International Journal of Agriculture and Crop Sciences.

Available online at www.ijagcs.com

IJACS/2013/5-3/292-297
ISSN 2227-670X 2013 IJACS Journal




Studying some effective parameters on
transesterification reaction to produce biodiesel from
safflower oil

Kambiz Tahvildari, Sharareh Esmaeili, Amir Abdollah Mehrdad Sharif

Department of Applied Chemistry, Faculty of Chemistry, Islamic Azad University Tehran-North Branch, Iran.

Corresponding author email: [email protected]

ABSTRACT: Biodiesel fuel, due to uncontrollable prices of fossil fuels, reduction of its resources and
environmental pollution, has become increasingly important. Biodiesel (the mono alkyl esters of fatty
acids) is a renewable and green energy, derived from vegetable oils and animal fats. The high viscosity of
vegetable oils prevents their direct use in diesel engines, so, among different methods of chemical
modification, transesterification is used to produce biodiesel. In this study, safflower plant oil was used to
produce biodiesel. Safflower oil was extracted by soxhlet apparatus and its physical properties were
determined. The effect of molar ratio (oil to alcohol) and amount of catalyst on the conversion of oil to
methyl ester was studied. The results indicate that, catalyst amount (1%w/w) and 6:1 molar ratio of
alchohol to oil were the optimum conditions for producing of biodiesel and 96% yield of methyl esters has
been obtained. Produced biodiesel was within recommended standards of biodiesel fuel (ASTMD6751-
09).

Keywords: biodiesel, esterification, transesterification, safflower oil, viscosity

INTRODUCTION

The invention of IC engines and the following ameliorations in engine designing technology have led to the
large usage of oil resources and to rapid evacuation of these sources. Now it is obviously determined that the world
will face the crisis correspond to the decrease or to the finishing of fossil fuels resources specially the oil because
of the 80 billion barrels extraction of oil per day. On the other hand, the combustion of these fuels has led to the
increase in greenhouse gases, ozone layer demolition and environment pollution as well as breathing disorders in
large cities. In addition, the consumer countries tend to depend much more on the countries that export oil products
,such as petrol and gasoline , which has led to the increase in oil products price so that the energy security of these
countries are at risk.
Vegetable oils were used as the fuel of diesel engines by Radolph Diesel. High-Kinematic viscosity of
these oils is the fundamental issue that inhibits the direct use of these vegetable oils in diesel engines. The high-
Kinematic viscosity of these oils would cause difficulty in fuel pouring and atomizing located in the combustor, and
would bring dysfunction of lubricating and deficient combustion leading to the carbon silting in the cylinder (Ma and
Hanna, 1999). The renewable fuels possess the vegetable and animal base and pollute less compared to that of
the fossil fuels when combustion (Dorado et al, 2003; Nabi et al, 2006).
Biodiesel is defined as the mono alkyl esters of fatty acids with long chains which is obtained through the
renewable fuels such as vegetable oils or animal fats (Fukuda et al, 2001). The indispensable attribute of vegetable
oils are their renewability and viability which would not come to end. Each country holding these vegetable
products will have the capability of producing fuel from them; hence providing the whole or part of its exigency.
In order to reduce the viscosity of vegetable oils, one would survey four methods, namely
transesterification, pyrolysis, dilution and micro-emulsion among which the transesterification is the most common
used method in industry so as to reduce the viscosity. Transesterification is defined as the reaction between the oil
or fat with alcohol. The products of this reaction are biodiesel and glycerin. Figure 1 shows the transesterification
reaction. Because it takes a long time for the alcohol and oil to do the reaction, one can claim that using the
Intl J Agri Crop Sci


catalyst, mechanical stirrin
biodiesel production




catalyst is the most current kind of catalysts being used in biodiesel production. The excellence corresponding to
this kind of catalyst is that it
(Canakci et al, 1999).

alkali catalysts to produce soaps that in
FFAs to methyl esters, it is used as a pretreatment for the high FFA feedstocks. Then, when the FFA level has
been reduced to 0.5%, or lower, an alkali catalyst is added to conv
process can convert high free fatty acid feedstocks quickly and effectively

methyl
which the alcohol and H




oil and to produce biodiesel through using
investigate


The materials and equipment

p
Company were provided. Also, the Anton
made in Belgium Analyze company
experiments.

The experiments procedure

thimble and then in Soxhlet
300
extracted oil. The maximum amount of extracted oil from
Intl J Agri Crop Sci


catalyst, mechanical stirrin
biodiesel production



Diverse catalysts can be used in transesterification reaction,
catalyst is the most current kind of catalysts being used in biodiesel production. The excellence corresponding to
this kind of catalyst is that it
(Canakci et al, 1999).
Many
alkali catalysts to produce soaps that in
FFAs to methyl esters, it is used as a pretreatment for the high FFA feedstocks. Then, when the FFA level has
been reduced to 0.5%, or lower, an alkali catalyst is added to conv
process can convert high free fatty acid feedstocks quickly and effectively
The free fatty acids do the reaction with methanol in the presence of acidic catalyst (sulfuric acid) that yield
methyl ester and H
which the alcohol and H


Figure 2. esterification reaction in the presence of acidic catalyst in order to

The aim of this research is to
oil and to produce biodiesel through using
investigate alcohol to oil molar ratio and catalyst


The materials and equipment
Safflower
potassium hydroxide 99
Company were provided. Also, the Anton
made in Belgium Analyze company
experiments.

The experiments procedure
The Safflower seed was prepared as the powder through using rotary mill and 100g of it was put into
thimble and then in Soxhlet
300 ml of n-
extracted oil. The maximum amount of extracted oil from
Intl J Agri Crop Sci. Vol., 5 (
catalyst, mechanical stirrin
biodiesel production (Knothe et al, 2005)
Diverse catalysts can be used in transesterification reaction,
catalyst is the most current kind of catalysts being used in biodiesel production. The excellence corresponding to
this kind of catalyst is that it
(Canakci et al, 1999).
Many of feedstocks contain large amounts of free fatty acids (FFAs).
alkali catalysts to produce soaps that in
FFAs to methyl esters, it is used as a pretreatment for the high FFA feedstocks. Then, when the FFA level has
been reduced to 0.5%, or lower, an alkali catalyst is added to conv
process can convert high free fatty acid feedstocks quickly and effectively
The free fatty acids do the reaction with methanol in the presence of acidic catalyst (sulfuric acid) that yield
ester and H
2
O, as shown in figure 2. It is probable for the esterification reaction to occur sequentially in
which the alcohol and H
2
O
Figure 2. esterification reaction in the presence of acidic catalyst in order to
The aim of this research is to
oil and to produce biodiesel through using
alcohol to oil molar ratio and catalyst
The materials and equipment
Safflower seeds from Tabriz University of Agriculture, n
hydroxide 99%, Methanol 99.7%, sulfuric acid 99% and i
Company were provided. Also, the Anton
made in Belgium Analyze company
experiments.
The experiments procedure
The Safflower seed was prepared as the powder through using rotary mill and 100g of it was put into
thimble and then in Soxhlet
-hexane as the solvent in 6 hour
extracted oil. The maximum amount of extracted oil from
. Vol., 5 (3), 292-29
catalyst, mechanical stirring with high intensity, and increasing the temperature
(Knothe et al, 2005)
Figure
Diverse catalysts can be used in transesterification reaction,
catalyst is the most current kind of catalysts being used in biodiesel production. The excellence corresponding to
this kind of catalyst is that it yields much ester in a short time during the appropriate circumstances of reaction
feedstocks contain large amounts of free fatty acids (FFAs).
alkali catalysts to produce soaps that in
FFAs to methyl esters, it is used as a pretreatment for the high FFA feedstocks. Then, when the FFA level has
been reduced to 0.5%, or lower, an alkali catalyst is added to conv
process can convert high free fatty acid feedstocks quickly and effectively
The free fatty acids do the reaction with methanol in the presence of acidic catalyst (sulfuric acid) that yield
, as shown in figure 2. It is probable for the esterification reaction to occur sequentially in
O being produced should be derived away.
Figure 2. esterification reaction in the presence of acidic catalyst in order to
The aim of this research is to
oil and to produce biodiesel through using
alcohol to oil molar ratio and catalyst
The materials and equipment
seeds from Tabriz University of Agriculture, n
%, Methanol 99.7%, sulfuric acid 99% and i
Company were provided. Also, the Anton
made in Belgium Analyze company and the clarus
The experiments procedure
The Safflower seed was prepared as the powder through using rotary mill and 100g of it was put into
thimble and then in Soxhlet apparatus
hexane as the solvent in 6 hour
extracted oil. The maximum amount of extracted oil from
97, 2013
g with high intensity, and increasing the temperature
(Knothe et al, 2005).
Figure 1. transesterification reaction
Diverse catalysts can be used in transesterification reaction,
catalyst is the most current kind of catalysts being used in biodiesel production. The excellence corresponding to
yields much ester in a short time during the appropriate circumstances of reaction
feedstocks contain large amounts of free fatty acids (FFAs).
alkali catalysts to produce soaps that inhibit the reaction
FFAs to methyl esters, it is used as a pretreatment for the high FFA feedstocks. Then, when the FFA level has
been reduced to 0.5%, or lower, an alkali catalyst is added to conv
process can convert high free fatty acid feedstocks quickly and effectively
The free fatty acids do the reaction with methanol in the presence of acidic catalyst (sulfuric acid) that yield
, as shown in figure 2. It is probable for the esterification reaction to occur sequentially in
being produced should be derived away.
Figure 2. esterification reaction in the presence of acidic catalyst in order to
The aim of this research is to extract Safflower (
oil and to produce biodiesel through using alkali-
alcohol to oil molar ratio and catalyst concentration
MATERIALS AND METHODS
seeds from Tabriz University of Agriculture, n
%, Methanol 99.7%, sulfuric acid 99% and i
Company were provided. Also, the Anton paar viscometer of SVM
and the clarus
The Safflower seed was prepared as the powder through using rotary mill and 100g of it was put into
apparatus in order to extract the oil
hexane as the solvent in 6 hours. Next, the rotary device was used for
extracted oil. The maximum amount of extracted oil from
g with high intensity, and increasing the temperature
1. transesterification reaction
Diverse catalysts can be used in transesterification reaction,
catalyst is the most current kind of catalysts being used in biodiesel production. The excellence corresponding to
yields much ester in a short time during the appropriate circumstances of reaction
feedstocks contain large amounts of free fatty acids (FFAs).
hibit the reaction. Since acid catalysis is relatively fast for converting the
FFAs to methyl esters, it is used as a pretreatment for the high FFA feedstocks. Then, when the FFA level has
been reduced to 0.5%, or lower, an alkali catalyst is added to conv
process can convert high free fatty acid feedstocks quickly and effectively
The free fatty acids do the reaction with methanol in the presence of acidic catalyst (sulfuric acid) that yield
, as shown in figure 2. It is probable for the esterification reaction to occur sequentially in
being produced should be derived away.
Figure 2. esterification reaction in the presence of acidic catalyst in order to
2010).
Safflower (Carthamus tinctoriu
- transesterification reaction.
concentration
MATERIALS AND METHODS
seeds from Tabriz University of Agriculture, n
%, Methanol 99.7%, sulfuric acid 99% and i
paar viscometer of SVM
and the clarus-580, Perkin Elmer Gas chromatograph
The Safflower seed was prepared as the powder through using rotary mill and 100g of it was put into
in order to extract the oil
s. Next, the rotary device was used for
extracted oil. The maximum amount of extracted oil from Safflower
g with high intensity, and increasing the temperature
1. transesterification reaction (Gerpen et al, 2004).
Diverse catalysts can be used in transesterification reaction, such as
catalyst is the most current kind of catalysts being used in biodiesel production. The excellence corresponding to
yields much ester in a short time during the appropriate circumstances of reaction
feedstocks contain large amounts of free fatty acids (FFAs).
. Since acid catalysis is relatively fast for converting the
FFAs to methyl esters, it is used as a pretreatment for the high FFA feedstocks. Then, when the FFA level has
been reduced to 0.5%, or lower, an alkali catalyst is added to convert the triglycerides to methyl esters. This
process can convert high free fatty acid feedstocks quickly and effectively
The free fatty acids do the reaction with methanol in the presence of acidic catalyst (sulfuric acid) that yield
, as shown in figure 2. It is probable for the esterification reaction to occur sequentially in
being produced should be derived away.
Figure 2. esterification reaction in the presence of acidic catalyst in order to convert

Carthamus tinctoriu
transesterification reaction.
concentration percent on the biodiesel conversion percent
MATERIALS AND METHODS
seeds from Tabriz University of Agriculture, n-Hexane 99% from Mojallali
%, Methanol 99.7%, sulfuric acid 99% and isoprop
paar viscometer of SVM-3000 model, the
580, Perkin Elmer Gas chromatograph
The Safflower seed was prepared as the powder through using rotary mill and 100g of it was put into
in order to extract the oil. The extraction process was done through using
s. Next, the rotary device was used for
Safflower seed was
g with high intensity, and increasing the temperature lead to the decreasing
(Gerpen et al, 2004).
such as acidic, base, and enzyme. The alkali
catalyst is the most current kind of catalysts being used in biodiesel production. The excellence corresponding to
yields much ester in a short time during the appropriate circumstances of reaction
feedstocks contain large amounts of free fatty acids (FFAs). These free
. Since acid catalysis is relatively fast for converting the
FFAs to methyl esters, it is used as a pretreatment for the high FFA feedstocks. Then, when the FFA level has
ert the triglycerides to methyl esters. This
(Gerpen et al, 2004)
The free fatty acids do the reaction with methanol in the presence of acidic catalyst (sulfuric acid) that yield
, as shown in figure 2. It is probable for the esterification reaction to occur sequentially in
convert free fatty acids to methyl ester
Carthamus tinctoriu) oil, to survey
transesterification reaction. The goal of this research paper is
on the biodiesel conversion percent

Hexane 99% from Mojallali
opropyl alcohol 99% from Germany Mer
3000 model, the
580, Perkin Elmer Gas chromatograph
The Safflower seed was prepared as the powder through using rotary mill and 100g of it was put into
. The extraction process was done through using
s. Next, the rotary device was used for
was 29%.
to the decreasing
acidic, base, and enzyme. The alkali
catalyst is the most current kind of catalysts being used in biodiesel production. The excellence corresponding to
yields much ester in a short time during the appropriate circumstances of reaction
hese free fatty acids will react with
. Since acid catalysis is relatively fast for converting the
FFAs to methyl esters, it is used as a pretreatment for the high FFA feedstocks. Then, when the FFA level has
ert the triglycerides to methyl esters. This
(Gerpen et al, 2004).
The free fatty acids do the reaction with methanol in the presence of acidic catalyst (sulfuric acid) that yield
, as shown in figure 2. It is probable for the esterification reaction to occur sequentially in
free fatty acids to methyl ester
to survey the physical attributes of
goal of this research paper is
on the biodiesel conversion percent
Hexane 99% from Mojallali
l alcohol 99% from Germany Mer
3000 model, the flash point device of P611A
580, Perkin Elmer Gas chromatograph device were used for the
The Safflower seed was prepared as the powder through using rotary mill and 100g of it was put into
. The extraction process was done through using
s. Next, the rotary device was used for solvent separation from the
to the decreasing in the time of

acidic, base, and enzyme. The alkali
catalyst is the most current kind of catalysts being used in biodiesel production. The excellence corresponding to
yields much ester in a short time during the appropriate circumstances of reaction
fatty acids will react with
. Since acid catalysis is relatively fast for converting the
FFAs to methyl esters, it is used as a pretreatment for the high FFA feedstocks. Then, when the FFA level has
ert the triglycerides to methyl esters. This
The free fatty acids do the reaction with methanol in the presence of acidic catalyst (sulfuric acid) that yield
, as shown in figure 2. It is probable for the esterification reaction to occur sequentially in

free fatty acids to methyl ester (Hingu et al,
the physical attributes of
goal of this research paper is
on the biodiesel conversion percentage.
Hexane 99% from Mojallali Company
l alcohol 99% from Germany Mer
point device of P611A
device were used for the
The Safflower seed was prepared as the powder through using rotary mill and 100g of it was put into
. The extraction process was done through using
solvent separation from the
293
the time of
acidic, base, and enzyme. The alkali
catalyst is the most current kind of catalysts being used in biodiesel production. The excellence corresponding to
yields much ester in a short time during the appropriate circumstances of reaction
fatty acids will react with
. Since acid catalysis is relatively fast for converting the
FFAs to methyl esters, it is used as a pretreatment for the high FFA feedstocks. Then, when the FFA level has
ert the triglycerides to methyl esters. This
The free fatty acids do the reaction with methanol in the presence of acidic catalyst (sulfuric acid) that yield
, as shown in figure 2. It is probable for the esterification reaction to occur sequentially in
(Hingu et al,
the physical attributes of
goal of this research paper is to
age.
Company,
l alcohol 99% from Germany Merck
point device of P611A
device were used for the
The Safflower seed was prepared as the powder through using rotary mill and 100g of it was put into
. The extraction process was done through using
solvent separation from the
Intl J Agri Crop Sci



appropriate
2007)

me
solution in the presence of Phenolphthalein


Where A is the catalyst volume
(N=0.1) and W
FFA esterification reaction was carried out using methanol and sulfuric acid.
was poured
acid we
reaction
composed of
the reaction was titrated again and y
containing 0.1% free fatty acid is

poured
reflux and stirring in the presence of KOH and methanol
separating funnel so as to phase separation (biodiesel and glycerin)
separating
Drawing attention toward the purifying of biodiesel after extricating glycerin,
performed and then it was dried with magne

reaction was implemented at three levels of 0.5%, 1%, and 1.5% for the catalyst concentration and for three molar
ratios of alco
experiments through using weight method.



determined
fatty acid.

Intl J Agri Crop Sci


The presence of 1% free fatty acid in oil sparks the beginning of
appropriate separation
2007).
The titration method was applied in order to measure the free fatty acid of Safflower oil. According to this
method, a determined amount of oil (3 or 4 drops) was titrated in the solved isopropyl alcohol with 0.1 normal KOH
solution in the presence of Phenolphthalein


Where A is the catalyst volume
(N=0.1) and W
FFA esterification reaction was carried out using methanol and sulfuric acid.
was poured in a two
acid were added to it. The reaction was done for 10 hours between 60
reaction, the interior content of the balloon was poured into the separat
composed of
the reaction was titrated again and y
containing 0.1% free fatty acid is
In order to run the transesterfication reaction,
poured in a two
reflux and stirring in the presence of KOH and methanol
separating funnel so as to phase separation (biodiesel and glycerin)
separating funnel because of the low
Drawing attention toward the purifying of biodiesel after extricating glycerin,
performed and then it was dried with magne
In order to survey the contribution of the catalyst weight
reaction was implemented at three levels of 0.5%, 1%, and 1.5% for the catalyst concentration and for three molar
ratios of alco
experiments through using weight method.


The derived oil was methylated via
determined by GC. Figure 3 depicts the fatty acid
fatty acid.

Intl J Agri Crop Sci. Vol., 5 (
The presence of 1% free fatty acid in oil sparks the beginning of
separation of organic and
The titration method was applied in order to measure the free fatty acid of Safflower oil. According to this
thod, a determined amount of oil (3 or 4 drops) was titrated in the solved isopropyl alcohol with 0.1 normal KOH
solution in the presence of Phenolphthalein
Where A is the catalyst volume
(N=0.1) and W
cat
is the molecular
FFA esterification reaction was carried out using methanol and sulfuric acid.
in a two-neck round bottom flask
re added to it. The reaction was done for 10 hours between 60
the interior content of the balloon was poured into the separat
composed of water and extra methanol was separated after turning out to two
the reaction was titrated again and y
containing 0.1% free fatty acid is
In order to run the transesterfication reaction,
a two-neck round bottom flask
reflux and stirring in the presence of KOH and methanol
separating funnel so as to phase separation (biodiesel and glycerin)
funnel because of the low
Drawing attention toward the purifying of biodiesel after extricating glycerin,
performed and then it was dried with magne
In order to survey the contribution of the catalyst weight
reaction was implemented at three levels of 0.5%, 1%, and 1.5% for the catalyst concentration and for three molar
ratios of alcohol to oil ( 6:1, 7:1, and 8:1)
experiments through using weight method.
The derived oil was methylated via
by GC. Figure 3 depicts the fatty acid
. Vol., 5 (3), 292-29
The presence of 1% free fatty acid in oil sparks the beginning of
of organic and
The titration method was applied in order to measure the free fatty acid of Safflower oil. According to this
thod, a determined amount of oil (3 or 4 drops) was titrated in the solved isopropyl alcohol with 0.1 normal KOH
solution in the presence of Phenolphthalein
Where A is the catalyst volume (KOH) need
the molecular weight of the catalyst (g) which is equal to 56.1 g/gmol for KOH.
FFA esterification reaction was carried out using methanol and sulfuric acid.
neck round bottom flask
re added to it. The reaction was done for 10 hours between 60
the interior content of the balloon was poured into the separat
and extra methanol was separated after turning out to two
the reaction was titrated again and y
containing 0.1% free fatty acid is used
In order to run the transesterfication reaction,
neck round bottom flask
reflux and stirring in the presence of KOH and methanol
separating funnel so as to phase separation (biodiesel and glycerin)
funnel because of the low
Drawing attention toward the purifying of biodiesel after extricating glycerin,
performed and then it was dried with magne
In order to survey the contribution of the catalyst weight
reaction was implemented at three levels of 0.5%, 1%, and 1.5% for the catalyst concentration and for three molar
hol to oil ( 6:1, 7:1, and 8:1)
experiments through using weight method.
The derived oil was methylated via
by GC. Figure 3 depicts the fatty acid
Figure 3. The chromatogram of
97, 2013
The presence of 1% free fatty acid in oil sparks the beginning of
of organic and aqueous
The titration method was applied in order to measure the free fatty acid of Safflower oil. According to this
thod, a determined amount of oil (3 or 4 drops) was titrated in the solved isopropyl alcohol with 0.1 normal KOH
solution in the presence of Phenolphthalein (Equation 1)
FFA
(KOH) needed for oil titration
weight of the catalyst (g) which is equal to 56.1 g/gmol for KOH.
FFA esterification reaction was carried out using methanol and sulfuric acid.
neck round bottom flask, and
re added to it. The reaction was done for 10 hours between 60
the interior content of the balloon was poured into the separat
and extra methanol was separated after turning out to two
the reaction was titrated again and yielded 0.1% oil free fatty acid.
used for the transesterification reaction with KOH
In order to run the transesterfication reaction,
neck round bottom flask and heated up
reflux and stirring in the presence of KOH and methanol
separating funnel so as to phase separation (biodiesel and glycerin)
funnel because of the low-density attribute on the part of the biodiesel compared to that of glycerin.
Drawing attention toward the purifying of biodiesel after extricating glycerin,
performed and then it was dried with magnesium sulfate.
In order to survey the contribution of the catalyst weight
reaction was implemented at three levels of 0.5%, 1%, and 1.5% for the catalyst concentration and for three molar
hol to oil ( 6:1, 7:1, and 8:1). The amount of methyl ester (biodiesel) was obtained for the whole
experiments through using weight method.
RESULTS AND DISCUSSION
The derived oil was methylated via Metcalf method
by GC. Figure 3 depicts the fatty acid
Figure 3. The chromatogram of
The presence of 1% free fatty acid in oil sparks the beginning of
phases through saponification
The titration method was applied in order to measure the free fatty acid of Safflower oil. According to this
thod, a determined amount of oil (3 or 4 drops) was titrated in the solved isopropyl alcohol with 0.1 normal KOH
(Equation 1) (Knothe et al, 2005).
FFA=
0.5 A
w
for oil titration (ml), W is the amount of sample
weight of the catalyst (g) which is equal to 56.1 g/gmol for KOH.
FFA esterification reaction was carried out using methanol and sulfuric acid.
and heated up to 55
re added to it. The reaction was done for 10 hours between 60
the interior content of the balloon was poured into the separat
and extra methanol was separated after turning out to two
ielded 0.1% oil free fatty acid.
the transesterification reaction with KOH
In order to run the transesterfication reaction, 50 g of the production obtained from the esetrification was
heated up to 55
reflux and stirring in the presence of KOH and methanol. After that,
separating funnel so as to phase separation (biodiesel and glycerin)
density attribute on the part of the biodiesel compared to that of glycerin.
Drawing attention toward the purifying of biodiesel after extricating glycerin,
sium sulfate.
In order to survey the contribution of the catalyst weight
reaction was implemented at three levels of 0.5%, 1%, and 1.5% for the catalyst concentration and for three molar
. The amount of methyl ester (biodiesel) was obtained for the whole
RESULTS AND DISCUSSION
Metcalf method
by GC. Figure 3 depicts the fatty acid profile of the
Figure 3. The chromatogram of Safflower
The presence of 1% free fatty acid in oil sparks the beginning of
phases through saponification
The titration method was applied in order to measure the free fatty acid of Safflower oil. According to this
thod, a determined amount of oil (3 or 4 drops) was titrated in the solved isopropyl alcohol with 0.1 normal KOH
(Knothe et al, 2005).
N w
cct
w

(ml), W is the amount of sample
weight of the catalyst (g) which is equal to 56.1 g/gmol for KOH.
FFA esterification reaction was carried out using methanol and sulfuric acid.
heated up to 55 C, and 11 g methanol as well as 1 g sulfuric
re added to it. The reaction was done for 10 hours between 60-70
the interior content of the balloon was poured into the separat
and extra methanol was separated after turning out to two
ielded 0.1% oil free fatty acid. The production of the esterfication reaction
the transesterification reaction with KOH
50 g of the production obtained from the esetrification was
to 55 C. Next, the reaction was
. After that, the balloon content was poured into the
separating funnel so as to phase separation (biodiesel and glycerin). Biodiesel is set at the upper phase of the
density attribute on the part of the biodiesel compared to that of glycerin.
Drawing attention toward the purifying of biodiesel after extricating glycerin,
In order to survey the contribution of the catalyst weight percent v
reaction was implemented at three levels of 0.5%, 1%, and 1.5% for the catalyst concentration and for three molar
. The amount of methyl ester (biodiesel) was obtained for the whole
RESULTS AND DISCUSSION
Metcalf method and the profile of the
of the Safflower oil, and table 1 shows the percent of each
Safflower oil used in the study
The presence of 1% free fatty acid in oil sparks the beginning of secondary
phases through saponification (Hingu et al, 2010; Meka et al,
The titration method was applied in order to measure the free fatty acid of Safflower oil. According to this
thod, a determined amount of oil (3 or 4 drops) was titrated in the solved isopropyl alcohol with 0.1 normal KOH
(Knothe et al, 2005).
(ml), W is the amount of sample
weight of the catalyst (g) which is equal to 56.1 g/gmol for KOH.
FFA esterification reaction was carried out using methanol and sulfuric acid. In order to do this, primarily, 50g of oil
C, and 11 g methanol as well as 1 g sulfuric
70 C under re
the interior content of the balloon was poured into the separating funnel and the lower phase which
and extra methanol was separated after turning out to two-phase status.
The production of the esterfication reaction
the transesterification reaction with KOH alkali
50 g of the production obtained from the esetrification was
Next, the reaction was
the balloon content was poured into the
. Biodiesel is set at the upper phase of the
density attribute on the part of the biodiesel compared to that of glycerin.
Drawing attention toward the purifying of biodiesel after extricating glycerin, the water washing process was
percent variables and alcohol to oil molar ratio,
reaction was implemented at three levels of 0.5%, 1%, and 1.5% for the catalyst concentration and for three molar
. The amount of methyl ester (biodiesel) was obtained for the whole

and the profile of the
oil, and table 1 shows the percent of each
oil used in the study
secondary reactions and prevents the
(Hingu et al, 2010; Meka et al,
The titration method was applied in order to measure the free fatty acid of Safflower oil. According to this
thod, a determined amount of oil (3 or 4 drops) was titrated in the solved isopropyl alcohol with 0.1 normal KOH
(ml), W is the amount of sample (g), N
weight of the catalyst (g) which is equal to 56.1 g/gmol for KOH.
In order to do this, primarily, 50g of oil
C, and 11 g methanol as well as 1 g sulfuric
C under reflux and stirring.
funnel and the lower phase which
phase status. The oil participating in
The production of the esterfication reaction
alkali catalyst.
50 g of the production obtained from the esetrification was
Next, the reaction was done for 6 hours under
the balloon content was poured into the
. Biodiesel is set at the upper phase of the
density attribute on the part of the biodiesel compared to that of glycerin.
the water washing process was
ariables and alcohol to oil molar ratio,
reaction was implemented at three levels of 0.5%, 1%, and 1.5% for the catalyst concentration and for three molar
. The amount of methyl ester (biodiesel) was obtained for the whole
and the profile of the Safflower oil fatty acid was
oil, and table 1 shows the percent of each

reactions and prevents the
(Hingu et al, 2010; Meka et al,
The titration method was applied in order to measure the free fatty acid of Safflower oil. According to this
thod, a determined amount of oil (3 or 4 drops) was titrated in the solved isopropyl alcohol with 0.1 normal KOH
N is the normality
weight of the catalyst (g) which is equal to 56.1 g/gmol for KOH. The reduction of
In order to do this, primarily, 50g of oil
C, and 11 g methanol as well as 1 g sulfuric
x and stirring. After the
funnel and the lower phase which
The oil participating in
The production of the esterfication reaction

50 g of the production obtained from the esetrification was
done for 6 hours under
the balloon content was poured into the
. Biodiesel is set at the upper phase of the
density attribute on the part of the biodiesel compared to that of glycerin.
the water washing process was
ariables and alcohol to oil molar ratio,
reaction was implemented at three levels of 0.5%, 1%, and 1.5% for the catalyst concentration and for three molar
. The amount of methyl ester (biodiesel) was obtained for the whole
oil fatty acid was
oil, and table 1 shows the percent of each

294
reactions and prevents the
(Hingu et al, 2010; Meka et al,
The titration method was applied in order to measure the free fatty acid of Safflower oil. According to this
thod, a determined amount of oil (3 or 4 drops) was titrated in the solved isopropyl alcohol with 0.1 normal KOH
is the normality
The reduction of
In order to do this, primarily, 50g of oil
C, and 11 g methanol as well as 1 g sulfuric
After the
funnel and the lower phase which
The oil participating in
The production of the esterfication reaction
50 g of the production obtained from the esetrification was
done for 6 hours under
the balloon content was poured into the
. Biodiesel is set at the upper phase of the
density attribute on the part of the biodiesel compared to that of glycerin.
the water washing process was
ariables and alcohol to oil molar ratio, the
reaction was implemented at three levels of 0.5%, 1%, and 1.5% for the catalyst concentration and for three molar
. The amount of methyl ester (biodiesel) was obtained for the whole
oil fatty acid was
oil, and table 1 shows the percent of each
Intl J Agri Crop Sci. Vol., 5 (3), 292-297, 2013

295

Based on the GC chromatogram, the Safflower oil contains these components: Myristic acid (C14} methyl
ester in minute 13.93, Palmitic acid (C16:0) methyl ester in minute15.87, Stearic acid methyl ester (C18:0) in
minute17.84, Oleic acid methyl ester (C18:1) in minute18.05, Oleic acid methyl ester cis (C18:1C) in 18.11 minute,
and Linoleic acid methyl ester (C18:2) in minute 18.61.


Table 1. fatty acid composition of safflower oil
Fatty acid Amount Unit
Myristic acid (C 14:0) 0.37 Wt.%
Palimitic acid 7.33 Wt.%
Stearic acid 2.91 Wt.%
Oleic acid 14.31 Wt.%
Linoleic acid 75.08 Wt.%
The average molecular weight of Safflower oil 874.139 g/gmol

Some of the properties of extracted oil from the Safflower seed were measured. Results are shown in table 2.

Table 2. Some physical properties of Safflower oil.
properties amount
Kinematic viscosity (40), mm
2
/s 29.9
Density (15) g/cm
3
0.91
Flash point (C) 257
Acid Value 5.38

Primarily, the transesterification reaction was run at three catalyst levels (0.5, 1, and 1.5
w
w
/ %) based on
the 6:1 molar ratio of alcohol to oil. As figure 4 depicts, the percent of biodiesel conversion is maximum at 1%
catalyst concentration. Since by increasing the catalyst weight up to 1%, the transesterification reaction steps
toward the progression of methyl ester production leading to the increase in biodiesel production, but the level
upper 1% weight of KOH causes the saponification reaction which makes the transesetrfication reaction to be
converted with lower percentage. So, the amount of produced methyl ester being formed is less for the catalyst of
1.5%.
In order to pave the efficient circumstances for biodiesel production from Safflower oil, the catalyst
concentration assumed to be fixed (constant) which was produced by 7:1 and 8:1 alcohol to oil molar ratio. The
results showed that by increasing the molar ratio from 6:1 to 8:1, the conversion percent increased by 2.8% (Fig 5).





Figure 4. The biodiesel conversion percent in different catalyst concentration including 1:6 alcohol to oil molar ratio
Catalyst concentration (%w/w)
C
o
n
v
e
r
s
i
o
n
(
%
)

90.6
96.1
76.3
70
80
90
100
0 0.3 1 1.3 2
Intl J Agri Crop Sci. Vol., 5 (3), 292-297, 2013

296





Figure 5. The biodiesel conversion percent for different alcohol to oil molar ratios (1% catalyst concentration)

Although one can say that by increasing the alcohol to oil molar ratio the reaction tends to progress toward
methyl ester production, in 6:1 molar ratio and 1% catalyst more than 96% of the oil is converted to methyl ester
and the reaction production containing 96% methyl ester can be introduced as the biodiesel fuel based on the
ASTM D6571-09 standard. Thus, 6:1 molar ratio and 1% catalyst weight percent were obtained as the optimal
variables, primarily because the minimum amount of alcohol consuming is optimal in transesterfication reaction,
secondly reproducing the excessive alcohol would cost more on the part of the energy.
In addition, some of the Safflower biodiesel properties were measured and compared with
ASTM D6751-09 standard. The characteristics of produced biodiesel from Safflower oil are in concordance with
ASTM D6751-09 which can be used as fuel.

Table 3. The produced biodiesel attributes comparison with the standard biodiesel
Fuel Properties Safflower biodiesel ASTM D6751-09 standard
Kinematic viscosity (40) mm
2
/s 4.52 1.9-6.10
Density (15 ), g/cm
3
0.87 -
Flash point, (C) 167 >130
Pour point (C) -10 -
Cloud point (C) -7 -
Freezing point (C) -12 -
Boiling point (C) 326 315 - 356

CONCLUSION

The Safflower plant is one of the regional plants of Iran which has the capability of producing oil as the
primary element of biodiesel thank to its conformity to Iran weather conditions. Biodiesel production from the
obtained oil is economical according to the high efficiency of this oily seed and producing lateral productions such
as Safflower meal and its natural pigments from the leaves.
Safflower oil contains more than 75% of linoleic acid. The unsaturated fatty acids lead to improve the pour
and cloud points efficient. This oil acid value was 5.38, 257 C of boiling point, 29.9 mm
2
/s of Kinematic viscosity,
and 0.91 g/cm
3
of density.
Assuming the lower pour and cloud points on the part of the Safflower biodiesel, one can claim that it is
appropriate to be used in cold climates. The reason behind the lower cloud point and pour point is the upper
degree of unsaturation status, and the results obtained from GC confirm this claim. Because the safflower biodiesel
contains more than 70% of linoleic acid.
Since the most kind of fatty acid is that of the linoleic in Safflower biodiesel, the boiling point of the
structure is high which plays an important role in terms of safety in saving and transportation.
The optimum conditions were obtained 6:1 alcohol to oil molar ratio and 1% catalyst concentration for
biodiesel production.
The produced biodiesel is in concordance with the D6751-09 standard in terms of optimum conditions
including 96% of methyl ester content, 4.52 mm
2
/s of Kinematic viscosity and 167 C of flash point which can be
used as the biodiesel fuel.


Molar ratio
C
o
n
v
e
r
s
i
o
n
(
%
)

96.1
98.2
98.8
90
92
94
96
98
100
3 3.3 6 6.3 7 7.3 8 8.3 9
Intl J Agri Crop Sci. Vol., 5 (3), 292-297, 2013

297

REFRENCES

Canakci M, Van Gerpen J. 1999. Biodiesel production via acid catalysis, Transactions of Agricultural and Biological Engineers, 42, 1203-1210.
Dorado MP, Ballesteros E, Arnal JM, Lopez FJ. 2003. Exhaust Emissions From a Diesel Engine Fueled with Transesterified Waste Olive Oil,
Journal of Fuel, 82, 1311-1315.
Fukuda H, Kondo , Noda H. 2001. Journal of Bioscience and Bioengineering, 92, 405-416.
Gerpen JV. et al. 2004.Biodiesel Production Technology, National Renewable Energy Laboratory, 1617 Cole Boulevard, Golden.
Hingu MH, Gorate PR, Rathod VK. 2010. Synthesis of biodiesel from waste cooking oil using sonochemical reactors , Ultrason Sonochem,
17, 827832.
Knothe G, Van Gerpen JH, Krahl J. 2005. The biodiesel handbook, Amer Oil Chemists Society.
Ma F, Hanna MA. 1999. Biodiesel Production: a review, Bioresource Technology, 70, 1-15.
Meka PK, Tripathi V, Singh RP. 2007. Synthesis of biodiesel fuel from safflower oil using various reaction parameters, Journal of Oleo
Science, 56(1), 9-12.
Nurun Nabi Md, Shamim Akhter Md, Zaglul Shahadat, Mhia Md. 2006. Improvement of Engine Emissions with Conventional Diesel Fuel and
Diesel-Biodiesel Blends, Journal of Biosource Tecnology, 97, 372-378.