012; Encinar et al., 2005) and the viscosity of the produced biodiesel increases on account of
formation of fatty acid salts (soap), decrease in activity of catalyst and difficulty in separation of glycerol.
In the next stage of the study, catalyst concentration of 1.25 giving the lowest viscosity was kept constant and
the other parameters were changed.

Fig. 1. Change of kinematic viscosity with respect to catalyst concentration.

3.2. Effects of reaction temperature

To determine the effect of reaction temperature on kinematic viscosity of produced biodiesel,

. catalyst concentration: 1.25

 Atilla Bilgin et al. / Procedia - Social and Behavioral Sciences 195 (2015) 2492 – 2500 2497

. the alcohol/oil molar ratio: 9:1

. reaction time: 90 minutes

were kept constant throughout this set of the experiments and reaction temperature was changed as 60, 70, 80 and
90 . Fig. 2 shows the changes of kinematic viscosity versus reaction temperature. In this figure, when reaction
temperature is increased, the kinematic viscosity of produced biodiesel gradually decreases until the reaction
temperature of 70 . At this point, the viscosity takes a minimum value of 4.441 . Then, as the reaction
temperature is continued to increase, the viscosity gradually increases. Kinematic viscosity of biodiesel produced at
low reaction temperatures (e.g., 60 ) is higher since transesterification reaction cannot be effectively completed. As
the reaction temperature is increased, the yield of the transesterification reaction improves due to higher energy
input (Uzun et al., 2012), and the viscosity of produced biodiesel decreases. In case of increasing reaction
temperature higher than the boiling point of ethyl alcohol, viscosity of produced biodiesel increases due to
diminishing of alcohol concentration by evaporating from reaction medium. Moreover, the saponification and
decomposition of esters in biodiesel at higher temperatures may also be contributed to increase in viscosity of
produced biodiesel. According to results, reaction temperature of 70 giving the lowest viscosity was regarded to
be optimal value.

Fig. 2. Change of kinematic viscosity with respect to reaction temperature.

3.3. Effects of reaction time

In order to investigate the effect of reaction time on kinematic viscosity of biodiesel,

. catalyst concentration: 1.25

. reaction temperature: 70
. alcohol/oil molar ratio: 9:1

were kept constant throughout this set of the experiments and reaction time was changed as 60, 90, 120 and 150
minutes. Fig. 3 represents the changes of kinematic viscosity of biodiesel with respect to reaction time. Kinematic
viscosity of produced biodiesel gradually decreases until the reaction time of 120 minutes when reaction time is
increased. At this point, kinematic viscosity takes a minimum value of 4.387 . Then, as the reaction time is
continued to increase, the viscosity gradually increases. The yield of transesterification reaction decreases in short
reaction periods because of insufficient time for the reaction and thus viscosity of biodiesel becomes higher. With
increasing in reaction time (Encinar et al., 2005), viscosity of biodiesel decreases due to the increase in yield of
transesterification reaction and makes a minimum value at about 120 minutes. When reaction time is continued to
2498 Atilla Bilgin et al. / Procedia - Social and Behavioral Sciences 195 (2015) 2492 – 2500

increase, the transesterification reaction may shift towards reactants and thus causes to increase in viscosity of
biodiesel.
In the next stage of the study, based on these results, reaction time of 120 minutes giving the lowest viscosity was
considered to be an optimum condition.

Fig. 3. Change of kinematic viscosity with respect to reaction time.

3.4. Effects of alcohol/oil molar ratio

To analyze the effect of ethyl alcohol/oil molar ratio on kinematic viscosity of biodiesel,

. catalyst concentration: 1.25

. reaction temperature: 70
. reaction time: 120 minutes

were kept constant throughout this set of the experiments and molar ratio was changed as 6:1, 9:1, 12:1 and 15:1.
Fig. 4 shows the change of kinematic viscosity of biodiesel versus molar ratio. Kinematic viscosity of produced
biodiesel decreases until a value between 9:1 and 12:1 when molar ratio is increased. Considering the measurement
values, the kinematic viscosity takes a minimum value as 4.347 cSt at 12:1 molar ratio. Then, as the molar ratio is
continued to increase, the viscosity tends gradually to increase. According to the experimental results, the biodiesel
has the maximum viscosity with 4.559 by using molar ratio of 6:1. When more alcohol/oil molar ratio is used
(e.g., 9:1 or 12:1), because the transesterification reaction shifts toward products (El-Sabagh et al., 2011), the yield
of the transesterification reaction increases and viscosity of biodiesel declines. Molar ratio of 15:1 gives higher the
viscosity than 12:1 and 9:1 molar ratios because use of excess alcohol could be attributed to deactivation of the
catalyst and increase in the solubility of the glycerol in the ethyl ester phase. Alcohol/oil molar ratio of 12:1 giving
the lowest viscosity was taken to be optimal value.
 Atilla Bilgin et al. / Procedia - Social and Behavioral Sciences 195 (2015) 2492 – 2500 2499

Fig. 4. Change of kinematic viscosity with respect to alcohol/oil molar ratio.

4. Conclusion

In this study, the individual effects of catalyst concentration, reaction temperature, reaction time and ethyl
alcohol/oil molar ratio on kinematic viscosity of produced biodiesel were investigated parametrically to produce the
lowest viscosity waste cooking oil biodiesel by using NaOH as catalyst. It was determined that:

. 1.25 catalyst concentration

. 70 reaction temperature
. 120 minutes reaction time
. 12:1 ethyl alcohol/oil molar ratio

give the lowest kinematic viscosity of 4.347 .

Acknowledgments

The authors express their gratitude to Karadeniz Technical University Scientific Research Projects Fund for
financial support received (Project No: 9745).

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