International Journal of Chemical

& Petrochemical Technology (IJCPT)

ISSN(P): 2277-4807; ISSN(E): 2319-4464
Vol. 4, Issue 5, Oct 2014, 5-12
TJPRC Pvt. Ltd.

MICROWAVE TRANSESTERIFICATION OF SOXHLET EXTRACTED JATROPHA

CURCUS & KARANJA OILS AND ITS ANALYSIS
SATYENDRA SINGH TOMAR1, DEEPAK GUPTA2, MEENAKSHI KUSHWAH3 & SHALINI GUPTA4
1,2

Department of Chemical Engineering, S. S. S. U. T. M. S, Sehore, Madhya Pradesh, India

3
4

Jiwaji University, Gwalior, Madhya Pradesh, India

Bundelkhand University, Jhansi, Uttar Pradesh, India

ABSTRACT
A number of methods for biodiesel fuel production have been industrialized, among which transesterificationgives
high levels of conversion of triglycerides to their corresponding methyl esters using alcohol and alkali-catalysis in lesser
reaction times. This process has therefore been widely utilized for biodiesel fuel production in a number of countries.
In this research work the oils from Jatropha Curcus and Karanja seeds where extracted by Soxhlet extraction process.
These oils were converted into their respective methyl esters (known as biodiesel) via microwave transesterification.
The reaction in the presence of catalyst (NaOH) was carried out to study the optimum conditions and to detect the effects
of reaction variables like alcohol (methanol) to oil molar ratios, catalyst concentrations, reaction temperatures and reaction
times. The physiochemical properties of oils and derived biodiesels were studied and compared with the values of
conventional diesel.

KEYWORDS: Soxhlet Extraction, Alkali-Catalysis, Microwave Transesterification Biodiesel

INTRODUCTION
Biodiesel is an alternative fuel made from renewable biological sources such as vegetable oils both (edible and
non-edible oil) and animal fats. Non-edible plant oilsmay provide better alternatives for energy persistence. Plant-derived
oils could be used directly in diesel engines or blended with petro-diesel, still, their high viscosity lead to problems in the
engine.[1,2] Inefficient oil - air mixing causes poor injector system performance which leads to incomplete combustion
hence producing high smoke and causing ringsticking, filter plugging and engine deposits. [3] Converting to biodiesel is one
of the options to reduce the viscosity of vegetable oils.
In the present work Jatropha Curcus & Karanja seeds (Non-edible oil sources) were utilized as feed stocks for the
production of biodiesel (alkyl esters). The oils from seeds were extracted by Soxhlet extraction process. Derived oils were
converted to biodiesel by Microwavetransesterification. Jatropha Curcus & Karanja oils are the prime non-edible sources
available in India.
Jatropha Curcus & Karanja contains 30% or more oil in their seed, fruit or nut. India has more than 300 species of
trees, which produce oil bearing seeds. [4]
Jatropha Curcus is a poisonous, semi-evergreen shrub or small tree, reaching a height of 6 m.[5] It is resistant to a
high degree of aridity, allowing it to be grown in deserts. The seeds contain 27 - 40% oil (average: 34.4%) [6,7] that can be
processed to produce a high-quality biodiesel fuel, usable in a standard diesel engine. Karanja oil is obtained from the
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Satyendra Singh Tomar, Deepak Gupta, Meenakshi Kushwah & Shalini Gupta

seeds of the Millettia pinnata tree, which is inherent to tropical and temperate Asia. The seeds contain Karanja oil 2736%
by weight. This nonedible oil is bitter, red brown, thick and non-drying.
oil. Many studies have been done to convert Karanja oil into biodiesel.

[8]

[9, 10]

This oil is also commonly named as pongamia

Basic nutritional components of Karanja seeds

may change depending the season and maturity of the tree.

Presently, viable biodiesel production processes are centered on either conventional or supercritical heating
methods. Commonly used methods are Pyrolysis, Micro-emulsions, Dilution and Transesterification of oils to esters.
[11- 14]

Among these techniques, transesterification is the simplest and the most efficient path to produce biodiesel.

Transesterification of oils from any feedstock is to simply reduce the viscosity of the oils derived from them. In this
process alcohol (methanol) in the presence of a catalyst (acid, alkali or enzyme) is used to chemically break the molecule
of the oils into methyl esters of the renewable fuel.The overall process is a series of three consecutive and reversible
reactions, in which di and mono glycerides are formed as intermediates, yielding one ester molecule in each step.
The stoichiometric reaction requires 1 mole of a triglyceride and 3 moles of the alcohol (methanol). The reaction
mechanism is shown in figure 1. As methanol is used in this process it is also called methanolysis.

Figure 1: Transesterification Reaction for Biodiesel Production

However, excess amount of alcohol (methanol) is used to increase the yields of the alkyl esters (methyl esters) by
shifting the equilibrium towards the formation of esters and to allow its phase separation from the glycerol formed as a
byproduct. The product of transesterification process is biodiesel.
Transesterification of organic feedstock to yield biodiesel can be performed by various methods like Conventional
heating with acid, base catalysts and co-solvents,[15] Sub and super-critical methanol conditions with co-solvents and
without catalyst,[16] Enzymatic method using lipases,[17] Microwave irradiation with acid, base and heterogeneous catalysts.
[18]

Among these methods, conventional heating method needs longer reaction periods with higher energy efforts and losses

to the ambient.

[18]

Super and sub-critical methanol process operates in expensive reactors at high temperatures and

pressures resulting in higher energy inputs and higher production costs.

much lower temperatures, requires much longer reaction times.

[17]

[19]

The enzymatic method, though operates at

Microwave transesterification, in contrast,

is energy-efficient and quick process to produce biodiesel from different feedstock.

[18]

The advantage of microwave

assisted reactions clearly reflects in short reaction times by rapid heating and cooling and produces cleaner reaction
products. A very high increase in (5 to 1000 times) reaction rates was reported by early investigators. [16, 20]

Impact Factor (JCC): 2.9866

Index Copernicus Value (ICV): 3.0

Microwave Transesterification of Soxhlet Extracted Jatropha Curcus & Karanja Oils and its Analysis

MATERIALS AND METHODS

Jatropha Carcus and Karanja seeds collected from local market at Bhopal, M. P, India. All the chemicals utilized
were of analytical grade.
Oil Extraction
Oil extraction of seeds was performed using a Chemglass 300 mL soxhlet apparatus with n-hexane as solvent.
The Soxhlet apparatus allowed the extraction of oil from the seeds using a distillation extraction method. 20 grams of
kernels were grinded in a food processing unit. The grinded seeds were placed into a porous cellulose thimble inside the
extraction chamber. The extraction chamber was placed into the Soxhlet apparatus above a flask containing 300 mL of
n-hexane and under an overhead condenser. The flask was submerged in a water bath and heated to approximately 90 C
using a hotplate, evaporating the solvent into the condenser which trickled back down into the extraction chamber soaking
the grinded seeds. Finally the oil was concentrated in the bottom flask, and the n-hexane was evaporated and reclaimed into
another flask using an overhead condenser leaving only the lipids behind.
Biodiesel by Microwave Transesterification
The chemical conversion of the oils obtained to its corresponding fatty esters (biodiesel) were performed using
methanol (solvent) in the presence of sodium hydroxide (NaOH) as a catalyst to break chemically the molecule of the raw
seeds oil into methyl esters with glycerol as a by-product. The reaction occurred while being irradiated with 600W of
microwave power, for 60 to 180 seconds at atmospheric pressure in a multimode microwave reactor which was
mechanically modified to perform the reaction. Resulting mixture was cooled and allows separating for 12 hours. The byproduct (glycerol) was decanted out and the obtained methyl esters were analyzed. Here, the biodiesel obtained from seeds
were abbreviated as KOME (Karanja oil methyl esters) and JOME (Jatropha oil methyl esters).

RESULT AND DISCUSSIONS

The compositions of Jatropha and Karanja seeds are shown in table 1.
Table 1: Chemical Composition of Seeds
Jatropha (wt %)
Karanja (wt %)

:
:

Moisture
6.2
18

Protein
18
34

Oil
38
33

Carbohydrates
17
6

Fiber
15.5
6.5

Ash
5.3
2.5

The oil component of Jatropha and Karanja seeds were found to be 38 and 33 % respectively.
Analysis of Jatropha (JO) and Karanza Oil (KO) obtained from Soxhlet extraction is being illustrated in table 2.
Table 2: Fatty Acid Composition of Jatropha (JO) and Karanza Oil (KO) in wt %
Systematic Name
Myristic acid
Palmitic acid
Palmitolileic acid
Stearic acid
Oleic acid
Linoleic acid
Linolenic acid
Arachidice acid
Behenic acid
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Formula
C14H28O2
C16H32 O2
C16H30O2
C18H38O2
C18H34O2
C18H32O2
C18H30O2
C20H40O2
C22H44O2

JO wt.%
0.1
15
1.1
6.3
40
38
0.2
0.3
0.1

KO wt.%
7
7
51
27
6
1
1
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Satyendra Singh Tomar, Deepak Gupta, Meenakshi Kushwah & Shalini Gupta

Effect of Alcohol to Extracted Oil Ratio

The reaction was carried out by varying the molar ratio of alcohol (methanol) to oil (obtained from Jatropha &
Karanja seeds) and reaction time at 65 oC in microwave for reaction time 60, 120 and 180 seconds respectively.
The concentration of catalyst (NaOH) was kept constant to 1% w/w of oil. The Biodiesel (methyl ester) content increased
as the alcohol to oil ratio increased for both type of oils extracted from Jatropha & Karanja seeds. The methyl esters
content for alcohol to oil molar ratio of 5:1 was 92.8 % w/w for Jatropha oil and about 91 % for Karanja oil after 60
seconds. The biodiesel at ease of 97.2 and 96.1 & % w/w at alcohol to oil molar ratio of 5:1 were attained in 180 seconds
for Jatropha and Karanja seeds respectively as shown in figure 2, where JOME (Jatropha oil methyl ester) and KOME
(Karanja oil methyl ester).

Figure 2: Microwave Transesterification of Jatropha and Karanja Oil at Different Alcohol to Oil Molar
Ratios and Time Periods
Though for alcohol to oil molar ratios of 10:1, 15:1 and 20:1 the higher yield of biodiesel contents was obtained in
a reduced amount of time, these higher ratios should be evaded for cost-effective motives. Thus, alcohol to oil molar ratios
of 5:1 was selected as being the optimum.Statistically it was predicted that this reaction was faster for higher alcohol to oil
molar ratio, whereas substantially more time was required to get the same methyl ester content for lower alcohol to oil ratio
for both seeds oil. This has also been reported by Maher et al. [15, 20]
For industrial uses, methanol can be recovered by distillation to minimize the methanol consumption in the
biodiesel production and it can then be returned to the process, bringing about in a decrease of both environmental
influences and operative overheads.
Effects of Catalyst Concentration
In the present study, low cost alkali (NaOH) was chosen as catalyst for transesterification of extracted Jatropha
and Karanja oils. The experiments were conducted varying the catalyst concentrations and reaction times using alcohol to
oil molar ratio of 5:1 at 65 C.
It was observed that the concentration of NaOH had a significant effect on transesterification. The Biodiesel
(methyl ester) content increased with higher catalyst concentrations. These results were found to concur with those
obtained by Maher et al.

[15, 20]

However, with the catalyst concentration greater than 2% w/w oil it was not possible to

achieve the products due to the formation of soap and a viscous deposit in the reaction mixture. A similar result was also

Impact Factor (JCC): 2.9866

Index Copernicus Value (ICV): 3.0

Microwave Transesterification of Soxhlet Extracted Jatropha Curcus & Karanja Oils and its Analysis

observed by Leung et al.

[21]

Again it was also found that the reaction virtually not arising with a catalyst concentration of

0.25% w/w of oils. At a catalyst concentration of 1% w/w of oils, the biodiesel content achieved 97.2 and 96.1 % w/w after
180 seconds for Jatropha and Karanja oils respectively as shown in figure 3.

Figure 3: Microwave Transesterification of Jatropha and Karanja Oil at Different Catalyst (NaOH)
Concentrations
Although, the catalyst concentration of 1.5 % w/w of oils provided better biodiesel content than that of 1% w/w of
oils for all reaction times. The methyl ester (biodiesel) layer obtained has to be washed with hot distilled water several
times in the water washing stage, so there is a option of mislaying some biodiesel product to emulsion formation.
On account of the cost of the additional NaOH, and the cost of removing the residual catalyst from the biodiesel
layer, higher concentration of NaOH should be avoided. For such causes, 1% w/w of oils was considered as optimized
catalyst concentration.
Effects of Reaction Temperature
The operating conditions were fixed at alcohol to oil molar ratio of 5:1 and a catalyst concentration of 1% w/w of
oils. The experiments were conducted varying the reaction temperature for both the oils. It was specified from the effects
of changing temperature that transesterification could not occur at room temperature for both for Jatropha and Karanja oils,
even if the reaction time were extended.
The biodiesel contents of the Jatropha and Karanja oils increased with temperature for the same reaction time.
These results were covenant with those obtained by other researchers.[20, 22] The increase in the biodiesel (methyl ester)
content may be due to the decreasing viscosity of the oil with a raise in reaction temperature. Resulting in an increase in the
solubility of the oils in the alcohol and enhancing the contact between the oils and the alcohol.[21,23,24] Hence, at higher
temperature the reaction was faster. The transesterification progressed to achieve in 180 seconds in microwave at 65 C,
and the diesel content of 97.2 and 96.1 % w/w for Jatropha and Karanja oils respectively. Hence, 65 C was chosen as the
optimum reaction temperature as shown in figure 4.

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10

Satyendra Singh Tomar, Deepak Gupta, Meenakshi Kushwah & Shalini Gupta

Figure 4: Microwave Transesterification of Jatropha and Karanja Oil at Different Reaction Temperatures
The physiochemical properties of oils extracted from Jatropha and Karanja seeds by Soxhlet Extraction and their
respective methyl esters obtained by microwave transesterification were compared with the properties of standard biodiesel
(EN14214:2008)and are shown in table 3.
EN 14214 is a European Standard that describes the requirements and test methods for Fatty Acid Methyl Ester
(FAME) the most common type of biodiesel.
Table 3: Comparison of Fuel Properties of Diesel (EN 14214:2008)
to Derived Seed Oils and Their Respective Methyl Esters
Properties

JO

JOME

KO

KOME

Density@ 15 C (gm/cc)
0.916 0.875
0.909 0.876
Viscosity@ 40C (mm2/s)
40.06 4.2
41.06 4.66
Flash Point (C)
235
186
232
183
Carbon Residue (%)
0.38
0.18
1.51

Sulphur Content (%)

0.8
0.0036 0.007
Acid Value (mg of KOH/gm) 3.71
0.27
5.91
0.42
Iodine Value
101.7 104
89
91
Saponification Value
195
202.6
185
187
Calorific Value (MJ/kg)
39.63 39.65
36.87 37.12
Cetane Number
46.3
5762 54
55
*JOME (Jatropha oil methyl ester); KOME (Karanja oil methyl ester).

Biodiesel
(EN14214:2008)
0.86-0.90
3.5-5.0
>120
<0.3
<0.01
<0.5
<120
>51

CONCLUSIONS
In this paper, an investigation of Jatropha curcas and Karanja oil as the sustainable source for biodiesel has been
conducted. Crude oils from the seeds were extracted using a Soxhlet apparatus and chemically converted to biodiesel in a
microwave via alkaline catalyst transesterification process.
Important properties of extracted oils and methyl esters such as viscosity, density, flash point, calorific value, acid
value, iodine value, Carbon residue have been determined and found that most of the parameters of methyl ester comply
with Diesel (EN14214:2008) specifications.
On microwave transesterification of extracted oils it was observed the biodiesel (methyl ester) content increased
as the alcohol to oil molar ratio increased. It was observed that the concentration of catalyst (NaOH) had a significant
Impact Factor (JCC): 2.9866

Index Copernicus Value (ICV): 3.0

11

Microwave Transesterification of Soxhlet Extracted Jatropha Curcus & Karanja Oils and its Analysis

effect on transesterification. The Biodiesel (methyl ester) content increased with higher catalyst concentrations. It was also
found that the reaction virtually not arising with a catalyst concentration of 0.25% w/w of oils.However, with the catalyst
concentration greater than 2% w/w oil it was not possible to achieve the products due to the formation of soap and a
viscous deposit in the reaction mixture.
Transesterification could not occur at room temperature for both for Jatropha and Karanja oils, even if the reaction
time were extended. The biodiesel contents of the Jatropha and Karanja oils increased with temperature for the same
reaction time. These higher ratios should be evaded for cost-effective motives. The biodiesel at ease of 97.2 and 96.1 & %
w/w at alcohol (methanol) to oil molar ratio of 5:1, Catalyst (NaOH) 1% w/w of oil were attained in 180 seconds for
Jatropha and Karanja seeds respectively.

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Impact Factor (JCC): 2.9866

Index Copernicus Value (ICV): 3.0