Biofuels

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An empirical and statistical analysis of biodiesel

production by transesterification process

A. Murugesan, D. Subramaniam & A. Avinash

To cite this article: A. Murugesan, D. Subramaniam & A. Avinash (2015) An empirical and
statistical analysis of biodiesel production by transesterification process, Biofuels, 6:1-2, 79-86,
DOI: 10.1080/17597269.2015.1050643

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Published online: 16 Jun 2015.

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Biofuels, 2015
Vol. 6, Nos. 1 2, 79 86, http://dx.doi.org/10.1080/17597269.2015.1050643

An empirical and statistical analysis of biodiesel production by transesterification process

A. Murugesana, D. Subramaniamb and A. Avinashc*
a
Department of Mechatronics Engineering, K. S. Rangasamy College of Technology, Tiruchengode, 637215 Tamil Nadu, India;
b
Department of Mechanical Engineering, K. S. Rangasamy College of Technology, Tiruchengode, 637215 Tamil Nadu, India; cInternal
Combustion Engineering Division, Department of Mechanical Engineering, Sri Venkateswara College of Engineering, Sriperumbudur
602105, Tamil Nadu, India

(Received 10 December 2014; accepted 4 May 2015)

Despite the fragile bio-fuel market of the present day, numerous research works are being carried out all over the globe to
discover a viable alternate source to fossil fuels. In this regard, the present study enumerates the production of methyl
esters of Pungamia oil by transesterification process. Also, the parameters influencing biodiesel production such as the
stirrer speed, reaction time, and quantity of catalyst were studied and discussed. In this work, sodium methoxide (mixture
of sodium hydroxide and methanol) and potassium methoxide (mixture of potassium hydroxide and methanol) gave good
conversion yields and high quality of biodiesel during transesterification process. Also, the maximum ester content of
biodiesel was witnessed for potassium hydroxide catalyst and the amount of catalyst used was less than that with sodium
hydroxide for the same mass of the feedstock oil.
Keywords: Pungamia oil; transesterification; bio-diesel; ANOVA

1. Introduction Compression Ignition (CI) engine fuel. The high viscosity of

In the past few decades or so, greater awareness about the
environment rose among people to search for an alterna-
tive fuel that could burn with less environmental pollu-
tion. Perhaps Rudolf Diesel’s prediction has come true
today after a very long period with the usage of biodiesel
all over the world. Indeed, the steps towards alternative
fuels were on the go from the invention of the diesel
engine by Rudolf Diesel in 1885. [1]
Many researchers and scientists have tried out differ-
ent types of fuels for diesel engines. Among those, vegeta-
ble oils and alcohols (methanol and ethanol) are
encouraging renewable liquid fuels. In fact, Straight Veg-
etable Oil (SVO) can be used as sole fuel in conventional
diesel engines, but the high viscosity of SVO interferes
with the injection process and leads to poor fuel atomiza-
tion. Also, the inefficient mixing of SVO with air contrib-
utes to incomplete combustion, leading to heavy smoke
emission. These problems can be solved if the SVO is
chemically modified into biodiesel, which is similar in
characteristics to conventional diesel fuel. [2 4]
Murugesan et al. [5] reported that vegetable oils have
a different chemical structure and they have up to three
fatty acids that are linked to a glycerin molecule with ester
linkages. In fact, these fatty acids vary in their carbon
chain length and in number of double bonds. Palmitic
(16 carbon atoms) and Stearic (18 carbon atoms) are the
two most common saturated fatty acids present in every
vegetable oil (containing at least a small amount of either
Palmitic acid or Stearic acid).
An investigation by Sangeeta Kanakraj et al. [6] reported
the problems coupled with directly using SVOs as a
SVOs compared to diesel oil is the main problem reported.
Also, elevated viscosity paves the way for poor fuel atomi-
zation, incomplete combustion, and deposits in the combus-
tion chamber. Therefore, in order to overcome these
problems there are many potential methods such as heating,
dilution, blending, emulsification, and transesterification.
In general, vegetable oil contains 97% triglycerides and
3% di- and monoglycerides and fatty acids. The process of
removal of all glycerol and fatty acids from the vegetable
oil in the presence of a catalyst is called transesterification.
In the transesterification process, vegetable oil reacts with
a monohydric alcohol, like methanol or ethanol, and forms
esterified vegetable oil (esters of SVO) in the presence of
sodium or potassium hydroxide as a catalyst. [7 9]
Ofoefule et al. [7] reported that transesterification of vege-
table oils with low molecular weight alcohols (methanol,
ethanol, propanol, butanol and amyl alcohol) has been
established as the best option to reduce the high viscosity,
low volatility, heavy engine deposits, and toxic substance
formation associated with the direct use of vegetable oils.
In the transesterification reaction, the important variables
affecting the esters yield are the effects of free fatty acids
and moisture, the catalyst type and concentration, the molar
ratio of alcohol to oil and type of alcohol, the effect of the
reaction time and temperature, and the mixing intensity.
First, the free fatty acid and moisture content are key
parameters for determining the viability of the vegetable
oil for transesterification process. To complete the base
catalyzed reaction, a free fatty acid value lower than 3%
is needed. The higher the acidity of the oil, the smaller the
conversion efficiency. [10]

*Corresponding author. Email: avinashandromeda@gmail.com

Ó 2015 Taylor & Francis

80 A. Murugesan et al.
Furthermore, the catalysts used for the transesterifica-
tion of triglycerides are classified as alkali, acid, enzyme,
or heterogeneous catalysts, among which alkali catalysts
like NaOH and KOH are more effective. In addition, if
the oil has a high free fatty acid content and more water,
an acid catalyst is suitable. The acids could be H2SO4,
H3PO4, HCl, or organic sulfonic acids. [11 12]
Another important variable affecting the yield of esters
is the molar ratio of alcohol to vegetable oil. The stoichi-
ometry of the transesterification reaction requires three
moles of alcohol per mole of triglyceride to yield three
moles of fatty esters and one mole of glycerol. However,
transesterification is an equilibrium reaction in which a
large amount of excess alcohol is required to drive the
reaction. A molar ratio of 6:1 is normally used in industrial
process because the yield of esters is higher than 98% by
weight. Also the molar ratio has no effect on acid, perox-
ide, saponification, and iodine value of methyl esters. [13]
The report of Freedman et al. [14] revealed that the rate
of transesterification reaction is strongly influenced by the
temperature. However, given enough time, the reaction
will proceed to near completion even at room temperature.
[15] However, the reaction is completed when the tempera-
ture is raised to the boiling point of alcohol at atmospheric
pressure. Such mild reaction conditions require the removal
of free fatty acids from the oil by refining or pre-transester-
ification. Therefore, degummed and de-acidified oil is used
as feedstock. [14] Pretreatment is not required if the reac-
tion is carried out under high pressure of 9000 KPa and
high temperature of 240 C. Under these conditions, simul-
taneous esterification and transesterification can take place.
The maximum yield of esters occurs at temperatures rang-
ing from 60 C to 80 C at a molar ratio of (alcohol to oil)
6:1. Further increasing the temperature, the yield of esters
has a negative effect on the conversion. Furthermore, reac-
tion time is the controlling factor for determining the yield
of methyl esters as per the conclusion of Feuge and Gros
[16] and Fillieres et al. [17]
Finally, Trathnigg and Mittelback [18] and Meher et al.
[19] reported that mixing is very important in the transes-
terification reaction, as oil or fat are immiscible with
NaOH-MeOH solution. Once the two phases are mixed
and the reaction is started, stirring is no longer needed.
Methanolysis was conducted with different rates of stirring
such as 180, 360, and 600 revolutions per minute (rpm).
The reaction is incomplete with 180 rpm and rate of mix-
ing was insignificant for methanolysis. The yield of methyl
esters at 360 rpm and 600 rpm was same after three hours
of reaction as reported by Meher et al. [19]
The prohibitive cost of edible oils in developing coun-
tries like India prevents their use in biodiesel preparation.
Therefore, non-edible oils are affordable for viable biodiesel
production in that country. It is also estimated that India can
produce one million tons of biodiesel per year. In this
regard, Jatropha (Jatropha curcas), Karanja (Pungamia pin-
nata), Neem (Azadirachta indica), and Mahua (Madhuca
longifolia) plant species are desirable for biodiesel produc-
tion in India. [5] From this point of view, present research
work is centered on producing methyl esters of Pungamia
oil with the aid of a transesterification unit. Besides the
effects of stirrer speed, reaction time and quantity of ester
yield had been studied and presented in an in-depth manner.
2. Materials and methods
2.1 Biodiesel production
Vegetable oil characteristically contains free fatty acids,
phospholipids, sterols, water, odorants, and additional impu-
rities. Owing to their presence, the oil requires chemical
modifications like esterification, transesterification, pyroly-
sis, and emulsification. Among these, transesterification is
an imperative process to produce a clean and environment
friendly fuel from vegetable oil and it appears to be a more
suitable process because the by-product (glycerol) has com-
mercial value. The process flow chart for biodiesel produc-
tion by transesterification is depicted in Figure 1.
2.2 Experimental setup of a biodiesel production unit
A small batch type unit had been fabricated to produce bio-
diesel from all types of non-edible oils. It is very compact
and can produce five liters of biodiesel from non-edible
oils in a period of 11/2 hours. In addition, the production of
biodiesel is approximately 40 to 50 liters per day. Besides,
it has the following features. The fabrication cost of the
production unit is less and it is easy to operate. The unit is
provided with an automatic temperature controller to vary
the temperature of the oil from 30 to 250 C. This feature is
highly useful for pretreatment, transesterification and evap-
orating water molecules present in the biodiesel after bub-
ble washing. A variable speed DC motor is used to vary
the speed of the stirrer from 200 to 900 rpm. The speed of
the stirrer was monitored using a digital speed sensor along
with a digital speed indicator. Thus, it is possible vary stir-
rer speed depending up on the requirements. Overall, it is
possible to produce a biodiesel yield of about 80 96%
based on the nature of oils and reactants.
2.3 Description of the biodiesel production unit
The transesterification unit, which was fabricated in the
laboratory, consists of a stainless steel container with a
capacity of six liters and a variable speed DC motor fixed
to the top of the container. The DC motor is attached with
a mechanical stirrer. The operating tip speed of the
mechanical stirrer varies from 200 rpm to 900 rpm. The tip
speed of the stirrer can be easily varied with the help of an
electronic speed regulator and the tip speed of the
stirrer was monitored using a digital speed sensor along
with a digital speed indicator. The stirrer consists of eight
stainless steel blades at an angle of 45 (oriented at 45 to
the base).
A heater having a capacity of 1.5 kW was fixed at the
bottom of the container for heating the oil. A temperature
control unit was used to vary the temperature of the oil
from 30 to 250 C. The temperature of the oil was mea-
sured using a Chromel Alumel (k-type) thermocouple
along with a digital temperature indicator. An electronic
microprocessor was used to control the motor speed and
 Biofuels 81

Figure 1. Process flow chart for biodiesel production.

the temperature. A cooling fan was provided inside the The line diagram and photographic view of the biodiesel
electronic kit to absorb the heat from the transformer and production unit are shown in Figures 2 and 3. The disman-
integrated circuits. The top of the container has one inlet tled view, full view of heater and stirrer are shown in
valve, and the bottom of the container has one drain valve. Figures 4, 5 and 6, respectively.

Figure 2. Line diagram of the biodiesel production unit.

82 A. Murugesan et al.
Figure 3. Photographic view of biodiesel production unit.
Figure 4. View of dismantled biodiesel production unit.
Figure 5. Photographic view of heater along with thermocouple.
Figure 6. Photographic view of stirrer.
2.4 Production of methyl esters of biodiesel from raw
Pungamia oil
Transesterification is a reaction in which triglycerides
present in vegetable oil reacts with alcohol (usually meth-
anol or ethanol) in the presence of alkaline catalyst yield-
ing esters (biodiesel) and glycerol. Catalysts such as alkali
metals/alkaline hydroxide (alkoxide) such as potassium
hydroxide (KOH) and sodium hydroxide (NaOH) are used
as the alkaline catalysts. Transesterification reaction is
proceeded essentially by mixing the reactants. [8,10,11]
2.5 Alkaline transesterification
The first step for biodiesel production is the transesterifi-
cation of vegetable oils. By this process, the molecular
size of the component (triglycerides) reduces. The transes-
terification process is as follows: one liter of Pungamia oil
was placed in a round bottom flask and was heated to
110 C in order to remove the moisture content present in
it. An alkaline catalyst was dissolved in methyl alcohol
and the reaction temperature was maintained at 65 C for a
period of 60 minutes. The reaction products were permit-
ted to settle under gravity in a separating funnel for
24 hours to separate methyl esters and glycerol. Due to
the higher density of glycerol it settled at the bottom of
the funnel and apparently methyl esters occupied the top
surface. The methyl ester was then washed with warm
water to remove un-reacted methanol, catalyst, and impu-
rities. The washed methyl ester was again heated to
110 C to remove the moisture content.
Normally, alkali based transesterification reaction is
conducted at a temperature close to the boiling point of
alcohol (methanol: 65 C) and the stoichiometry of trans-
esterification reaction requires three moles of alcohol per
mole of triglyceride to yield three moles of fatty ester and
one mole of glycerol as reported by Bojan and Durairaj
[9] and Sathya and Manivannan. [20] In this work, experi-
mental tests were conducted three times and their average
values have been presented.
2.6. Statistical analysis
In this work, statistical procedure was adopted for the
analysis of quantitative responses from experimental
units. Analysis of variance (ANOVA) had been carried
out to analyze the significant mean differences with
three different brands of KOH on ester yield. The analy-
sis of variance, or more briefly ANOVA, refers broadly
to a collection of experimental situations and statistical
procedure for the analysis of quantitative responses
from experimental units. The simplest ANOVA problem
is referred to variously as a single-factor, single-classifi-
cation, or one-way ANOVA, and involves the analysis
of data from experiments in which more than two
treatments have been used. [21] In this work, single-fac-
tor ANOVA was examined. Tukey’s procedure was car-
ried out to compute which group means are different
from one another.

3. Results and discussion
3.1 Effect of stirrer speed on ester yield
Mixing is very important in the transesterification reaction
as oil and fat are immiscible with hydroxide-methanol
solution. Once the two phases are mixed, the reaction is
started. Methanolysis was conducted with different rates
of stirrer such as 350, 400, 450, 500, 550 and 600 revolu-
tions per minute (rpm). The variation of methyl esters
yield with different rates of stirrer is shown in Figure 7. It
was observed from the figure that the reaction was incom-
plete up to 500 rpm and rate of mixing was insufficient for
methanolysis. The yield of methyl esters at 550 rpm was
79% and, with further increase in speed of stirrer to
600 rpm, the yield of methyl esters was reduced to 76%.
Therefore, further increase in stirrer speed did not provide a
better yield but a decrease in ester yield. Leevijit et al. [22]
observed a similar trend in their experiments; however the
reason for this trend is unclear. Overall, in this experimental
work, a speed of 550 rpm is suggested for production of
maximum yield of Pungamia biodiesel. This result agrees
with the experimental works conducted by Ong et al., [23]
Venkanna and Venkataramana Reddy, [24] Malaya Naik
et al. [25] and Rashid and Farooq Anwar. [26]
3.2 Effect of reaction time and reaction temperature
on ester yield
The reaction time required for the completion of alkaline-
catalyzed transesterification depends not only on the reac-
tion temperature but also on the degree of mixing in the
process. The reaction rate of transesterification increases
with increasing temperature and degree of mixing. The
reaction time of transesterification process is conducted at
65 C that is nearer to the boiling point of methanol. [27]
The variation of methyl esters yield with different reaction
times (50 100 min) is shown in the Figure 8.
It was observed that the yield of biodiesel was less at
the beginning and it reached a maximum at the reaction
time of 70 minutes at 65 C and was relatively constant
thereafter. The reaction time of the product yield was
examined by extending the reaction time from 70 minutes
to 100 minutes. The result indicated that the extension of
time from 70 minutes to 100 minutes has no significant
effect on the conversion of triglycerides, but it leads to a
Figure 7. Variation of methyl esters yield with different stirrer
speed.
Biofuels 83
Figure 8. Variation of methyl esters yield with different reac-
tion time.
reduction in the product yield, where it decreases from
89% to 86%. This is because the longer reaction time
enhances the hydrolysis of esters which results in the loss
of esters as well as causing more fatty acids to form soap.
Also, soaps that were more visible were observed during
experimental study. The gradual increase of reaction time
shows the negative effect on the product yield. This pat-
tern was also observed in the experimental study con-
ducted by Leung and Guo. [27] It is clear that the reaction
time is an important controlling factor for the product
yields. The optimal reaction time for transesterification
of raw Pungamia oil was 70 minutes at 65 C with the
optimal mixing of 550 rpm.
3.3 Quantity of catalyst on ester yield
The effects of the two catalysts used in the transesterifica-
tion were compared through examining the esters content
in the biodiesel product obtained. The two catalysts exhib-
ited similar trends on the conversion of triglycerides to
esters, but a different quantity of catalyst was required for
achieving the same conversion. The effect of NaOH and
KOH quantity on the transesterification of the raw Punga-
mia oil was investigated with its quantity varying from 13
to 18 g. The operating conditions during the reaction pro-
cess were fixed (reaction temperature: 65 C, reaction
time: 70 minutes, amount of methanol used: 400 ml) and
these conditions were selected based on the previous liter-
ature. Figure 9 presents the result of variation of yield
with different quantities of NaOH and KOH as catalysts.
Two catalyst exhibited similar trends on the conversion of
triglycerides to esters but different amount yields were
obtained for the same amount of catalyst used.
Figure 9. Variation of methyl esters yield with different cata-
lyst quantity.
84 A. Murugesan et al.

Maximum esters content of the biodiesel product

reached to 93% and 89% for catalyst quantity of 16 g
(KOH) and 17 g (NaOH), respectively. Also, the amount
of KOH used was less than that of NaOH for same mass
of feedstock oil. Hence, KOH is the better catalyst com-
pared to NaOH. A similar observation was reported by
Malaya Naik et al., [25] Rashid and Farooq Anwar [26]
and Karmee and Anju Chadha. [28]
It can be seen from Figure 9 that an increase in NaOH
or KOH concentration beyond the optimal value results in
the drop of yield of biodiesel. This was observed during
the experimental study. This is because addition of excess
of alkaline catalyst (NaOH or KOH) caused more trigly-
cerides participating in the saponification reaction with
NaOH or KOH producing more soap thereby reducing the
yield of esters. Another possible reason is addition of
excess amount of catalyst gave rise to the formation of an
emulsion, which increased the viscosity and led to the for-
mation of gels. Similar results were observed by Malaya
Naik et al. [25] and Karmee and Anju Chadha. [28]

3.4. Separation of intermediate product

Two catalysts, namely KOH and NaOH, were used in the
reaction and the final product of mixture derived from
transesterification exhibited some differences in physical
states. Figures 10 and 11 show the state of final product
mixture settled overnight produced from the transesterifi-
cation of raw Pungamia oil using those catalysts. For the
NaOH catalyst after settling overnight the product mixture
separated in to two layers: crude esters layer in liquid state
(upper layer) and glycerol layer (lower layer) as shown in
Figure 11. Photographic view of crude esters using KOH as
catalyst.
Figure 10. It is known that glycerol is a viscous liquid in
ambient temperature and pressure. When more and more
solid soaps sunk to the bottom, a mixture of glycerol and
soap in solid state was formed after settling overnight.
For KOH catalyst, the product mixture separated as
two liquid layers after settling overnight (crude esters
layer in liquid state [upper layer] and glycerol layer [lower
layer]) as shown in Figure 11. Because potassium soap is
softer than sodium soap, its residues formed during the
transesterification unlike sodium soap did not sink into
the glycerol layer at the bottom, but suspended in the
crude esters layer, thus resulting in a viscous glycerol
layer. Therefore, for separation of esters layer from the
glycerol in the industrial production, using KOH as cata-
lyst is the undoubtedly more convenient and simpler pro-
cess because the glycerol layer in the liquid state can be
easily removed by direct out flowing from the bottom of
the separation unit. Apart from this, biodiesel may contain
high levels of sodium as residue from the biodiesel pro-
duction process. When not removed adequately, sodium
will form soaps that can cause a variety of operational
problem. For this reason, KOH is commonly used for pro-
ducing biodiesel from non-edible oils. These results are in
accordance with the experimental work done by Leung
and Guo [27] and Sharma and Singh. [29]

3.5. ANOVA (analysis of variance)

In this section, single-factor ANOVA has been focused.
The effects of stirrer speed, reaction time, and catalyst
Figure 10. Photographic view of crude esters using NaOH as quantity on biodiesel yield have already been presented in
catalyst. Sections 3.1, 3.2, and 3.3, and also the optimum operating

Table 1. ANOVA for three brands of KOH on methyl ester
yield.
Source SS df MS F Fcriticla p-vlaue
Between 297.612 2 148.81 7.3365 3.6823 0.0060
Within 304.247 15 20.283
Total 601.858 17
SS D sum of squares, df D degrees of freedom, MS D mean squares
conditions for higher ester yield have been reported.
Hence the maximum conversion efficiency was found
using KOH catalyst, the further experiments were con-
ducted with three different brands of KOH on ester yield
to analyze the variance by carrying out F test (testing the
null hypothesis: H0). Also, further analysis of the data
when H0 has been rejected is reported in Section 3.5.
The single-factor ANOVA was examined by consider-
ing the effects of three different brands of KOH on methyl
ester yield by considering six observations for each brand.
Table 1 is an ANOVA table for the present work. The last
column of the table gives the p-value, which is .006.
Using a significance level of .05, the null hypothesis H0 is
rejected, since p-value .006 < .05. Thus, undoubtedly
there is a significant difference among all treatment
means. This significant difference might be due to the var-
iation in purity of the three brands of KOH catalysts
selected for the study. Therefore, the purity of selected
catalysts for transesterification reaction will also play a
significant role in ester yield.
3.6. Tukey’s procedure (the T method)
Since the computed value of the F statistic in single-factor
ANOVA is significant (H0 is rejected), further analysis
was carried out to compute which of the treatment means
are different from one another by using multiple compari-
sons procedure. Tukey’s procedure is one among the mul-
tiple comparison procedures, which involves the use of
probability distribution called the studentized range distri-
bution. The distribution depends on two parameters: a
numerator degree of freedom (m) and a denominator
degree of freedom (v). Let q0 denote the upper-tail a criti-
cal value of the studentized range distribution and this
value can be used to obtain simultaneous confidence inter-
vals for all pairwise differences. Table 2 shows the T
method for identifying significantly different means. It is
evident from T method that the difference between the
group means (A-B and A-C) is significant.
Table 2. Tukey’s procedure for pairwise comparison of means.
A A D Brand A (KOH)
r 3 B Sig B B D Brand B (KOH)
n-r 15 C Sig C D Brand C (KOH)
q0 3.67
T 6.74773
Sig D significant
Biofuels 85
4. Conclusions
In this study, optimization of the important parameters
like stirrer speed, concentration of catalysts like NaOH
and KOH, and reaction time and reaction temperature for
producing higher yield of methyl esters from Pungamia
oil were presented. A batch type biodiesel production unit
was used for this purpose. The following observations
were made during the biodiesel production process:
 The optimal reaction time for transesterification of
raw Pungamia oil was 70 minutes at 65 C with the
optimal mixing of 550 rpm.
 During the transesterification process, sodium
methoxide and potassium methoxide gave good
ester conversions. However, the maximum ester
content of biodiesel (93%) was witnessed for the
KOH catalyst (16 g). Also the amount of KOH used
was less than that of NaOH for the same mass of
feedstock oil. Therefore, the catalyst KOH was
found to be superior to NaOH.
 Furthermore, for separation of esters layer from the
glycerol in the industrial production, using KOH as
catalyst is more convenient and simpler process
because the glycerol layer in the liquid state can be
easily removed by direct out flowing from the bot-
tom of the separation unit.
 Finally, statistical analysis of the conducted work
revealed that there is a significant difference among
mean values of three different brands of KOH cata-
lysts and between one another. This pattern clearly
reveals that the purity of catalysts plays a significant
role in ester yield.
Disclosure statement
No potential conflict of interest was reported by the authors.
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