Biodiesel

Optimization of Oil Extraction and Transesterification
Processes and Preliminary Tests on CI Engine with

Soapnut Biodiesel
A
Project Report
Submitted in partial fulfillment of the requirement for the award of the
degree of
Master of Technology
in
Thermal & Fluids Engineering
By
Moon Vaibhav Harichandra
(Regn. No. MT2015613)
Under the Guidance of

Dr. Madhukar S. Tandale
Department of Mechanical Engineering,

Dr. Babasaheb Ambedkar Technological University,
Lonere - 402 103, Dist- Raigad, Maharashtra
2016-2017
Approval Sheet
The project report entitled “Optimization of oil extraction and transesterification

processes and preliminary test on CI engine with Soapnut biodiesel” by Moon Vaibhav
Harichandra (MT2015613) is approved for partial fulfillment of the award of the degree of
Master of Technology in Thermal & Fluids Engineering in the Department of Mechanical
Engineering.
Dr. Madhukar S. Tandale Dr. M Sadaiah

Guide Head
Department of Mechanical Engineering Department of Mechanical Engineering
Dr. Babasaheb Ambedkar Technological
University, Lonere – 402103, Raigad
Examiners
1) --------------------------------------------------------
2) ---------------------------------------------------------
Acknowledgement
I am very sincerely thankful to my guide Dr. Madhukar S. Tandale who has given lot of
Intellectual and valuable guidance for completing this project. He gave me worthy
suggestions whenever necessary. He gives constant supply of inspiration, and motivation
during entire project work. He has abundant technical, practical knowledge & more idea
about purchasing the equipment, it is helpful for accomplished this work.
I sincerely thanks to Dr. Mudigonda Sadaiah, the Head of Mechanical Engineering

Department for his encouragement and support. I specially thanks to Dr. N. Agrawal for
their suggestion, motivation. I particularly thanks to Dr. V. P. Jawanjal, HOD Petrochemical
Engineering for permitting to use Lab facility of their department for properties checking. I
appreciate Mr. Chaudhari and Mr. Lad for their valuable suggestions & help during work
of biodiesel property checking.
I express gratitude to Mr. Sangram Jadhav, Mr. Kiran Khot and Mr. Anil Poshetti for
their support and guidance during this project work. I can‟t forget my all friends and I give
heartly thanks to them for their support, help, inspiration, co-operation and love.
Finally, I am always obliged to my dear Father, Mother, Sister, Brother and my family
members for their invaluable support.
Date: Vaibhav H. Moon

Abstract
In today‟s world, the transport sector heavily depends on oil liquid derived products such as
gasoline and diesel, globally occupies the third place when the total energy consumption and
greenhouse gas emissions are considered. This consumption is predicted to increase by 60%
by 2030 mainly due to enormous growth in population, industrialization and exposure to
better living standards. Biodiesel is one of the renewable sources of energy for meeting the
global energy demand and reducing the GHC emissions effectively. The use of non-edible
feedstock is very noteworthy because it can grow in harsh and marginal lands which require
less maintenance and less soil fertility and less water as opposed to arable lands for growing
edible oils. However, it is noted that the nonedible feedstocks can also be grown in arable
lands, but this is not a general practice and is not recommended.
The tree of Sapindus Mukorossi (Soapnut) is available in north eastern region of India. Fruit
of Soapnut has many traditional usages and kernel contain 30% (w/w) of oil. Very little
research has been done on utilization of Soapnut oil for biodiesel production and on
optimization of oil extraction using Soxhelet extractor and transesterification process using
homogenous catalyst and heterogeneous catalyst. So the current done on study oil extraction
and transesterification process of Soapnut oil.
A taguchi L9 orthogonal array was used to model the relationship between the input
parameters and output responses. ANOVA technique is used to identify and quantify the most
noteworthy factor that contributes the maximum yield. The density, Flash point, cloud and
pour points for Soapnut oil methyl esters verified that almost all the characteristics of SOME
are comparable to those of diesel and this makes it a potential substitute for fuel in CI
Engines. Current work done on Soapnut finds suitability of Soapnut oil as a potential source
for biodiesel. B5 can be used as a complete replacement to diesel as its performance is close
to diesel and is concluded as optimum blend with efficiency 25.667% compared to 34.603%
of diesel. However long term study need to be carried out before suggesting SOME as an
alternative to diesel.
Keywords- Biodiesel, Soapnut, Soapnut oil methyl ester (SOME), Transesterification,

Taguchi method, Analysis of variance (ANOVA)
Contents
Abstract i
List of Figures ii
List of Tables iv
Abbreviations vi
Chapter Title
Page
1. Introduction
1
1.1 Background
1
1.1.1 Indian petroleum product scenario
2
1.1.2 International petroleum product scenario
3
1.2 Biodiesel- an Alternative Fuel to Petro-diesel
3
1.3 Scope of Work
5
1.4 Aim and Objectives of Present Study
6
1.5 Report Layout
6
2. Literature Review
8
2.1 Introduction
8
2.2 Biodiesel Feedstocks
9
2.3 Oil Extraction Techniques
11
2.3.1 Mechanical extraction
11
2.3.2 Chemical or solvent extraction
12
2.3.2.1 Soxhelet extraction
13
2.3.3 Enzymatic extraction
14
2.3.4 Supercritical fluid extraction 14
2.3.5 Microwave assisted extraction
15
2.4 Preparation of Biodiesel
16
2.4.1 Pyrolysis
17
2.4.2 Dilution
18
2.4.3 Micro-emulsification
18
2.4.4 Transesterification
19
2.4.4.1 Catalytic transesterification
20
2.4.4.1.1 Alkali catalyzed
transesterification 21
2.4.4.1.2 Acid catalyzed

2.4.4.1.3 Enzyme catalyzed

2.4.4.2 Non catalytic transesterification methods

24
2.4.4.2.1 Supercritical alcohol
2.4.4.2.2 Microwave assisted

2.4.4.2.3 Ultrasound assisted

2.5 Review of Oil Extraction and Transesterification Process

25
2.5.1 Performance characteristics of biodiesel
29
2.6 Sapindus Mukorossi (Soapnut)
32
2.7 Transesterification of Soapnut Oil
36
2.8 Performance Characteristics of Soapnut Biodiesel
37
2.9 Design of Experiments with the Taguchi Method
38
2.9.1 Signal to noise ratio analysis
38
2.9.2 Analysis of variance (ANOVA) 39
2.10 Summary of the Literature Review
39
3. Oil Extraction and Preparation of Biodiesel

41
3.1 Introduction
41
3.2 Development of Biodiesel Preparation Set-up
42
3.3 Summary
46
4. Experimental Set-up and Plan of Experiment

47
4.1 Fuel Used for Test
48
4.2 Design of Experimentation
49
4.2.1 Optimization of oil extraction Process
49
4.2.2 Optimization of transesterification Process
50
4.2.3 SOME diesel blends operations at standard engine
setting 52
4.3 Summary
52
5. Results and discussion
54
5.1 Oil Extraction
54
5.1.1 Effect of seeds size on oil yield
54
5.1.2 Effect of reaction temperature on oil yield
55
5.1.3 Effect of reaction time on oil yield
55
5.1.4 Effect of volume of solvent on oil yield
56
5.2 Effect of Type of Solvent on Oil Yield
57
5.3 Transesterification Process (Homogeneous Catalyst)
57
5.3.1 Effect of molar ratio on biodiesel yield
57
5.3.2 Effect of catalyst type on biodiesel yield
58
5.3.3 Effect of catalyst concentration on biodiesel yield
59
5.3.4 Effect of reaction temperature time on biodiesel yield
60
5.4 Transesterification Process (Heterogeneous Catalyst)
61
5.4.1 Effect of molar ratio on SOME yield
61
5.4.2 Effect of Stirrer speed on SOME yield
62
5.4.3 Effect of Catalyst concentration on SOME yield
62
5.4.4 Effect of reaction temperature on SOME yield
63
5.5 Effect of Type of Catalyst on SOME Yield
64
5.6 S/N Ratios of Experiments
65
5.7 Analysis of Variance (ANOVA) of Experiments
67
5.8 Performance Analysis of SOME at Various SOME Blends
68
5.8.1 Effect on BTE at varying loads for SOME blends
69
5.8.2 Effect on SFC at varying loads for SOME blends
69
6 Conclusions
71
References
74
Appendix 1 Specifications of the engine

78
Appendix 2 Specifications of the dynamometer
79
Appendix 3 Reading table
80
Appendix 4 Result table
83
Appendix 5 Uncertainty analysis
85
List of Figures
Figure Title Page
2.1 Manual and Automatic oil expeller 12
2.2 Schematic representation of Soxhelet extractor 13
2.3 Process of Enzymatic extraction 14
2.4 Supercritical fluid extraction 15
2.5 Microwave assisted extraction 16
2.6 Process flow chart of non-edible seeds to produce biodiesel 17
2.7 Basic transesterification technology 19
2.8 Transesterification reaction of triglycerides 19
2.9 Mechanism of alkali catalyzed transesterification of vegetable oil 22
2.10 Mechanism of acid catalyzed transesterification 23
2.11 Soapnut seeds and Kernels 34
3.1 Mechanism of transesterification reaction 41
3.2 Experimental Soxhelet extraction unit 42
3.3 Schematic diagram of biodiesel production setup 43
3.4 Biodiesel production set up 43
3.5 Flow chart of biodiesel production from crude Soapnut oil 44
3.6 Settling and Seperation 45
4.1 Schematic of engine set up 47
4.2 Overall view of engine set up 48
5.1 Effect of seeds size on oil yield 54
5.2 Effect of reaction temperature on oil yield 55
5.3 Effect of reaction time on oil yield 56

5.4 Effect of volume of solvent on oil yield 56
5.5 Effect of type of solvent on oil yield 57
5.6 Effect of molar ratio on SOME yield (Homogenous catalyst) 58
5.7 Effect of catalyst type on SOME yield (Homogenous catalyst) 59
5.8 Effect of catalyst concentration on SOME yield (Homogenous catalyst) 60
5.9 Effect of reaction temperature on oil yield (Homogenous catalyst) 60
5.10 Effect of molar ratio on SOME yield (Heterogeneous catalyst) 61
5.11 Effect of stirrer speed on SOME yield (Heterogeneous catalyst) 62
5.12 Effect of catalyst concentration on SOME yield (Heterogeneous 63

catalyst)
5.13 Effect of reaction temperature on SOME yield (Heterogeneous 64

catalyst)
5.14 Effect of type of catalyst on SOME yield 64
5.15 Brake thermal efficiency v/s load for various blends 69
5.16 Specific fuel consumption v/s load for different blends 70

List of tables
Tables Title Page
2.1 Comparison of the standards for diesel and biodiesel based on 8

American Society for Testing and Materials (ASTM).
2.2 Feedstock‟s available for biodiesel production 10
2.3 Estimated oil yields of various non-edible vegetable oil resources 11
2.4 Comparison of oil yields between common oil seeds crops 34
2.5 Major fatty acid composition of Soapnut and popular seeds 35

4.1 Properties of fuel studied 48
4.2 Comparison of the standards for diesel and biodiesel based on 49

American Society for Testing and Materials (ASTM).
4.3 Design of experimentation (Oil Extraction) 50
4.4 Design of experiments, with four parameters at three levels, for the 50
production of SOME (Homogeneous Catalyst)
4.5 Design of experimentation (Transesterification Process using 51
Homogeneous catalyst)
4.6 Design of experiments, with four parameters at three levels, for the 51
production of SOME (Heterogeneous Catalyst)
4.7 Design of experimentation (Transesterification Process using 52
Heterogeneous catalyst)
5.1 S/N ratios of the experiments (oil extraction) 65
5.2 S/N ratios of the experiments (Transesterification process using 66

homogeneous catalyst)
5.3 S/N ratios of the experiments (Transesterification process using 66
heterogeneous catalyst)
5.4 Analysis of variance for oil extraction process 67
5.5 Analysis of variance for transesterification process using 68

homogeneous catalyst
5.6 Analysis of variance for transesterification process using 68
heterogeneous catalyst
Abbreviations
CI- Compressed Ignition
BP- Brake Power
BTE- Brake Thermal Efficiency (%)
SFC- Specific Fuel Consumption (kg/kWh)
EGT- Exhaust Gas Temperature (°C)
BD- Biodiesel
SOME- Soapnut Oil Methyl Ester
SN 5 - SOME 5% with Diesel 95% by Vol.
SN 100 - SOME 100% by Vol.
ANOVA- Analysis of Variance

Chapter 1
Introduction
1.1 Background:
Majority of the world‟s energy needs are supplied through petrochemical sources, coal and
natural gases, with the exception of hydroelectricity and nuclear energy, of all, these sources
are finite and at current usage rates will be consumed shortly. Diesel fuels have an essential
function in the industrial economy of a developing country and used for transport of
industrial and agricultural goods and operation of diesel tractor and pump sets in agricultural
sector. Economic growth is always accompanied by commensurate increase in the transport.
The high energy demand in the industrialized world as well as in the domestic sector, and
pollution problems caused due to the widespread use of fossil fuels make it increasingly
necessary to develop the renewable energy sources of limitless duration and smaller
environmental impact than the traditional one. This has stimulated recent interest in
alternative sources for petroleum-based fuels. An alternative fuel must be technically
feasible, economically competitive, environmentally acceptable, and readily available. One
possible alternative to fossil fuel is the use of oils of plant origin like vegetable oils and tree
borne oil seeds [1]. Biodiesel in another definition is a non-petroleum based fuel consisting of
alkyl esters derived from transesterification of triglycerides (TG) or by the esterification of
free fatty acids (FFA) with low molecular weight alcohols [2]. This fuel is biodegradable and
non-toxic and has low emission profiles as compared to petroleum diesel. Usage of biodiesel
will allow a balance to be sought between agriculture, economic development and the
environment. [1]
The term compressed-ignition (CI) is used all over the world to denote diesel oil engines.
This includes two or four stroke engines with airless fuel injection. The combustion is
initiated by injection of fuel to the highly compressed air. The concept of compressed-
ignition (CI) Engines is credited to great German Engineer Rudolf Diesel. Great inventor of
diesel engines Rudolf Diesel was born in Paris (1858-1913). In 1892, he proposed
“compression of air alone until a sufficiently high temperature was attained to ignite the
fuel which was to be injected at end of compression stroke”. In his first experiment, he
tried to inject coal dust into a cylinder containing air that has been already highly
compressed. He was successful only to some extent. Later on he turned to liquid and
achieved success after four years of extreme hard work. The invention of diesel engine was
financed by M.A.N of Augsburg. Later by end of journey of this great inventor, engine he
invented and fuel used are known by his name called “Diesel Engine” for CI Engines. [3]
One prominent key on liquid fuel was given by Rudolf Diesel. He used peanut oil as fuel for
demonstration on CI Engine, and suggested it as an alternative fuel option. However, he
quoted very true predicting fact as, „„the use of vegetable oil for engine fuels may seem
insignificant today. But such oils may become, in course of time, as important as
petroleum and the coal tar products of the present time‟‟- Rudolf Diesel, 1912. After
eight decades, the awareness about environment rose among the people to search for an
alternative fuel that could burn with less pollution. Rudolf Diesel‟s prediction is becoming
true today with more and more bio-diesel being used all over the world. [4]
CI Engines are well known as better power source due to high thermal efficiency, fuel
economy, higher compression ratio, lean air-fuel mixture operation, good reliability, higher
performance, and fuel economy compared to Spark Ignition (SI) Engine. Due to these merits,
CI Engines are predominantly used to drive tractors, heavy Lorries, trucks, buses, moving
machinery etc. Also, CI Engines are quality governed engines. Owing to low fuel
consumption, CI Engines have become increasingly attractive for small Lorries, various
agriculture machines and passenger cars [3, 5, 7]. Besides, CI Engines run on diesel, dual fuel
such as LPG, CNG, bio-gas, producer gas, with diesel as pilot fuel, and alternative fuels like
bio-diesel, its blend with diesel. Diesel is abundantly used as fuel for CI Engines. Also,
diesel, bio-diesel fuels are non-volatile, more viscous and self-lubricating [5]. However,
biodiesel is emerging efficient and economical alternative fuel for diesel in CI Engines
without any considerable modifications in existing engine. [6]
1.1.1 Indian petroleum products scenario:
At present, India is producing only 30% of the total petroleum fuels required. The remaining
70% is being imported, which cost about Rs. 80,000 crore every year. It is an astonishing fact
that mixing 5% biodiesel fuel to the present diesel fuel is made available in our country,
which can save Rs. 4000 crore every year. It is estimated that India will be able to produce
288 metric tons of biodiesel by the end 2012, which will supplement 41.14% of the total
demand of diesel fuel consumption in India. The Planning commission of India has launched
a bio-fuel project in 200 districts from 18 states in India. It has recommended two plant
species, viz. Jatropha and Karanja for biodiesel production. The recent auto fuel policy
document states that biofuels are eco-friendly and 100% natural energy alternative to
petroleum fuels. [7]
1.1.2 International petroleum product scenario:
Petroleum consumption has increased over the last few decades due to expansion of human
population and industrialization, which has resulted in depletion of fossil fuel reserves and
increasing petroleum price. Furthermore, the scarcity of conventional fossil fuels, increasing
emissions of combustion generated pollutants, greenhouse gases have led to atmospheric
pollution ad global warming. These and additional effects of their growing costs will make
biofuels more attractive. [10]
Use of biodiesel is catching up all over the world especially on developed countries. In
Malaysia, the tropical climate encourages production of biodiesel from palm oil. The US is
contributing 25% of the world‟s greens house. We also need to recognize its 70% of oil
consumption is in transportation. The cost of biofuels is $3.00 a gallon. With the tax subsidy
available legally now, it could be sold for about for about $1.80. It is clearly known that the
future depends on biofuels as replacement for fossil fuels. At present US uses 50 million
gallons and European countries use 350 million gallon of biodiesel annually. [7]
The increasing price factor coupled with increased awareness about environmental
degradation has prompted governments and scientific community the world over to look for
suitable alternative fuels. During the last decades the uses of alternative fuels for diesel
engines have received renewed serious attentions. It is important to explore the feasibility of
substitution of diesel with an alternative fuel, which can be produced within the country on a
massive scale for commercial utilization. [8]
1.2 Biodiesel – an Alternative Fuel to Diesel
Biodiesel an alternative fuel to diesel is renewable, biodegradable, technically feasible,

economically competitive, environmental friendly, non-toxic, portable, eco-friendly, fuel and
easily available. It is derived from vegetable oils as well as animal fast through esterification
and transesterification reaction of free fatty acids and triglycerides, respectively that occur
naturally in renewable biological resources. In other words, biodiesel can be defined as a
mixtu7re of alkyl esters of long chain fatty acids, which is synthesized through esterification
and transesterification of free fatty acids and triglycerides. [10]
It can offer lots of benefits, including reduction of greenhouse gas emissions, regional
development, and social structure especially to developing countries. In addition, biodiesel
methyl esters improve the lubrication properties of the diesel fuel blend. It is a good lubricant
which is about 66% better than diesel. Based on the overall life cycle analysis, biodiesel is
shown to be sustainable. However the higher cost of production than petroleum diesel is the
main drawback for the commercialization of biodiesel. [10]
Merits of biodiesel:
1. It is renewable and energy efficient fuel

2. It can be used as a 20% blend in most diesel equipped with no or only minor
modifications.
3. It can reduce global warming gas emissions‟
4. It can reduce tail pipe emissions, including air toxics, biodiesel is an oxygenated fuel.
5. It is nontoxic, biodegradable and suitable for sensitive environments
6. The higher flash point makes the storage safer
Demerits of biodiesel:
1. Slight decrease in fuel economy on energy basis.

2. Density, viscosity is more than diesel fuel.
3. More expensive due to less production of vegetable oil.
4. Long term operations and storage of respective biodiesel should be checked.
5. NOX and PM emissions to serious level.
Diesel engine is the most fuel efficient combustion engine among the available ones and
transport sector mainly uses diesel fuel due to its better fuel economy and more effective
power. Several countries such as USA, Germany, France, Italy, Brazil and Indonesia are
using biodiesel blended with diesel. Malaysia normally uses palm oil biodiesel as an
alternative to diesel in their country. The rapeseed and soybean biodiesels are generally used
in USA and Europe. In a country like India, biodiesel can also be used as alternative
automotive fuel. India has huge potential for biodiesel, but it is not yet explored properly to
replace at least some percentage of mineral diesels with biodiesel. [11]
1.3 Scope of the Work
Soybean oil is so far the leading feedstock for production of biodiesel in U.S. Sunflower,
canola, palm, cotton seed are the major biodiesel production sources in Brazil. India,
although produces edible oils, is not self-sufficient even to fulfil its domestic requirements.
Considering this issue, edible oils cannot be utilized for production of biodiesel in India.
Thus, the raw materials which are presently intended for biodiesel production in India are
non-edible vegetable oils like Jatropha curcas (Ratanjyot), Pongamia glabra (Karanja) ,
Hevea brancilis (Rubber) and Madhuca indica (Mahua). These are commonly found in the
forests of India. In addition to above species, identification of new feedstocks for biodiesel
production have been carried out with promising result. [12]
Indian National Biofuel Policy not permits the production of biodiesel from edible oil as done
in America and European Countries, only non-edible oil seeds are used for production of
biodiesel. The Policy aims at mainstreaming of biofuels and, therefore, envisions a central
role for it in the energy and transportation sectors of the country in coming decades. The
Policy will bring about accelerated development and promotion of the cultivation, production
and use of biofuels to increasingly substitute petrol and diesel for transport and be used in
stationary and other applications, while contributing to energy security, climate change
mitigation, apart from creating new employment opportunities and leading to
environmentally sustainable development. [13]
The Goal of the Policy is to ensure that a minimum level of biofuels become readily available
in the market to meet the demand at any given time. An indicative target of 20% blending of
bio-fuels, both for bio-diesel and bio-ethanol, by 2017 is proposed. The focus for
development of bio-fuels in India will be to utilize waste and degraded forest and non-forest
lands only for cultivation of shrubs and trees bearing non-edible oil seeds for production of
bio-diesel. [13]
The scope of this work is to utilize Soapnut (Sapindus mukorossi), which is available over the
India as a source of feedstock for biodiesel. Compare Physiochemical properties of Soapnut
biodiesel with ASTM standards for biodiesel. Study of oil extraction from Soapnut seeds
using Soxhelet extraction technique and biodiesel production by using transesterification
process. Assess its feasibility as a potential feedstock for biodiesel.
1.4 Aim and Objectives of the Present Study
The main aim of the study was to optimize the oil extraction and transesterification process
and to study the performance of diesel engine using SOME blends. In order to achieve the
aim, following objectives were decided for the project:
 To study oil extraction of Soapnut seeds using Soxhelet Apparatus.

 To study biodiesel production process through transesterification of Soapnut oil.
 To check properties of biodiesel and blends.
 To study effect of different parameters such as seeds size, reaction temperature, reaction
time and volume of solvent on oil yield.
 To study effect of solvent on the oil yield.
 To study effect of different parameters such as oil to methanol ratio, catalyst type, catalyst
concentration and reaction temperature on SOME yield when homogeneous catalyst was
used for transesterification.
 To study effect of different parameters such as oil to methanol ratio, Stirrer speed, catalyst
concentration and reaction temperature on SOME yield when heterogeneous catalyst was
used for transesterification.
 To study the effect of type of catalyst (Homogeneous and Heterogeneous catalyst) on
SOME yield.
Evaluate performance of CI engine fuelled with Soapnut oil methyl esters and its blends with
diesel.
1.5 Report Layout
Layout of chapters in the report is as follows. The report is framed into six chapters.
1. Chapter 1 introduces Indian and international petroleum scenario, biodiesel an
alternative fuel to diesel, background of CI engines.
2. Chapter 2 describes literature review in regard with various biodiesel feedstock‟s,
various oil extraction techniques, different biodiesel production techniques, review on
oil extraction and transesterification process, performance characteristics of biodiesel.
3. Chapter 3 describes the laboratory scale oil extraction setup, biodiesel preparation
set-up and preparation of biodiesel from Soapnut raw oil.
4. Chapter 4 includes fuel used for test, design of experimentation by taguchi method,
optimization of oil extraction and transesterification process and SOME diesel blends
at optimized engine parameters.
5. Chapter 5 illustrates results of oil extraction, transesterification process and
performance of single cylinder diesel engine using Soapnut oil methyl ester for
different blends.
6. Chapter 6 describes conclusion in regard with oil extraction, transesterification
process and performance of diesel engine using Soapnut oil methyl ester and diesel
blends.
Chapter 2
Literature Review
2.1 Introduction
Biodiesel is a liquid fuel similar to petroleum diesel in combustion properties, but essentially
free of sulphur, making it a cleaner burning fuel than petroleum diesel. Biodiesel is derived
from renewable energy sources, such as vegetable oils and animal fats. It has similar physical
and chemical properties with petro-diesel fuel. However, biodiesel properties can sometimes
be superior to that of petro-diesel fuel because the former has higher flash point, ultra-low
sulphur concentration, better lubricating efficiency, and better cetane number. The standards
for biodiesel and petroleum based diesel are provided in Table 1 for the comparison. [4]
Table 2.1 Comparison of the standards for diesel and biodiesel based on American
Society for Testing and Materials (ASTM). [10]
Property Diesel Biodiesel
Standards ASTM D975 ASTM D6751
Composition Hydrocarbon Fatty acid methyl esters
Specific gravity (g/ml) 0.85 0.88
Flash point (K) 333–353 373–443
Cloud point (K) 258–278 270–285
Pour point (K) 243–258 258–289
Water (vol%) 0.05 0.05
Carbon (wt%) 87 77
Hydrogen (wt%) 13 12
Oxygen (wt%) 0 11
Sulphur (wt%) 0.05 0.05
Cetane number 40–55 48–60
2.2 Biodiesel Feedstocks
Diesel engine is the most fuel efficient combustion engine among the available ones and the
transport sector mainly uses diesel fuel due to its better fuel economy and more effective
power. Several countries such as USA, Germany, France, Italy, Brazil, and Indonesia are
using biodiesel blended with diesel. Malaysia normally uses palm biodiesel as an alternative
to diesel in their country despite the use of palm oil as edible oil also. The soybean and the
rapeseed biodiesels are generally used in USA and Europe respectively. In a country like
India, biodiesel also can be used as alternative automotive fuel and also in other sectors as CI
engine fuels. Biodiesel is a fastest growing alternative fuel. India has huge potential for
biodiesel, but it is not yet explored properly to replace at least some percentage of mineral
diesels with biodiesel. [11]
A considerable amount of research has been conducted on alternative feedstocks for biodiesel
production all over the world. However, selecting the cheapest feedstock is the vital issue to
ensure low production cost of biodiesel. As much as possible, the biodiesel feedstock should
fulfil two requirements for the production of biodiesel; these are: low production and large
production scale. The availability of feedstock for biodiesel production depends on the
regional climate, geographical locations, local soil conditions, agricultural practices of any
country. The developing countries have focussed attention on nonedible oil due to low cost.
India has promoted non edible seeds like mahua, karanja, jatropha etc. for biodiesel
production. [10]
In general biodiesel fuel can be categorized into into four groups: (a) edible vegetable oil, (b)
Non edible vegetable oil (c) waste or recycled oil (d) animal fats. Among those, non-edible
vegetable oils, waste or recycled oils, animal fats are regarded as second generation biodiesel
feedstocks. It is very important to consider some parameters when comparing different
feedstocks. Each feedstock should be evaluated based on the life cycle analysis. These
includes: (a) availability of land (b) cultivation practices (c) energy supply and balance (d)
Emission of greenhouse gases (e) injection of pesticides (f) soil erosion and fertility (g)
contribution to biodiversity value losses (h) logistic cost (i) direct economic value of the
feedstock considering the co-products (j) creation of maintenance of employment (k) water
requirements and water availability (l) effects of feedstock on air quality. [10]
Table 2.2 Feedstock available for biodiesel production [10]
Edible oil Non edible oil Animal oil Other oil
Soybeans Jatropha Curcas Lard Bacteria

(Ratanjot)
Groundnut Calophyllum Tallow Fungi

Inophyllum (Surangi)
Oat Madhuca Indica Poultry Fat Algea

(Mahua)
Wheat Pongamia Glabra Fish oil Micro Algea

(Koroch )
Rice Pongamia Pinnata Tarpenes

(karanja)
Sorghum Hevea Brasiliensis Latexes

(Rubber seed)
Rapeseed Azadirachta Indica Cooking Oil

(Neem)
Canola Nicotania Tabaccum

(Tobacco)
Sunflower Ricinus Communis L

(Castor)
Barley Simmondsia Chinensis

(Jojoba)
Coconut Cerbera Odallum (Sea

Mango)
Cotton Seeds Sapindus Mukorossi

(Soapnut)
Palm seed
Rice Bran
Table 2.3 Estimated oil content yields of various non-edible oil vegetable resources [11]
Species Oil fraction (%) Kg oil/ha
Castor 45–50 1188
Jatropha 50–60 1590
Kusum 55-70 -----
Mahua 35–40 -----
Linseed 35–45 402
Neem 20–30 2670
Pongamia (Karanja) 30–40 900-9000
Simarouba Glauca 50–65 2.0-2.5
Sapindus Mukorossi 50-52 ------
2.3 Oil Extraction Techniques
There are six methods that have been identified for the extraction of the oil: (i) mechanical
extraction, (ii) solvent extraction and (iii) enzymatic extraction (iv) accelerated solvent
extraction (v) Supercritical fluid extraction (vi) Microwave assisted extraction. Mechanical
pressing and solvent extraction are the most commonly used methods for commercial oil
extraction. Before the oil extraction takes place, seeds have to be dried. Seed can be either
dried in the oven (105˚ C) (3weeks).Mechanical expellers or presses can be fed with either
whole seeds or kernels or a mix of both, but common practice is to use whole seeds.
However, for chemical extraction only kernels are used as feed. [10]
2.3.1 Mechanical extraction
The technique of oil extraction using mechanical presses is the most conventional practice. In
this type, either a manual ram press or an engine driven screw press can be used. It has been
found that, engine driven screw press can extract 68–80% of the available oil while the ram
presses only achieved 60–65%. However, it must be noted that oil extracted by mechanical
presses needs further treatment of filtering process and degumming. It has been found that,
pre-treatment of the seeds, such as cooking can increase the oil yield of screw pressing up to
89% after single pass and 91% after dual pass. [10]
Fig 2.1 Manual and Automatic oil expeller [48]
2.3.2 Chemical or solvent extraction
Solvent extraction is the process in which constituent is removed from a solid by means of a
liquid solvent. It is also called leaching. The chemical extraction using n-hexane method
results in the highest oil yield which makes it the most common method. Although the oil
extraction technique using the mechanical screw press was obtained at a low cost but this is
ineffective due to relatively lower oil yields. On the contrary, the chemical oil extraction
technique was found to be very effective because of high oil yield and for its consistent
performance. It has been observed that this method consumes much more time compared to
other techniques .In addition, it has been also found that the n-hexane solvent extraction has
a negative environmental impact because of the waste water generation, higher specific
energy consumption and higher emissions of volatile organic compounds and human health
impacts (working with hazardous and inflammable chemicals). [10]
2.3.2.1 Soxhelet extraction
A Soxhelet extraction is used when the desired compound has limited solubility in a solvent
and the impurity is insoluble in that solvent. Soxhelet extractor is a piece of laboratory
apparatus used for extraction of lipid from solid. [14]
Fig 2.2 Schematic representation of a Soxhelet extractor [14]
The solvent is heated to reflux. The solvent vapour travels up a distillation arm, and floods
into the chamber housing the thimble of solid. The condenser ensures that any solvent vapour
cools, and drips back down into the chamber housing the solid material. The chamber
containing the solid material slowly fills with warm solvent. Some of the desired compound
dissolves in the warm solvent. When the Soxhelet chamber is almost full, the chamber is
emptied by the siphon. The solvent is returned to the distillation flask. The thimble ensures
that the rapid motion of the solvent does not transport any solid matter to the still pot. This
cycle may be allowed to repeat many times, over hours or days. After extraction the solvent is
removed, typically by means of a rotary evaporator, yielding the extracted compound. The
non-soluble portion of the extracted solid remains in the thimble, and is usually discarded.
[14]
2.3.3 Enzymatic extraction
Aqueous enzymatic oil extraction (AEOE) method is a promising technique for extraction of
oil from plant materials. The main advantages in this process are: it is environmental-
friendly and does not produce volatile organic compounds. Appropriate enzymes are used to
extract the oil from crushed seeds. However, the main disadvantage in this method is, it takes
very long time to complete the process. [11]
Fig 2.3 Process of Enzymatic extraction [49]
2.3.4 Supercritical fluid extraction
Supercritical fluid extraction (SFE) technique has been developed since the 1980s to avoid
the use of organic solvents and to increase the speed of extraction. SFE using CO2 has
numerous advantages over the solvent extraction. However, the main limitation of the SFE is
the high cost at production scale, not only due to the use of high pressure equipment but also
because of the raw material should be freeze- dried to reduce its moisture to values below
20%. [10]
Fig 2.4 Supercritical fluid extraction [50]
2.3.5 Microwave assisted extraction
Microwave-assisted extraction (MAE) also called microwave extraction, is a new extraction

technique, which combines microwave and traditional solvent extraction. MAE has been
recognized as a technique with several advantages over other, such as reduction of costs,
shorter time, less solvent, higher extraction rate and better products with lower cost reduce
energy consumption and CO2 emissions. Therefore, MAE extraction is an interesting
alternative to conventional liquid solvent extraction methods, especially in the case of plant
material. [15]
It has been found that the MAE method needs a few minutes compared to SFE and the
apparatus of MAE extraction is simpler and cheaper, and can be used with a variety of
materials with less limit of the polarity of extractants. Therefore, MAE extraction is an
interesting alternative to conventional liquid solvent extraction methods, especially in the
case of plant material. [15]
Fig 2.5 Microwave assisted extraction [51]
2.4 Preparation of Biodiesel
A lot of efforts have been made to develop and improve vegetable oil derivatives in order to
approximate the properties and performance of hydrocarbon-based diesel fuel. It has been
remarked that high viscosity, low volatility and polyunsaturated characters are the main
barriers that prevent the use of direct vegetable oils in conventional diesel engines. However,
direct use of vegetable oils has been deemed unsatisfactory due to the presence of high
viscosity, FFA content and the presence of carbon deposits. In addition, refinement is
necessary to turn those vegetable oils into quality fuel. In order to overcome those problems,
many technologies and methods have been employed nowadays to produce biodiesel from
various non-edible feedstock‟s as well as waste materials and animal fats. These include
pyrolysis, dilution, micro-emulsification and transesterification. [10]
Generally, methanol is used to produce biodiesel because of its availability and lower
reaction time, and the final product (biodiesel) is called as methyl ester of the raw oil used.
Sometimes, ethyl alcohol is also used for the production of biodiesel, and it is called as the
ethyl esters of the corresponding oil. Ideally, transesterification is potentially a less expensive
way of transforming the large, branched molecular structure of the bio-oils into smaller,
straight chain molecules of the type required in regular diesel combustion engines. The
efficiency of transesterification is greater than other biodiesel conversion process and it is
about 90-99%. [11]
Fig 2.6 Process flow chart of nonedible oil seed to produce biodiesel [10]
2.4.1 Pyrolysis
Pyrolysis is the method of thermal conversion of the organic matters without the presence of
oxygen and in the presence of a catalyst. The available paralysed materials are vegetable oils,
animal fats, bio-waste, natural fatty acids or methyl esters of fatty acids. Pyrolysis of the
vegetable oil can produce a product with high cetane number, low viscosity, low water
content and smaller proportions of sediments, and reasonable amounts of sulphur and copper
corrosion values. However, unacceptable amounts of ash contents, carbon residues and pour
points can be produced. The advantages of this process are simple, waste less, pollution-free
as well as cost effective when compared with other cracking processes. [15]
2.4.2 Dilution
Vegetable oils can be used as an alternative diesel fuel with dilution modification technique.
The direct use of vegetable oils in diesel engines creates problems and has many inherent
failings. Mainly, vegetable oils are blended with diesel fuel in order to reduce the viscosity
and to improve the performance of the engine. This method does not require any chemical
process. It has been observed that blending of 20–25% vegetable oil with diesel fuel has been
considered to give good results for diesel engine. [10]
2.4.3 Micro-emulsification
Micro-emulsification is the formation of micro-emulsions(co-solvency) which can be made

of vegetable oils with an ester and dispersant, or of vegetable oils, and immiscible liquids
such as methanol, ethanol, butanol, hexanol and ionic or non-ionic amphiphiles, and is a
potential solution for solving the problem of high viscosity vegetable oils. Furthermore,
micro- emulsification technique has been taken into account as a reliable approach to solve
the problem of the high viscosity of vegetable oils. [11]
2.4.4 Transesterification
Transesterification is presently one of the most attractive and widely accepted technologies
for biodiesel production. It is regarded as the best technique and the most promising solution
to the high viscosity problem among other approaches due to its low cost and simplicity.
Moreover, this technique has been identified as a widely available technique for
industrialized biodiesel production due to its high conversion efficiency and low cost. It has
been realized that the conventional method for biodiesel production involves the use of
homogeneous base catalysts under mild heating (50˚C–60˚C), albeit there are many other
methodologies available. The process consists of a number of consecutive, reversible
reactions. It has many advantages than the other processes e.g., it is achieved under normal
conditions and it returns good yield of better quality biodiesel. However, there are many
companies around the world that use this technology commercially because of its relatively
lower energy consumption, high conversion efficiency and cost effective reactants and
catalysts. [15]
Fig 2.7 Basic transesterification technology [10]
In transesterification process, alcohol is reacted with vegetable oil in the presence of

appropriate catalyst. Generally, ethyl or methyl alcohol is used to produce ethyl/methyl
esters. After completing the reaction, two distinct layers of liquids i.e., ethyl/ methyl ester and
glycerin appeared and are separated as shown in Fig. The vegetable oil is reacted with
methanol already mixed with catalyst and the results produced are crude biodiesel and crude
glycerin. The glycerin is refined and disposed of for further use. The crude biodiesel is also
refined and alcohol is separated from it which is reused in the cycle. [11]
Fig 2.8 Transesterification reaction of triglycerides [11]
The technology of biodiesel production includes transesterification of oils (triglycerides) with

alcohol which gives biodiesel FAME (fatty acid methyl esters) as the main product and
glycerol as the by- product. The basic transesterification reaction is illustrated in Fig.3. In this
reaction, the first step is the conversion of triglycerides to di-glycerides, which is followed by
the conversion of di-glycerides to mono-glycerides and then of mono-glyceride to glycerol,
yielding one methyl ester molecule from each glyceride at each step. There are many factors
which affect the transesterification process such as, mixing intensity, the nature of the
feedstock, reaction temperature, reaction time, reaction pressure, alcohol/oil molar ratio, type
and concentration of catalyst, free fatty acids, moisture and water content, rate and mode of
stirring, effect of using organic co-solvents, specific gravity as well as purity of reactants.
[10]
The alcohols used in the transesterification process are generally short chain alcohols such as,
methanol, ethanol, propanol, and butanol. However, methanol and ethanol are generally used
commercially among the other alcohols because of their low cost and physical and chemical
advantages. Generally, the reaction temperature near the boiling point of the alcohol is
recommended. Albeit, the reaction may be occurs at room temperature. The reactions also
take place at low temperature (338K) and at modest pressures (2atm, 1atm=101.325kPa). The
produced biodiesel is further treated by washing and evaporation to remove any remaining
methanol. The input materials such as, oil (87%), alcohol (9%), and catalyst (1%) are used
for the production of biodiesel (86%) which is the main output. It was reported that a FFA
value of lower than 3% is required for completing their action and the other materials should
be substantially anhydrous. Ideally, the FFA value should be kept below 1% to obtain
biodiesel. The presence of water gives rise to hydrolysis of some of the produced ester with
consequent soap formation whereas, the soap formation reduces catalyst efficiency, causes an
increase in viscosity, leads to gel formation and makes the separation of glycerol difficult.
[15]
Generally, there are two mostly used methods for transesterification reaction, such as,
catalytic and non-catalytic transesterification. Catalytic transesterification method includes:
base-catalysis, acid catalysis as well as enzyme catalysis. On the other hand, non-catalytic
transesterification process includes: supercritical alcohol and BIOX-co solvent. Besides,
microwave assisted and ultrasound assisted transesterification processes are also considered
as an alternative technique for biodiesel production. [10]
2.4.4.1 Catalytic transesterification methods
The transesterification reaction can be catalysed by alkalis, acids and enzymes. Vegetable oils
are transesterified by reacting them with an alcohol and a catalyst which is an important
industrial method used in biodiesel synthesis. The methanolysis reaction has been thoroughly
studied and established using acids or alkalis, such as sulphuric acid or sodium hydroxide as
catalyst. However, it has been found that these catalytic systems are less active or completely
inactive for long chain alcohols. In catalytic method, the suitable selection of the catalyst is
an important factor to lower the biodiesel production cost. Generally, sodium or potassium
hydroxide or sodium or potassium methoxide is used as a catalyst as they are relatively cheap
and quite active for this reaction. [10]
Transesterification reaction can be catalysed by both homogeneous (alkalis and acids) and
heterogeneous catalysts. In case of homogeneous catalysts, greater performance is obtained
toward transesterification to yield biodiesel when the free fatty acid content is >1%. On the
contrary, heterogeneous catalysts are significant for the transesterification reaction of
vegetable oils while the free fatty acid content is <1% and can be separated more easily from
reaction products. There are some disadvantages in homogeneous catalysts such as,
expensive separation of the homogeneous catalyst from the reaction mixture, production of
large amount of waste water during separation and cleaning up of catalyst and the products,
formation of unwanted by-product (i.e. soap) by reaction of the FFA. [15]
The drawbacks encountered in the homogeneous catalysts can be overcome by using the
heterogeneous catalysts. The undesired saponification reactions could be avoided and the
transesterification of vegetable oils or animal fats with high contents of FFAs could be
facilitated by using these catalysts. These catalysts are environmentally benign, less corrosive
nature, could be operated in continuous processes and they can be reused and regenerate. [11]
On the other hand, the enzymatic reactions are insensitive to FFA and water content in oil.
Hence, enzymatic reactions can be used in transesterification of used cooking oil. In enzyme-
catalysed transesterification method that using lipase as catalyst do not produce side reactions
but the lipases costs are very high for industrial scale production.
2.4.4.1.1 Alkali catalysed transesterification
The transesterification process is catalysed by alkaline metal alkoxides, hydroxides, as well

as sodium or potassium carbonates. However, it has been observed that the sodium
methoxide is the most widely used biodiesel catalyst and over 60% of industrial plants use
this catalyst. Alkaline catalysts require short reaction time and relatively low temperature and
little or no darkening of colour of the oil. The alkali-catalysed transesterification of vegetable
oils goes on faster than the acid-catalysed reaction and the mechanism of transesterification is
shown in Fig. 2.9. [16]
Fig 2.9 Mechanism of alkali catalysed transesterification of vegetable oil [10]
In the alkali catalytic methanol transesterification method, the catalyst (KOH or NaOH) is
dissolved into methanol by vigorous stirring in a small reactor. The oil is then transferred into
the biodiesel reactor and the catalyst/alcohol mixture is pumped into the oil. The final
mixture is stirred vigorously for 2 h at 340 K in ambient pressure. A successful
transesterification reaction produces two liquid phases‟ ester and crude glycerol. In general,
alkali-catalyzed transesterification processes are completed at low temperatures and pressures
(333–338 K and 1.4– 4.2 bar) with low catalyst concentrations (0.5–2 wt %). Alkaline metal
alkoxides (as CH3ONa for the methanolysis) are the most active catalysts as they give very
high yields (>98%) in short reaction times (30min) even if they are applied at low molar
concentrations (0.5 mol %). [11]
2.4.4.1.2 Acid catalysed transesterification

The main acid-catalysed transesterification methods for biodiesel production are methanolic
sulphuric acid, ferric sulphate, sulfonic acid, methanolic hydrogen chloride, and methanolic
boron tri-fluoride. The catalysts are dissolved into methanol by vigorous stirring in a small
reactor whereas the oil is transferred into the biodiesel reactor and then the catalyst/ alcohol
mixture is pumped into the oil. Currently, the mostly used catalysts in biodiesel production
are the organic acids, such as the derivatives of toluene sulfonic acid and, more often, mineral
acids such as sulphuric acids, hydrochloric acid. There are some advantages of acid-catalysed
transesterification process: it directly produces biodiesel from low-cost lipid feedstock‟s,
such as used cooking oil and greases, which commonly have FFAs levels of 46% and
insensitive to the FFAs content in the feedstock. [10]
Although the transesterification process using acid-catalysts is much slower than that
obtained from the alkali-catalysis which is typically 4000 times but due to the presence of
high contents of water and FFAs in the vegetable oil, acid-catalysed transesterification
method is considered to provide better results. The acid-catalysed reaction commonly occurs
at temperatures above 373K and requires reaction times of 3–48h, except when reactions
were conducted under high temperature and pressure. The mechanism of acid-catalysed
transesterification of vegetable oil (for a mono-glyceride) is presented in Fig 2.10.
Afterwards, it can be extended to di and triglycerides. The protonation of carbonyl group of
the ester leads to the carbonation, which after a nucleophilic attack of the alcohol produces a
tetrahedral intermediate. [8]
Fig 2.10 Mechanism of acid catalysed transesterification [11]
2.4.4.1.3 Enzyme catalysed transesterification
Enzymatic transesterification using a lipase catalyst looks attractive because of less energy
intensive; they do not promote side reactions, easy product separation, minimal waste water
treatment needed easy glycerol recovery and is more environmentally friendly. Enzyme
catalysed reactions have the advantages of reacting at room temperature without producing
consumed catalysts. However, enzyme-catalysed system requires a much longer reaction time
than the alkali and acid catalysed systems. [10]
2.4.4.2 Non catalytic transesterification methods
As in catalytic reaction process, the production of biodiesel through the conventional

transesterification system renders the process complicated, thus it gives areas on to
investigate the production of biodiesel from triglycerides via non-catalytic reactions. [10]
2.4.4.2.1 Supercritical alcohol transesterification
The transesterification of triglycerides by supercritical methanol, ethanol, propanol and

butanol has been proven to be the most promising option. Supercritical methanol
transesterification is the process, in which solvent is subjected to temperature and pressure
above its critical point. The problems associated with the two-phase nature of normal
methanol/oil mixtures can be solved by using supercritical methanol technique by forming a
single phase as a result of the lower value of the dielectric constant of methanol. Furthermore,
the process at higher temperature and pressure conditions provides improved phase solubility,
decreases mass transfer limitations, provides higher reaction rates, makes easier separation,
has a simpler purification steps, has a lower reaction time, is more environmental friendly, as
well as requires lower energy consumption. Supercritical methanol transesterification is the
process, in which solvent is subjected to temperature and pressure above its critical point.
However, the reaction is fast and conversion raises 50–95% for the first 10min but it requires
temperatures and pressures of 525–675K and 35–60 MPa, respectively. In addition, a novel
transesterification process of vegetable oils with non- catalytic supercritical methanol has
been developed to provide a new way of producing biodiesel. [15]
2.4.4.2.2 Microwave assisted transesterification
Microwave assisted transesterification is another alternative energy tool that can be used for
the production of biodiesel. It has been observed that microwave transfer energy has a
tendency to oscillate polar ends of molecules or ions continuously and the result is generated
heat energy due to the collision and friction between the moving molecules. Therefore, heat is
directly stored into the reaction media and results in rapid temperature increase throughout
the sample. [15]
2.4.4.2.3 Ultrasound assisted transesterification
Ultrasonic irradiation is known to be a useful tool for strengthening the mass transfer of
liquid-liquid heterogeneous systems. Under ultrasonic irradiation, the transesterification can
be carried out at a low temperature and smaller amounts of catalyst as well as methanol are
required. In addition, ultrasonication provides the mechanical energy for mixing and the
required activation energy for initiating the transesterification reaction. Besides,
ultrasonication increases the chemical reaction speed and yield of the transesterification of
vegetable oils/fats. However, ultrasonic technology has proven to be an effective tool in
enhancing the reaction rates in a biphasic (liquid–liquid) heterogeneous reaction system. It
was reported that the use of ultrasonication process yields highest methyl ester conversion of
95% (1.0% (w/w) with NaOH, time 10 min and room temperature). [11]
2.5 Reviews of Oil Extraction and Transesterification Process:
Jahirul et al. and bhuiya et al. used a mini screw press to extract to extract oil from beauty
leaf kernels (C. iniphyllum). It has been observed that the ram press can extract only 60-65%
while an engine driven screw press can extract 68-80% of the available oil this higher range
is due to the fact that seeds can be subjected to different number of extractions through the
expeller [17]. Mahanta P et al. and shrivastava A et. al reveals that the pretreatment of seeds
by cooking process can increase the yield of screw pressing upto 89% after single pass and
90% after dual pass. [18]
Devan et al. and Mahalaksmi et al. used one mechanical expeller to extract from sterculia
feotida L seeds. Yang et al. indicated mechanical expeller can be used to extract oil from
idesia polycarpa with high yield. Oil from dried and peeled Calophyllum inophyllum seed
can be extracted the crude jatropha oil using mechanical expeller. Foidl et al. used screw
press to extract oil from jatropha seeds. Mahanta et al. and srivastva et al. that one of the
problems associated with the nonedible seeds are that the mechanical presses are not efficient
for extraction of oils. Same mechanical press cannot be used for different type of seeds.
Therefore, several other methods have been proposed recently such as solvent extraction
techniques. [19]
Ashwath et al. and Jahirul et al. conducted the chemical oil extraction technique to extract
the oil from Australian native beauty leaf seeds (C. Inophyllum). According to Jahirul et al.
although the oil extraction the mechanical screw was obtained at low cost but this is
ineffective due to lower oil yields. On the contrary, the chemical oil extraction was found to
be very effective because for its high oil yield and consistent performance. It has been
observed that there are many factors affecting the rate of extraction such as particle size, the
type of liquid used for extraction. [20]
Mahanta et al. and Shrivastava et al. reported that the solvent extraction with n-hexane can be
used to extract from the seeds of Jatropha Curcas and Pongamia Pinnata and this would
produce about 41% and 95-99% of oil yield respectively. However it has been observed that
this method consumes much more time compared to other techiniques. In addition, it has
been also found that the n-hexane solvent has a negative environmental impact because of
waste water generation, higher specific energy consumption and higher emissions of volatile
organic compounds and human health impacts. Moreover, several other studies conducted by
kansedo et al. moser and Vaughn et al. and sarin et al. extracted the oil from cerbera odallum
(Sea mango), Coriander (Coriandrum sativum L), Moringa Oleifera and guizotia abyssinica L
using Soxhelet extractor with n-hexane as a solvent. [21]
Shah et al. used combination of combination of ultrasonication and enzymatic method to

extract oil from jatropha curcas seeds kernels using aqueous enzymatic oil extractions greatly
reduces problems such as waste water generation, specific energy consumption and higher
emissions of volatile organic compounds. [22]
Ma et al. studied the transesterification of beef tallow catalysed by NaOH in the presence of
free fatty acids and water. Without adding free fatty acids and water, the apparent yield of
beef tallow methyl esters (BTME) was highest. When 0.6% of FFA was added the apparent
yield of BTME reached lowest, less than 5%, with any level of water added. The products
were solid at room temperature similar to original beef tallow. When 0.9% of water is added
without the addition of FFA the apparent yield was about 17%. If the low qualities of beef
tallow or vegetable oil high FFA are used to make biodiesel fuel, they must be refined by
saponification using NaOH solution to remove free fatty acids. Conversely the acid catalysed
process was used for the esterification of free fatty acids. [23]
Turck et al. has investigated the negative influence of catalysed transesterification of

triglycerides containing substantial amount of free fatty acid. Free fatty reacts with the alkali
catalyst added for the reaction and gives rise to soap as a result of which one part of the
catalyst is neutralized, therefore no longer available for transesterification. These high FFA
content oils/fats are processed with an immiscible glycerol phase by means of monovalent
alcohol. The triglycerides are subjected to transesterification using base as catalyst to form
fatty acid alkyl esters, characterized in that after separation, the basic glycerol phase
produced during transesterification of triglycerides is used for processing oils/fats for
removal of free fatty acids. [24]
Enciner JM, Gonzalez JF, Rodriguez JJ, Tajedor A et al. reveals that the transesterification of
cynara oil with ethanol was studied at molar ratio between 3:1 and 15:1. The ester yield
increases as the molar ratio increases upto 12:1. The best results were for molar ratios 9:1 to
12:1. For molar ratios less than 6:1, the reaction was incomplete. For the molar of 15:1, the
separation of glycerine is difficult and the apparent yield of esters decreases because part of
glycerol remains in the biodiesel phase. Therefore molar ratio 9:1 is seems to be the most
appropriate. [25]
Maeda et al. and Thanh et al. produced biodiesel from vegetable oils assisted by ultrasound
which is a useful tool for strengthening the mass transfer of immiscible liquids. Ultrasonic
irradiation causes cavitation of bubbles near the phase boundary between the immiscible
liquid phases. The asymmetric collision of cavitation bubbles disrupts the phase and causes
emulsification instantly. Microjets are formed by impinging one liquid to another, lead to
intensive mixing of the system near phase boundary and enhance the reaction. Moreover,
Wen et al. fabricated a new reaction vessel – zigzag micro channel reactors in recent years
and found that energy consumption for biodiesel synthesis can be achieved by using this
reactor. [26]
Leung and Guo et al. studied the effect of operating conditions in product yield and pointed
the oil before mixing can increase the reaction rate and hence shorten the reaction time.
During this step in order to speed up the reaction, mixing brings the oil, the catalyst, and the
alcohol into intimate contact while the temperature is kept just below the boiling point of
alcohol. Normally the reaction pressure is close to the atmospheric to prevent the loss of
alcohol, and excess alcohol is used to ensure total conversion of oil to its esters. As
previously mentioned if the free fatty acid level or water level is too high, it may cause
problems downstream with the saponification and separation of glycerol by-product.
Therefore of water and free fatty acids in the feedstock oil should be monitored during the
reaction. [27]
Yousef Haik, Mohammad Y.E Selim and Tahir Abdulrehman et al. reveals that the algal oil
has been converted to fatty acid methyl esters by transesterification process. The extracted
algal oil is preheated to 60˚C and then added to the mixture of sodium hydroxide and
methanol. It was then mixed with a blender for an hour. The amount of methanol used was
20% of the amount of algal oil used. 3.5 gm of sodium hydroxide was used for a litre of oil.
After the transesterification the mixture is collected and kept for 8 hour or more to allow the
glycerine to settle at the bottom and fatty acid methyl will form at the top. The biodiesel is
separated and with water 4-5 times and was or dried in an air to evaporate the remaining
water. [28]
S Jindal, B.P Nandwana, N.S Rathore, V. Vashishta et al. reveals that jatropha methyl ester
was prepared from jatropha vegetable oil, which is gaining popularity due to its properties
and has been accepted and recommended by the national biodiesel board of India as a source
of alternative fuel for blending in the commercial diesel. The vegetable oil extracted from
fresh seeds was sourced from local oil mill and was transesterified by alkali catalysed
esterification using methanol (20%) and KOH (1%) as catalyst. Oil was heated to 60˚C and
the mixture of methanol and KOH in desired proportion was added. The mixture was agitated
for an hour and then left for settling for 24 hours. [29]
Joshua Folaranmi et al. has confirmed that Jatropha oil may be used as resource to obtain
biodiesel. The experimental results show that alkaline catalysed transesterification is a
promising area of research for the production in a large scale. Materials for use in the
production of biodiesel are readily available without the need of special equipment or scarce
chemicals. Used oil from the restaurant can be used in the production of biodiesel. On small
scale production, the cost of production is low, but if mass production and accuracy is the
goal, the cost is high. Glycerine which is the by-product of the chemical reaction can be sold
to the pharmaceutical companies, since it is used to produce valuables such as creams and
toothpaste. Effects of different parameters such as temperature, time, reactant ratio, and
catalyst concentration on the biodiesel yields were analysed. The best combination of the
methanol to oil ratio, 1% of KOH, 60˚C reaction temperature and 60 minutes of reaction time.
This optimum condition yielded 90% of biodiesel. [30]
Payal Choudhary, Brajesh Kumar, Surendra Kumar, V.K. Gupta reveals transesterification of
castor oil with methanol and sulphuric acid catalyst has been carried out in a lab reactor fo
capacity 500 ml at various operating conditions (reaction temperature = 35-65˚C, pressure = 1
atm, methanol to oil ratio 6:1 and 600 rpm). The effect of temperature is considered, followed
by the determination of the kinetics of the production of biodiesel. Experimental results have
been analysed with three types of kinetics namely the first order irreversible reaction, second
order reversible reaction and reversible reaction. For each the schemes, the activation energy
and arehenius constants were determined. The experimental data fits very well to second
order reversible reaction kinetics. Properties of fatty acid methyl esters produced from castor
oil have been experimentally determined. [31]
2.5.1 Performance Characteristics of Biodiesel
Gumus observed a reduction in brake thermal efficiency of a four stroke single cylinder
diesel engine using hazelnut kernel oil methyl ester (biodiesel) as fuel. This type of behaviour
was attributed to the lower heating value and higher viscosity of biodiesel than that of diesel,
which resulted fuel consumption and led to a decrease in brake thermal efficiency. He also
reported from his experimental investigation that with the advancement of injection timing
and increase in compression ratio and injection pressure, brake thermal efficiency increased
as the fuel consumption decreased under the above mentioned conditions. [32] (Ambarish
data)
Avinash Kumar Agarwal, Atul Dhar, Jai Gopal Gupta, Woong Il Kim, Kibong Choi, Chang
Sik Lee Sungwook Park investigation, effect of 10%, 20% and 50% Karanja biodiesel blends
on injection rate, atomization, engine performance, emissions and combustion characteristics
of common rail direct injection (CRDI) type fuel injection system were evaluated in a single
cylinder research engine at 300, 500, 750 and 1000 bar fuel injection pressures at different
start of injection timings and constant engine speed of 1500 rpm. In single injection mode,
BSFC for KOME50 and KOME20 were higher than mineral diesel . BSFC of KOME10 was
almost similar to mineral diesel due to insignificant difference in physical properties of the
test fuels. Reduction in calorific value of test fuel with increasing concentration of Karanja
biodiesel was responsible for increase in BSFC for KOME50 and KOME20 blends. Thermal
efficiency of lower biodiesel blends (KOME10 and KOME20) was higher than KOME50.
[33]
Atul Dhar, Roblet Kevin, Avinash Kumar Agarwa conducted experiments at 200 bar fuel
injection pressure to compare the performance of B05, B10, B20, B50 biodiesel blends and
B100 with mineral diesel BSFC was observed to have increased with increasing proportion of
biodiesel in the fuel. Brake thermal efficiency of B100 was highest among all the test fuels.
All blends have higher thermal efficiency than mineral diesel. BSFC for the biodiesel and its
blend increases due to lower calorific value of biodiesel in comparison with mineral diesel.
Presence of oxygen in the biodiesel molecules improve the combustion efficiency of
biodiesel hence its brake thermal efficiency increases with respect to mineral diesel. [34]
A.M. Liaquat, H.H. Masjuki, M.A. Kalam, I.M. Rizwanul Fattah, M.A. Hazrat, M. Varman,
M. Mofijur, M. Shahabuddin investigates the engine performance parameters for direct
injection diesel engine using coconut biodiesel blends without any engine modifications. A
total of three fuel samples, such as DF (100% diesel fuel), CB5 (5% coconut biodiesel and
95% DF), and CB15 (15% CB and 85% DF) respectively are used. Engine performance test
has been carried out at 100% load, keeping throttle 100% wide open with variable speeds of
1500 to 2400 rpm at an interval of 100 rpm. As results of investigations, there has been a
decrease in torque and brake power, while increase in specific fuel consumption has been
observed for biodiesel blended fuels over the entire speed range compared to net diesel fuel.
net diesel fuel shows some higher torque values than biodiesel blends due to the fact that
diesel fuel has higher heating value than biodiesel blends. The average torque reduction
compared to net diesel fuel is found as 0.69% for CB5 and 2.58% for CB15 respectively. The
engine brake power for biodiesel blends was found to be lower than obtained for net diesel
fuel. The lower brake power for CB5 and CB15 can be due to their respective lower heating
values. The average power reduction compared to diesel fuel over the entire speed range is
found as 0.66% for CB5 and 2.61% for CB10% respectively. [35]
For the biodiesel blends, heating value is found slightly higher than that for diesel fuel. This
may be attributed to the lower heating value and higher density of the blends. It is also known
that biodiesel contains oxygen content, which results in the lower heating value. Thus for the
same energy output from the engine, it requires larger mass fuel flow, which increases bsfc to
compensate the reduced chemical energy in the fuel. The average increase in bsfc compared
to diesel fuel is found as 0.53% for CB5 and 2.11% for CB15 respectively. [35]
Swarup Kumar Nayak, Bhabani Prasanna Pattanaik investigates about the production of
biodiesel from neat Mahua oil via base catalyzed transesterification and mixing of the
biodiesel with a suitable additive (Dimethyl carbonate) in varying volume proportions in
order to prepare a number of test fuels for engine application. The prepared test fuels are used
in single cylinder water cooled diesel engine at various load conditions to evaluate the
performance parameters of the engine. The results of investigation show increase in brake
power and brake thermal efficiency with load for all prepared test fuels. It is also noticed that
brake thermal efficiency increases with the percentage of additive in all the test fuels. The
brake specific fuel consumption decreases with increase in additive percentage. [36]
Exhaust gas temperature increases almost linearly with load for all test fuels and decreases
with increase in additive percentage. Diesel has highest brake thermal efficiency than that of
other test fuels which is because of its higher heat content, lower viscosity, lower density and
higher volatility in comparison to Mahua biodiesel. The BTE obtained at full load for diesel,
B100, B95, B90 and B85 are 30.09%, 26.63%, 28.01%, 29.74% and 29.97% respectively.
BSFC is highest for pure biodiesel and lowest for diesel because of high viscosity, density,
low volatility and low heat content of pure biodiesel when compared with that of diesel [28,
29]. However, increasing the additive percentage in biodiesel, BSFC decreases with respect
to load and shows close results to that of diesel. This may be due to improved combustion,
low viscosity, high volatility of the test fuels using additive .Different values of BSFC for
diesel, B100, B95, B90 and B85 are 0.387, 0.556, 0.503, 0.4993 and 0.4104 Kg /Kwh
respectively. [36]
Agarwal and Dhar used neat karanja oil and preheated karanja oil to run a four stroke diesel
engine. The decrease in efficiency with this straight vegetable oil was found to be even more.
It was also reported that when SVO was preheated, the efficiency increased but still remained
much lower than diesel fuel. The reductions in brake thermal efficiency were found to be
45% and 25% with non-preheated and preheated straight vegetable oils respectively. The
main reasons behind these reductions in thermal efficiency were reported to be poor volatility
and higher viscosity of both the above said fuels. [37]
Rakopoulos et al. tested a variety of vegetable oils blends of 10% and 20% respectively
including cotton seed oil in a standard, fully instrumented, four stroke, direct injection(DI),
Ricardo/Cussons „Hydra‟ Diesel engine located at the authors‟ laboratory. The authors found
that specific fuel consumption was a little higher than that for the corresponding diesel fuel in
both medium and high loads. The authors concluded that vegetable oil blends with normal
diesel fuel can be used safely and advantageously in small blending ratios with diesel fuel.
[38]
Mahanta et al. utilised pure karanja oil and its blends along with biodiesel of karanja and
tested in a 5-HP water cooled, direct injection, four stroke diesel engines. The SFC of B15
and B20 blends were marginally higher than diesel. The SFC increased with increase in
straight vegetable oil (SVO) content in the blend, though with B15 and B20, fuel
consumption decreased marginally when compared with SVO blends. In comparison to
diesel, the blends of methyl ester of karanja oil and diesel particularly B15 and B20 gave
higher brake thermal efficiency. However, SVO blends resulted in lower thermal efficiency
as compared to diesel. [39]
Jindal et al. evaluated the effects of engine parameters (compression ratio and injection
pressure) while working with jatropha methyl ester as fuel in single cylinder, water cooled, 4-
stroke, VCR (variable compression ratio) diesel engine connected to eddy current type
dynamometer. The results shows that increase in compression ratio associated with increase
in injection pressure improve the performance of the engine.
2.6 Soapnut (Sapindus Mukorossi)
The Soapnut is the fruit of the Soapnut tree, which is generally found in tropical and
subtropical climates in various parts of the world, including Asia, the Americas, and Europe.
Sapindus Mukorossi Gaertn., a member of the Sapindaceae family, is a deciduous tree widely
grown from Afghanistan in the west to China in the east, at altitudes ranging from 200 to
1500 m. The integration of Soapnut tree plantations along with community forestry in barren
lands is considered to have great potential for the mass production of soapnut seeds, which
are a potential non-edible oil feedstock for biodiesel production. [16]
 BOTANICAL NAME – Sapindus Mukorossi

 FAMILY – Sapindaceae
 COMMON NAMES – Soapnut, Reetha, Kekru, Aritha, Dodan.
 About the Plant
This tree flourishes in deep clayey loam soil and does best in areas experiencing nearly 150–
200 cm of annual rainfall. The seed is enclosed in a black, smooth and hard globose
endocarp. Soapnut contain saponins, a natural surfactant and have been used as detergent,
which is a good substitute for washing soap and is as such used in preparation of quality
shampoos, detergents, etc. Soapnut seeds contain 23% oil of which 92% is triglycerides . The
Soapnut trees have been used for multiple applications such as rural building construction, oil
and sugar presses, and agricultural implements. Sapindus Mukorossi has the leaves which are
alternate, 15-40 cm long, pinnate, with 14-30 leaflets and the terminal leaflet is often absent.
The flowers form in large panicles, each flower small, creamy white. The fruit is a small
leathery shinned drupe 1-2 cm in diameter, yellow repining blackish, containing one to three
seeds. [16, 41, 42]
 Distribution
Sapindus Mukorossi is native to northern India east to the Himalayas including Manipur. In
Maharashtra it is found in konkan areas and in Goa. Other species of this family are found in
different countries like China, southern Asia, India, Florida to Carolina, North America,
Hawaii, Mexico, United States, Caribban, island of Hawai, Pakistan, Leenh, American Samoa
etc. [16,42]
 Climate and Soil

Soapnut is the fruit of the Soapnut tree, which is generally found in tropical and sub-tropical
climate areas in various parts of the world, including Asia, the Americas, and Europe.
Fig 2.11 Soapnut seeds and kernels [42]
Table 2.4 Comparison of oil yields between common oilseed crops [10]
Non edible vegetable source Oil content Yield of various plant

oils
Seed (%) Kernel (%) ( kg oil/ha)
Sapindus Mukorossi (Soapnut) 35 % ----- -----
Azadirachta Indica (Neem) 20-30 % 25-45 % 2670
Calophyllum Inophyllum 65 % 22 % 4680

(Polanga)
Cerbera Odallam ( Sea Mango) 54 % 6.4 % -----
Pongamia Pinnata ( Karanja) 25-50 % 30-50 % 900-9000
Madhuca Indica (Mahua) 35-50 % 50 % -----
Nicotania Tabacum (Tobacco) 36-41 % 17 % 2825

Simondsia Chinensis (Jojoba) 45-55 % ----- 1528
Soapnut orchards are environmentally beneficial, as soapnut trees naturally grow in deep
clayey loam soil and flourish in areas with annual rainfall of 150-200 cm, where they prevent
potential soil erosion. [41]
Oil of soapnut seeds contain 92% triglycerides; the triglyceride fraction contains 30% oleo-
palmito-arachidin glyceride, 13.3% oleo diarachidin glyceride and 56.7% di-olein type
glycerides such as dioleo-palmitin, dioleo-stearin and dioleo-arachidin .
Table 2.5 Major fatty acid composition of Soapnut and popular seeds [15]
Feedstock
Fatty Acid Soapnut Canola Jatropa
Lauric Acid (C12:0) ----- ----- 0.31
Myristic Acid (C14:0) ---- 0.242 -----
Palmitic Acid (C16:0) 4.67 4.77 13.38
Palmitoleic Acid 0.37 0.363 0.88

(C16:1)
Stearic Acid (C18:0) 1.45 1.978 5.44
Oleic Acid (C18:1) 52.64 60.284 45.79
Linoleic Acid (C18:2) 4.73 20.029 32.27
Linolenic Acid 1.94 8.731 ----

(C18:3)
Arachidic Acid 7.02 0.582 -----
(C20:0)
Ecosenoic Acid 23.85 1.283 -----
(C20:1)
Behenic Acid (C22:0) 1.45 1.45 -----
Erucic Acid (C22:1) 1.09 1.09 -----
Lignoceric Acid 0.47 0.117 -----

(C24:1)
Others 0.32 1.621 1.93
Total 100 100 100

Sengupta et al evaluated the fatty acid composition of S. mukorossi seed oil by
spectrophotometry, urea complexation, and gas liquid chromatography (GLC). They found
percentages of individual acids to be: palmitic, 4.0; stearic, 0.2; arachidic, 4.4; oleic, 62.8;
linoleic, 4.6; linolenic, 1.6; and eicosenoic. The special characteristic of the S. mukorossi
seed oil is its content of 26.3% and 26.7% triolein and eicoseno-di-oleins, respectively. [15]
2.7 Transesterification of Soapnut Oil:
Biodiesel is prepared by acid esterification followed by alkaline transesterification because

the acid value of soapnut oil is greater than 6. So to reduce acid value esterification is
necessary.
Pretreatment: Methanol and vegetable oil at 6:1 ratio is taken in the reaction flask, and the
mixture is heated up to 55˚C. After attaining the temperature of 55˚C, 1 wt% of anhydrous
sulphuric acid is added drop-wise to the mixture. The reaction is continued for 60 minutes,
maintaining a constant stirring speed of 600 rpm. After esterification, the product is shifted to
separating funnel, followed by 3 hours of decantation. The upper layer consist of unreacted
methanol and free fatty acid. A layer containing the mixture of monoglycerides, diglycerides,
triglycerides and methyl ester formed during the reaction is settled at the bottom. The
unreacted methanol is then evaporated from the mixture using rotary evaporator. The lower
layer is then separated from the mixture. The acid value of the product is determined to
ensure the completion of reaction, so that the product could be taken to the second stage of
transesterification reaction. [43]
Alkaline transesterification:
The cooled dried product of first stage esterification is subjected to alkaline

transesterification. In this stage, the product of first stage is taken in 500 ml reaction flask and
kept over the constant temperature oil bath for uniform heating and variable speed stirrer is
used for mixing purpose. Methanol in specific proportion is then added into the oil. When the
mixture reaches 65˚C, fine powder of homogeneous catalyst (NaOH, KOH) or heterogeneous
catalyst (CaO, MgO) in specific proportion is added to the mixture as a catalyst and allowed
to stir upto 120 minutes at 600 rpm. After completion of the reaction, excess methanol from
the mixture with the help of rotary evaporator. The mixture is then transferred into the
separating funnel and allowed to settle. After 6 hours of decantation, two distinct layers of
methyl ester and glycerol are formed. Biodiesel is washed for 7-8 times with distilled water to
remove the trace amount of glycerol present in it. Finally biodiesel is dried by passing over
the heated sodium sulphate. [43]
2.8 Performance Characteristics of Soapnut Biodiesel:
R.D. Misra, M.S. Murthy using Soapnut (Sapindus mukorossi) oil as nonedible straight
vegetable oil was blended with petroleum diesel in various proportions to evaluate the
performance characteristics of a single cylinder direct injection constant speed diesel engine.
Diesel and soapnut oil (10%, 20%, 30% and 40%) fuel blends were used to conduct short-
term engine performance test at varying loads in terms of 25% load increments from no load
to full loads. Tests were carried out for engine operation and engine performance parameters
such as fuel consumption, brake thermal efficiency, and exhaust emissions (smoke, CO,
UBHC, NOx, and O2) were recorded. Among the blends SNO 10 has shown a better
performance with respect to BTE and BSEC. SNO 10% has an overall better performance
with regards to engine performance characteristics. [16]
BTE of all blends is lower than that of petro-diesel. Among the various blends SNO 10 has
better BTE at 75% loading conditions. When compared with petro-diesel the BTE with SNO
blends is slightly less. This may be due to higher viscosity of the blends resulting in poorly
formed fuel sprays and air entrainment affecting the combustion in the engine and further due
to lower volatility of vegetable oils. BSEC for all blends at all loads is more about 4–8%
With increasing blend percentage of SNO the BSEC is increasing. This may be due to lower
calorific value and higher density of soapnut oil. Among the blends BSEC for SNO 10 is
lowest at 85% loads which is normally the optimum loading for any diesel engine. Hence
from BSEC point of view SNO 10 may be advantageous. [16]
Vinoothan Kaliveer, Rolvin S. D‟Silva, Prashanth Kumar, K. Raju in their work, soap nut
oil, cotton seed oil methyl ester and diesel were blended in the proportion of 10:15:75 by
volume to form a bio diesel blend of B25. It has been observed that the calorific value is
lower and viscosity is higher for B25 as compared to diesel. The performance characteristics
were studied using a variable compression ratio diesel engine test rig for three different
compression ratios of 17, 17.5 and 18. The results showed that the brake thermal efficiency
has increased by 5.2% at a compression ratio of 18 compared to the brake thermal efficiency
at a compression ratio of 17. Brake specific fuel consumption has decreased by 4.7% with the
increase in compression ratio. However the brake thermal efficiency for B25 is lower than
that of diesel. [44]
2.9 Design of Experiments with the Taguchi Method
Taguchi is a statistical method developed by Genichi taguchi to investigate the effect of

different parameters on variance of oil extraction and transesterification process that
determines the suitable operating conditions of the process. Taguchi method making
statistical design by using orthogonal array also offers an opportunity to reduce the number
the experiments. Taguchi method computes signal to noise ratio based on experimental data.
This ratio defines an experiment level which gives the best yield in the test variables. In
addition, the effect of test parameters on the experiment outputs is statistically demonstrated
by ANOVA. Therefore with the help of both S/N ratio and ANOVA, operating parameters
required for oil extraction and transesterification process can be determined to provide
optimum yield.
2.9.1 Signal to noise ratio analysis:
S/N ratios obtained from Taguchi method are used to achieve the optimization of operating
parameters. S/N ratios are logarithmic functions of the expected experimental outcome which
is to provide a healthy optimization. There are three types of S/N ratios and these are nominal
is best, smaller the better and larger the better. In this study, while the largest highest yield
was used larger the better theorem calculated by equation 1.
S/N ratio = -10 log (∑ ) (1)

Where S/N ratio is signal to noise ratio (dB), Yi symbolizes the quality characteristics value
obtained from the tests, and n is the test number.
2.9.2 Analysis of variance (ANOVA):
ANOVA is a statistical method which is used to define the individual interactions into the test
results of all operating parameters. In this study, ANOVA analysis was performed with 95%
confidence level and 5% significance level as p contribution and p values of the operating
parameters which are indicated the significance of control factors. Furthermore, ANOVA is
used to estimate the response magnitude of each parameter in the L9 orthogonal experiment.
In this work, ANOVA is used to identify and quantify the most significant factor that
contributes to maximum yield. In ANOVA, the basic property is that the total variation is
equal to the sum of squares of the deviation of all the condition parameters and the error
components.
2.10 Summary of Literature Review
Use of vegetable oil as CI engine fuel is radically not a new concept despite direct use of it in
the engine creates unfavourable problems due to high viscosity. From the review of literature,
it was found that work done so far is mostly on Karanja and Jatropha. It was observed that,
there are still many supplementary potential options for alternative to diesel. Newer studies
on biodiesel like rice bran oil, jojoba oil, rubber seed, mahua oil, simarouba oil, sesame oil,
neem oil, undi oil, and large amount of regional oil has been done. However very few
research papers are available on Soapnut biodiesel as a potential substitute to diesel.
In view of the above, Soapnut seeds is a potential candidate for the optimization study of oil
extraction from its kernel and transesterification reaction of Soapnut oil and study the
performance of diesel engine using SOME. Soapnut seeds contain 30% oil of which 92% are
triglycerides. Soapnut is a fruit of the soap nut tree generally found in tropical and subtropical
climate areas including Asia, America, and Europe. The scientific name of Soapnut oil is
Sapindus Mukorossi. It is found in India, Nepal, Bangladesh and Pakistan. Soapnut trees
naturally grow in deep clay loam soil and flourish in areas with annual rainfall of 150-200 cm
where they prevent soil erosion. It is found that 16.5% of the S. mukorossi oil is saturated
while 81.6% of oil is unsaturated. Amongst the saturated fatty acid, arachidic acid is the
highest (7.5%), followed by palmitic acid (5.5%). The other saturated fatty acids are stearic
acid (2.3%), behenic acid (1%) and lignoceric acid (0.2%). Amongst the unsaturated fatty
acids, oleic acid (58.4%) is the most dominant one. The other types of unsaturated fatty acids
include linolenic (17.1%) and linoleic acid (5.4%). Trace amount of erucic acid (0.4%) and
palmitoleic acid (0.3%) are also present.
Very few studies are available on oil extraction of oil form Soapnut seeds, transesterification
of Soapnut oil using alkaline catalyst and the performance of diesel engine using SOME.
From literature it is found that, there is a scope for experimental study on following aspects
of Soapnut oil;
 Study of effect of operating parameters such as seeds size, reaction temperature, reaction
time and volume of solvent on oil extraction process by Soxhelet extractor.
 Study of effect of type of solvent on oil yield.
 Study of effect of operating parameters such as oil to methanol ratio, catalyst type,
catalyst concentration and reaction temperature on when homogeneous catalyst are used
during transesterification process.
 Study of effect of operating parameters such as oil to methanol ratio, stirrer speed,
catalyst concentration and reaction temperature on when heterogeneous catalyst are used
during transesterification process.
 Study of effect of type of catalyst (Homogeneous and Heterogeneous catalyst) on SOME
yield
 Study of performance of single cylinder diesel engine using Soapnut oil methyl ester and
its blends.
Chapter 3
Oil Extraction and Preparation of Biodiesel
3.1 Introduction
Oil from Soapnut seeds can be extracted by different extraction techniques such as
mechanical extraction, chemical or solvent extraction, accelerated solvent extraction,
enzymatic extraction, and supercritical fluid techniques. Although the oil extraction
techniques using mechanical expeller was obtained at low cost but this is relatively
ineffective due to lower oil yields. Therefore, chemical oil extraction technique was found to
be very effective because of high oil yield. Solvent extraction is the process in which
constituent is removed from a solid by means of solvent. Chemical extraction using n-hexane
results in the highest oil yield.
The viscosity of vegetable oils can be reduced by several methods which include blending of
oils, micro emulsification, pyrolysis and transesterification. Among this transesterification is
widely used for industrial biodiesel production. Because it gives high yield with low
temperature, pressure and short reaction time. Transesterification is a chemical reaction
involving triglycerides with alcohol in the presence of catalyst is shown in Fig. 3.1.
Fig no 3.1 Mechanism of Transesterification Reaction
R‟, R2”, R”‟ represent various alkoxy group. Based on the use of catalyst the
transesterification can be divided in to three types they are acid catalysed, alkali catalysed
and enzyme catalysed method. For transesterification process methanol was commonly used.
Because methanol is cheaper than ethanol and the recovery of unreacted methanol is easier.
In the case of base catalyst potassium hydroxide (KOH) or sodium hydroxide (NaOH) are
used, because it is less expensive and easy to handle in storage and transport. However most
of the studies show best properties of biodiesel was obtained by using potassium hydroxide.
Nevertheless base catalysed transesterification method is commonly employed for BD
production. Since, it is more economical method than other methods but base method is not
suitable if the oils having high FFA content. In this situation a two-step catalysed method
such as acid method followed by alkali method was used to prepare the biodiesel non-edible
oils like Jatropha, Pongamia, simarouba and Madhuca.
3.2 Development of Oil Extraction and Biodiesel Preparation Set-up
Fig. 3.2 Soxhelet Extraction Unit

To extract oil from Soapnut seeds kernel, Soxhelet extraction unit was used. The Soxhelet
extraction unit consist of round bottom flask, extractor and condenser. The solvents required
for oil extraction from seeds was poured into round bottom flask. Seeds from which oil was
extracted put into the extractor. Condenser was used for the condensation of solvent vapour
into liquid formed due to heating of solvent falls in the extractor. As the solvent comes in
contact with seeds it extracts oil. Heating mantle was used for the heating of solvent. Fig 3.1
shows the photograph of actual setup.
Fig 3.3 schematic diagram of biodiesel production set up [52]

Fig. 3.4 Biodiesel Production Set Up
To prepare methyl esters from Sapindus Mukorossi oil, laboratory-scale biodiesel preparation
set-up was developed. Laboratory scale transesterification set-up constitutes, 500 ml capacity
reaction flask which accommodate three necks one for motorized-stirrer another to attach
condenser and last one for thermometer. As reaction necessitates constant heating and
continuous stirring, Constant temperature oil bath and motorized stirrer are must. 1/2 hp-4000
rpm motorized stirrer and 450 W constant temperature oil bath are speed and temperature
control-equipped. Reflux plain condenser of 12” has used with water in-out connection to
collect water vapour inside reaction flask. Digital Thermocouple is used for measuring the
reaction temperature. Weighing scale, pH meter and other glassware accessories are passive
instruments and apparatus to the set-up. Fig. 3.2 shows schematics of set-up and fig. 3.3
shows the photograph of the actual set up.
Crude Soapnut oil
Methanol+ H2SO4 Esterification

Methanol +KOH Pre-treated oil
Transesterification Glycerol layer
Settling + Separation
Ester layer
Hot Water Washing and drying
Soapnut Biodiesel
Figure 3.5 Flow Chart of Biodiesel Production from Crude Soapnut Oil
 Materials:
i. Feedstock: Soapnut oil, ii. Acid catalyst: H2SO4,
iii. Homogeneous Base Catalyst: KOH, NaOH iv. Heterogeneous base catalyst: CaO, MgO .
v. Reactant: Methanol, vi. Reactor Vessel
Two step catalysed method such as acid method followed by alkali method was used to
produce biodiesel from crude Soapnut oil. In this method, methanol was used as reagent and
H2SO4 and KOH or CaO were used as catalysts for acid and base reactions, respectively.
 Esterification: In the esterification, high FFA content of non-edible oil is reduced by

using acid pre-treatment. The mixture of Soapnut oil and methanol at 6:1 oil to methanol ratio
is first heated to 55˚C. As soon as the temperature of mixture reaches 1 wt% of H2SO4 is
added. Continue the reaction with a constant stirring speed of 600 rpm and reaction
temperature of 60˚C for 60 minutes.
 Transesterification- Base Catalysed Reaction: Mixing of Alcohol and Catalyst: The

product obtained from esterification reaction is shifted to separating funnel and allow 3 hours
of decantation. After 3 hours two layers were formed, the upper layer consists of unreacted
methanol and free fatty acid and lower layer consist of triglycerides and methyl esters. The
lower is then separated from the mixture. For transesterification, this product and methanol at
specific oil to methanol ratio in put into reaction flask with a constant stirring speed of 600
rpm for proper mixing for 30 minutes.
 Transesterification Reaction: After 30 minutes, 1 wt% of homogenous alkali catalyst

such as KOH, NaOH, NaOCH3 or heterogeneous alkali catalyst such as CaO, MgO is added
to the mixture of oil and methanol maintaining a constant stirring speed of 600 rpm for
uniform mixing at a temperature of 60˚C. Allow the reaction for 3 hours.
 Settling and Separation:
Fig. 3.6 Settling and Separation

Once the reaction is complete, it is allowed for settling for overnight in separating funnel.
At this stage two major products obtained that are glycerine and biodiesel. The glycerine
phase is much denser than biodiesel phase and is settled down while biodiesel floated up.
Then, crude biodiesel was purified by washing with warm water to remove residual catalyst
or soaps.
 Drying of Biodiesel: This is normally the end of the production process to remove water
and methanol present in the biodiesel, this is removed by heating prepared biodiesel at 110˚C
for 30 min. it is clear that, the biodiesel recovery from Soapnut oil.
3.3 Summary
Two stages are required for preparation of Soapnut biodiesel. Two step catalysed method
such as acid method followed by alkali method was used to produce biodiesel from crude
Soapnut oil. Firstly, prepare small scale laboratory set-up for biodiesel preparation. Select the
optimum parameter from the literature survey. Then collect the raw oil extracted from seeds
kernel. Biodiesel was preparing from Soapnut crude oil by using transesterification set-up. It
is easy but time consuming process.
Chapter 4
Experimental Set-up & Plan of Experiment
The engine tests were conducted on a single cylinder four-stroke, naturally aspirated, open
chamber water-cooled CI engine. The engine was operated at a rated constant speed at 1500
rev/min and had a conventional fuel injection system. Fig. 4.1 shows the schematic diagram
of the set-up and Fig. 4.2 shows the overall view of the experimental set-up. The
specifications of the engine are given in Appendix 1. The injector opening pressure and the
static injection timing as specified by the manufacturer was 205 bar and 23oBTDC
respectively. The engine was provided with a toroidal combustion chamber with overhead
valves operated through push rods. Eddy current dynamometer has been used for
measurement of output. Cooling of the engine was accomplished by circulating water through
the jackets on the engine block and cylinder head. A piezoelectric pressure transducer was
mounted with the cylinder head surface to measure the cylinder pressure.
Fig. 4.1 Schematic of engine set-up

Fig. 4.2 Overall view of engine-setup
Fig.4.2 shows the complete experimental engine test rig with EGR arrangement
4.1 Fuels Used for Tests
Table 4.1 Properties of fuel studied
Sr. Property Units Diesel SOME SOME BD10 SOME SOME SOME
BD 5 BD 20 BD 30 100
no.
1 Density at 150C Kg/m3 830 832 833 835 840 870
2 Kinematic Cst. or 4.7 4.82 4.9 5.25 5.30 5.71

viscosity at 400C mm2/sec
3 Calorific value MJ/kg 42.5 41.52 41.10 40.68 40.10 38.50
4 Cetane number ---- --- --- --- --- --- 52.8

Fuels are used in the single mode of operation includes of diesel, Soapnut oil methyl ester
and its blend with diesel. Biodiesel-diesel blend was done on percent volume basis of diesel
and biodiesel for net unit volume. The combinations of blends BD5, BD10, BD20 and BD30
were studied for single cylinder CI engine. Whereas the number signifies, percent volume of
biodiesel in diesel fuel at unit volume. Soapnut oil methyl ester of good quality was used for
the study. All important properties of SOME were checked prior to test. The properties of
these fuels are given in Table 4.2
4.2 Design of Experiments
4.2.1 Optimization of oil extraction process:
Optimization of the oil extraction process by Soxhelet extraction unit for Soapnut seeds
kernels was done using taguchi method. In this a set of orthogonal array for performing
fewest experimental design based on the L9 (3) 4 matrix was employed are shown in table 4
and 5. Four factor at three level each namely seeds size (1 mm, 2 mm, 3 mm), Reaction
temperature (65˚C, 75˚C, 85˚C), Volume of solvent (400 ml, 450 ml, 500 ml), Reaction time
(1hr , 2 hr, 3 hr).
Table 4.2: Design of experiments, with four parameters at three levels, for the
extraction of oil
Parameters Level 1 Level 2 Level 3
Seeds Size 1 mm 2 mm 3 mm
Reaction Temperature 65˚C 75˚C 85˚C
Volume of Solvent 400 ml 450 ml 500 ml
Reaction time 1 hr 2 hr 3 hr
The above experimental results were analysed with ANOVA performed to more systemically
analyse the relative importance of each experimental parameter on the production of Soapnut
oil methyl esters.
Table 4.3 Design of experimentation (Oil Extraction)
Seeds Size Reaction Temperature Volume of Solvent Reaction time
1 1 1 1
1 2 2 2
1 3 3 3
2 1 2 3
2 2 3 1
2 3 1 2
3 1 3 2
3 2 1 3
3 3 2 1
Thus 9 experimental results were analysed with ANOVA. This was done for the systematic
analysis of the relative importance of each experimental parameter on the extraction of oil.
4.2.2 Optimization of transesterification reactions:
Optimization of transesterification process for Soapnut oil was done using taguchi method. In
this, a set of orthogonal array for performing fewest experimental design based on the L9 (3)
4 matrix was employed (are shown in table). Four factors at three level each namely catalyst
type ( KOH, NaOH, NaOCH3), Catalyst concentration in wt% to oil (0.5, 1, 1.5 wt%), Oil to
methanol molar ratio ( 1:6, 1:8, 1:10), Reaction temperature (50˚C, 55˚C, 60˚C) for
homogeneous catalyst.
Table 4.4 Design of experiments, with four parameters at three levels, for the
production of SOME (Homogeneous Catalyst)

Oil to methanol ratio 1:06 1:08 1:10
Catalyst type NaOH KOH NaOCH3
Catalyst concentration (wt%) 1 1.5 2
Reaction temperature 60°C 65°C 70°C
Table 4.5 Design of experimentation (Transesterification process using homogeneous
catalyst)
Oil to methanol ratio Catalyst Type Catalyst concentration Reaction Temperature
1 1 1 1
1 2 2 2
1 3 3 3
2 1 2 3
2 2 3 1
2 3 1 2
3 1 3 2
3 2 1 3
3 3 2 1
Four factors at three level consist of oil to methanol ratio (1:08, 1:10, 1:12), stirrer speed
(600, 700, 800 rpm), catalyst concentration (1, 1.5, 2 wt%) and reaction temperature (60˚C,
65˚C, 70˚C) using heterogeneous catalyst CaO.
Table 4.6 Design of experiments, with four parameters at three levels, for the
production of SOME (Heterogeneous Catalyst)
Oil to methanol ratio 1:08 1:10 1:12
Stirrer Speed (RPM) 600 700 800
Catalyst concentration (wt%) 1 1.5 2
Reaction temperature 60°C 65°C 70°C

The above experimental results were analysed with ANOVA performed to more
systematically analyse the importance of each experimental parameter on the production of
Soapnut oil methyl ester (SOME).
Table 4.7 Design of experimentation (Transesterification process using heterogeneous

catalyst)
Oil to methanol ratio Stirrer speed Catalyst concentration Reaction temperature
1 1 1 1
1 2 2 2
1 3 3 3
2 1 2 3
2 2 3 1
2 3 1 2
3 1 3 2
3 2 1 3
3 3 2 1
Thus 27 experimental results were analysed with ANOVA. This was done for the systematic
analysis of the relative importance of each experimental parameter on the production of
SOME.
4.2.3 SOME-Diesel blends operation at standard engine setting
In this phase, engine was operated on blends of BD5, BD10, BD20 and BD30 at standard
engine operating parameters which are recommended by manufacturer.
4.3 Summary
Taguchi method was used for the optimization of oil extraction process by Soxhelet
extraction unit. Four factors seeds size, reaction temperature, volume of solvent, reaction time
were considered to study the variation in yield of Soapnut oil. Experiment was design with
the help of taguchi method to reduce number of iterations.
Similarly taguchi was used for the optimization of transesterification process. Experiment
was designed with the help of taguchi method and the parameters considered were oil to
methanol ratio, catalyst type, catalyst concentration, reaction temperature when homogeneous
catalyst are used and the parameters were oil to methanol ratio, stirrer speed, catalyst
concentration (CaO) and reaction temperature when heterogeneous catalyst are used. Engine
was operated with SOME blends such as SN 5, SN 10, SN 20, and SN 30 to compare diesel
engine performance with diesel.
Chapter 5
Results and Discussion
The present study aimed to optimize the suitable reaction conditions of seeds size, reaction
temperature, volume of solvent and reaction time on the oil extraction process. Also to
optimize the suitable reactions conditions of oil to methanol ratio, type of catalyst, amount of
catalyst used and reaction time on transesterification. Table no shows the ANOVA of
Soapnut oil and Soapnut oil methyl ester, it shows that all the parameters are significant and
contribute the effect for yield conversion. The effect of seeds size, reaction temperature,
reaction time has the major effect on oil extraction while oil to methanol to methanol ratio,
types of catalyst and catalyst concentration has the major effect on transesterification. Check
the variation in oil yield with change of solvents such methanol and n-hexane. Finally studied
the effect of different blends of SOME with diesel on engine performance is presented in this
chapter.
5.1 Oil Extraction:
Four factors namely seeds size, reaction temperature, reaction time and volume of solvent are
selected to study their effects on oil yield.
5.1.1 Effect of seeds size on oil yield:

Effect of Seeds Size on Oil Yield
42.5
40.0
Mean of Oil Yield (wt%)

37.5
35.0
32.5
30.0
27.5
25.0
1.0 1.5 2.0 2.5 3.0

Seeds Size (mm)
Fig 5.1 Effect of Seeds Size on Oil Yield
The yield of oil from seeds depends on its size. As the size of seeds goes on reducing the
solvent used for oil extraction becomes more soluble in seeds so that it can easily extract oil
from seeds kernel. As the solubility increases the amount of oil extracted also increases.
It is seen from the figure that as the size of seeds reduces the yield of oil increases. Hence it is
suitable to extract oil from seeds of small size rather than bigger size.
5.1.2 Effect of reaction temperature on oil yield:
As the reaction temperature increases, the reaction rate and solubility of solvent increases.
With the increases in temperature, the number of cycles during which oil is extracted
increases for the same time when temperature is low, therefore amount of oil extracted
increases with increase in reaction temperature. Also the solubility of solvent of at higher
temperature is more than at lower temperature, hence yield increases with increase in
temperature.
Effect Reaction Temperature on Oil Yield
32.0
31.5
Mean of Oil Yield (wt%) 31.0
30.5
30.0
65 70 75 80 85
Reaction Temperature (˚C)
Fig 5.2 Effect of Reaction Temperature on Oil Yield
It is seen from the figure that as the reaction temperature increases the yield of oil extracted
increases. Hence it is suitable to extract oil at higher reaction temperature.
5.1.3 Effect of reaction time on oil yield:
As the reaction time increases, the amount of time solvent gets to extract oil from seeds
increases. So the time for which the seeds remain soluble in solvent increases. Therefore for
the same reaction temperature if the reaction time increases then yield of oil also increases.
It is seen from the figure that as the reaction time increases the yield of oil extracted
increases. Hence it is suitable to extract oil at higher reaction time.
Effect of Reaction Time on Oil Yield

33
32
31
30
29
28
1.0 1.5 2.0 2.5 3.0
Reaction Time in Hours
Fig 5.3 Effect of Reaction Time on Oil Yield
5.1.4 Effect of volume of solvent on oil yield:
There is not much effect of the parameter volume of solvent of oil yield, but as the volume of
solvent increases the amount of solvent which came in contact with the seeds increases and
therefore yields of oil increase.
Effect of Volume of Solvent on Oil Yield

32.0
31.5
31.0
30.5
30.0
400 420 440 460 480 500

Volume of Solvent (ml)
Fig 5.4 Effect of Volume of Solvent on Oil Yield
It is seen from the figure as the volume of solvent the yield of oil extracted increases. Hence
it is suitable to extract at higher volume of solvent.
5.2 Effect of Type of Solvent on Oil Yield

45
40
35
Oil Yield (wt%)

30
25 Oil Yield (wt%)
20 (n-hexane)
15
Oil Yield (wt%)
10 (Methanol)
5
0
0 1 2 3 4
Seeds Size (mm)
Fig 5.5 Effect of type of solvent on oil yield
The amount of oil extracted from Soapnut seeds changes with change in solvent such as
Methanol and n-hexane. It is seen from the figure the yield of Soapnut oil extracted from
Soapnut seeds varies with change in type of Solvent and it clear from the figure that the
amount of oil extracted using n-hexane is greater than amount of oil extracted using
methanol.
5.3Transesterification Process (using Homogeneous Catalyst)
Four factors namely molar ratio, catalyst type, catalyst concentration and reaction
temperature are selected to study their effects on SOME yield.
5.3.1 Effect of molar ratio on SOME yield:
In stoichiometric transesterification reaction, each mole of triglycerides requires three moles

of alcohol to produce three moles of fatty acid alkyl esters and one mole of glycerol, whereas
esterification requires one mole of FFA and one mole of alcohol to generate one mole of ester
and one mole of water. Since these reactions are reversible, excess alcohol is required to
drive the reaction towards product side for increasing and completing the conversion. The
average molecular weight of Soapnut oil was calculated from its composition and accordingly
the amount of methanol was taken into the reaction. The oil to methanol ratio was varied
from 1:6 to 1:10 to study its effect on yield of conversion process.
Effect of molar ratio on SOME yield
90
85
Mean of SOME Yield (wt%)

80
75
70
1:08 1:09 1:10 1:11 1:12

Oil to methanol ratio
Fig 5.6 Effect of molar ratio on SOME Yield
The mean yield of SOME at different molar ratio 1:6, 1:8, 1:10 are shown in figure. The
effect of methanol on in the range of 1:8 to 1:10 was investigated. It was found that the ester
yield increases with increase in molar ratio oil to methanol. At low molar ratio, low
proportion of methanol reduces the probability of breaking bonds of glycerol and
triglycerides reducing the yield. Though the stoichiometric ratio is 3:1, the general trend is
increase in the yield with increase in the molar ratio. Therefore the molar ratio at 1:10 shows
the optimum molar ratio for the yield of Soapnut oil. However there is need to experiment
with high molar ratio and more levels to find the optimum limit for the molar ratio.
5.3.2 Effect of catalyst type on SOME yield:
The type of catalyst required in the transesterification process usually depends on the quality
of feedstock and method applied for transesterification process. For a purified feedstock, any
type of catalyst cold be used for the transesterification process. However, for feedstock with
feedstock of high moisture content and free fatty acids contents, homogenous
transesterification process is unsuitable due to high possibility of saponification process
instead of transesterification process occur. Two step transesterification process is suggested
by many researcher. At present, homogenous catalyst such as NaOH and KOH are used by
biodiesel industry due to their simple usage and short time required for conversion of oils to
ester.
The homogenous catalyst (NaOH, KOH, NaOCH3) catalyst forms sodium and potassium
meth oxide due to its solubility in methanol which augment the completion of reaction. The
main advantage homogenous acid and alkali catalysts are high yield and low cost. However
they suffer form few limitations such as need of water washing, neutralization by respective
acids or alkali and needs drying process.
Fig 5.7 Effect of Catalyst Type on SOME Yield
The results obtained are presented in figure. The output values represented in figure are mean
percentage values of yield. There is significant effect of type of catalyst on yield. Amongst
the homogenous catalyst the output with KOH is greater than with NaOH, NaOCH3.
5.3.3 Effect of catalyst concentration on SOME yield:
Tests were conducted to study the effect of amount of catalyst used on conversion of Soapnut
oil to ester. The results of the tests are presented in fig. 5.8.
The amount of catalyst used during the test was varied from 0.5 to 1.5 % of weight of the oil
in a step of 0.5. Hence, yield of SOME increases with increase of catalyst concentration. If
we see the rate of yield conversion it is faster upto 1.0 wt% catalyst concentration after there
is slightly lower the yield conversion rate. As increase in catalyst concentration no doubt
yield increases, this is due to availability of more active sites by addition of larger amount
catalyst in the transesterification process. However, on economic perspective, larger amount
of catalyst may not be profitable due to cost of the catalyst itself. Hence for economic and
performance points of view, 1 wt % catalyst loading is optimum for Soapnut oil.
Effect of catalyst concentration on SOME yield
76.5
Mean of SOME yield (wt%)

76.0
75.5
75.0
74.5
0.50 0.75 1.00 1.25 1.50
Catalyst Concentration (wt%)
Fig 5.8 Effect of Catalyst Concentration on SOME Yield
5.3.4 Effect of reaction temperature on SOME yield:
The reaction temperature was varied from 50 to 60˚C. The results of the test are presented in
fig. The yield of Soapnut oil increases with increase in temperature up to 60˚C. The
Effect of reaction temperature on SOME yield

76.5
Mean of SOME yield (wt%)
76.0
75.5
75.0
60 62 64 66 68 70
Reaction temperature (˚C)
Fig 5.9 Effect of Reaction Temperature on SOME Yield
Maximum value mean yield was observed at 60˚C. It is interesting to note that maximum
yield was observed at temperature of 60˚C. However there is need to experiment with more
temperatures and more levels to find the optimum limit for reaction temperature.
5.4 Transesterification Process (using Heterogeneous Catalyst)
Four factors namely molar ratio, stirrer speed, catalyst concentration and reaction temperature
are selected to study their effects on SOME yield
5.4.1 Effect of molar ratio on SOME Yield:
In stoichiometric transesterification reaction, each mole of triglycerides requires three moles

of alcohol to produce three moles of fatty acid alkyl esters and one mole of glycerol, whereas
esterification requires one mole of FFA and one mole of alcohol to generate one mole of ester
and one mole of water. Since these reactions are reversible, excess alcohol is required to
drive the reaction towards product side for increasing and completing the conversion.
Effect of Oil to Methanol Ratio on SOME Yield

90
85
80
75
1:08 1:09 1:10 1:11 1:12

Oil to Methanol Ratio
Fig 5.10 Effect of molar ratio on SOME yield
The average molecular weight of Soapnut oil was calculated from its composition and
accordingly the amount of methanol was taken into the reaction. The oil to methanol ratio
was varied from 1:08 to 1:12 to study its effect on yield of conversion process.
The mean yield of SOME at different molar ratio 1:8, 1:10, 1:12 are shown in figure. The
effect of methanol on in the range of 1:08 to 1:12 was investigated. It was found that the ester
yield increases with increase in molar ratio oil to methanol. At low molar ratio, low
proportion of methanol reduces the probability of breaking bonds of glycerol and
triglycerides reducing the yield. Though the stoichiometric ratio is 3:1, the general trend is
increase in the yield with increase in the molar ratio. Therefore the molar ratio at 1:12 shows
the optimum molar ratio for the yield of Soapnut oil. However there is need to experiment
with high molar ratio and more levels to find the optimum limit for the molar ratio.
5.4.2 Effect of stirrer speed on SOME yield:
Mixing is an important factor in transesterification process for maximum conversion of

triglycerides into methyl ester. During transesterification, fat or oil is immiscible with
heterogeneous catalyst. After mixing of two these phases, no further mixing is required.
Therefore mixing intensity is considered to be an important factor in transesterification
process. Mixing intensity increases with increase in stirrer speed.
Effect of Stirrer Speed on SOME Yield

85
84
83
82
81
80
79
78
77
76
600 650 700 750 800
Stirrer Speed (RPM)
Fig. 5.11 Effect of stirrer speed on SOME yield
Thus it is seen from fig that as the stirrer speed increases the yield of biodiesel also increases.
At higher stirrer speed there will be proper mixing of oil and alcohol and maximum
conversion of triglycerides into methyl esters. However there is need to experiment with high
stirrer speed and more levels to find the optimum limit for the stirrer speed.
5.4.3 Effect of catalyst concentration on SOME yield:
Tests were conducted to study the effect of amount of catalyst used on conversion of Soapnut
oil to ester. The results of the tests are presented in figure 5.12.
Effect of Catalyst Concentration on SOME Yield
81.5
81.0
80.5
80.0
79.5
1.0 1.2 1.4 1.6 1.8 2.0

Catalyst Concentration (wt%)
Fig. 5.12 Effect of catalyst concentration on Biodiesel yield
The amount of catalyst used during the test was varied from 0.5 to 1.5 % of weight of the oil
in a step of 0.5. Yield of SOME increases with the increase in catalyst concentration. If we
see the rate of yield conversion it is faster upto 1.0 wt% catalyst concentration after there is
slightly lower the yield conversion rate. As increase in catalyst concentration no doubt yield
increases, this is due to availability of more active sites by addition of larger amount catalyst
in the transesterification process. However, on economic perspective, larger amount of
catalyst may not be profitable due to cost of the catalyst itself. Hence for economic and
performance points of view, 1 wt % catalyst loading is optimum for Soapnut oil.
5.4.4 Effect of reaction temperature on SOME yield:
The reaction temperature was varied from 60 to 70˚C with a unit step of 5°C. The results of
the test are presented in fig 5.13. The yield of Soapnut oil increases with increase in
temperature upto 70˚C. The Maximum value mean yield was observed at 70˚C. It is
interesting to note that maximum yield was observed at temperature of 70˚C. It is interesting
to note that the maximum was found at 70°C which is more than the boiling point of
methanol (65°C). The formation of vapour causes volatilization and the momentum between
the mono-glyceride, di-glyceride, triglyceride and glycerol which helps for breaking the
bond. However there is need to experiment with more temperatures and more levels to find
the optimum limit for reaction temperature.
Effect of Reaction Temperature on SOME Yield

81.2
81.0
80.8
80.6
80.4
80.2
80.0
60 65 70 75 80
Reaction Temperature (˚C)
Fig 5.13 Effect of Reaction Temperature on SOME yield
5.5 Effect of Type of Catalyst on SOME Yield
To increase the rate of reaction of reaction of transesterification process catalyst are added.
Generally homogeneous and heterogeneous alkali catalysts are added. From recent literature,
yield of biodiesel using homogeneous catalyst is more than in case of heterogeneous catalyst.
But during experimentation it has been that in case of Soapnut oil biodiesel yield using
heterogeneous catalyst is more than by using heterogeneous catalyst. It is clear from the fig.
5.14 the yield of SOME using heterogeneous catalyst is greater than by using homogeneous
catalyst. Although the yield of crude biodiesel is greater in case homogeneous catalyst but in
the process of removing impurities by washing SOME with warm water the yield of SOME
decreases as it is difficult to remove homogeneous catalyst from SOME.
100
Yield of SOME (wt%) 90
80
Yield of SOME using

hom. Catalyst (wt%)
70
Yield of SOME using
Het. Catalyst (wt%)
60
50
1:07 1:09 1:10 1:12 1:13
Oil to methanol ratio
Fig. 5.14 Effect of type of catalyst on SOME yield
However in case of heterogeneous catalyst the yield of crude biodiesel is less as compared to
yield with homogeneous catalyst. But it is very easy to remove heterogeneous catalyst from
SOME by washing it with warm water 2 to 3 times. Hence the yield of SOME is greater in
case of heterogeneous catalyst than homogeneous catalyst. So it is recommended to use
heterogeneous catalyst for transesterification of Soapnut oil.
5.6 S/N Ratios of Experiments
In this analysis, since the objective function is yield, larger the better types of control
function was used in calculating the signal to noise ratios. The expression used to calculate
the objective function is,
S/N ratio = -10 log (∑ )

Table 5.1 S/N Ratios of the Experiments (Oil Extraction)
Experiment Number S/N Ratio (dB)
1 25.7201
2 28.0004
3 28.8308
4 29.2420
5 28.3395
6 28.9370
7 32.1962
8 32.5062
9 31.9714
Table 5.2 S/N Ratios of the Experiments (Transesterification process using

homogeneous catalyst)

1 35.9176
2 36.8397
3 36.7138
4 36.7770
5 37.4431
6 36.9020
7 38.6900
8 39.2284
9 38.8402
Table 5.3 S/N ratios of the experiments (Transesterification process using heterogeneous
catalyst)
1 36.4825
2 37.4825
3 37.8786
4 37.6880
5 38.2402
6 38.4160
7 38.5884
8 38.9222
9 39.2436
The S/N ratios of all the experiments are calculated and tabulated in table 5.1, 5.2, and 5.3.
From table 5.1, 5.2, and 5.3 it is noted that,
 S/N ratio of oil extraction process for eighth experiment is 32.5062 shown in table 5.1
which imply that maximum yield of Soapnut oil can be achieved when the process
parameters are optimized to 1mm seeds size, 75°C reaction temperature, 3 hours of
reaction time and 500 ml volume of solvent.
 S/N ratio of transesterification process using homogeneous catalyst for eighth experiment
is 39.2284 shown in table 5.2 implies that maximum yield of SOME can be achieved
when the process parameters are optimized to 1:12 oil to methanol ratio, KOH as catalyst,
0.5 % catalyst concentration and 70°C reaction temperature.
 S/N ratio of transesterification process using heterogeneous catalyst for ninth experiment
is 39.2436 shown in table 5.3 implies that maximum yield of SOME can be achieved
when the process parameters are optimized to 1:12 oil to methanol ratio, 800 rpm stirrer
speed, 1.5% catalyst concentration and 60°C reaction temperature.
5.7 Analysis of Variance of Experiments:
Analysis of variance of is used to find percent contribution of different parameters on oil

extraction and transesterification process
Table 5.4 Analysis of variance for oil extraction process

Input Sum Sq. DOF Mean Sq. % Contribution
Seeds Size 33.3682 2 17.6841 86
Reaction Temperature 1.1453 2 0.5726 2.78
Volume of Solvent 1.0091 2 0.5046 2.45
Reaction Time 3.6 2 1.8 8.7
Error 0 0 0
Total 41.1225 8
It is seen from the table that the factor which has major impact on oil yield is seed size.
Reaction time is also an important parameter than reaction temperature and volume of
solvent. Thus smaller the seeds size higher will be the oil yield. However there is need to
experiment with much smaller seeds size.
Table 5.5 Analysis of variance for transesterification process using homogeneous

catalyst

Oil to Methanol Ratio 9.7337 2 4.86687 91.50
Catalyst Type 0.7535 2 0.37688 7.08
Catalyst Concentration 0.1064 2 0.0532 1
Error 0 0 0
Total 10.6388 8
It is seen from the table the parameter which has major impact on biodiesel yield is oil to
methanol ratio. Catalyst type is also an important parameter than catalyst concentration and
reaction temperature.
Table 5.6 Analysis of variance for transesterification process using heterogeneous
catalyst

Oil to Methanol Ratio 4.01945 2 2.00973 72.32
Stirrer Speed 1.34217 2 0.67108 24.15
Catalyst Concentration 0.13599 2 0.068 2.5
Error 0 0 0
Total 5.55806 8
5.8 Performance and Emission Analysis of SOME at various SOME-Diesel

Blends
The performance of engine is necessitated to check with SOME-diesel blends. In this section,
performance of engine with SOME-diesel blends operation at standard engine setting is
analysed with reference to diesel operation at standard engine setting.
5.8.1 Effect on BTE at Varying Loads for SOME-Diesel Blends
40
35
30
25 Diesel
BTE (%)
20 B5
15 B10
10 B20
5
B30
0
0 5 10 15 20
Load (kg)
Fig 5.15 Brake thermal efficiency v/s load for various blends
Fig. 5.9 shows brake thermal efficiency as a function of load in kg. Diesel operation gives
highest efficiency of 34.6032% than blends. Trend of decreasing BTE is noticed with
increase in percentage of SOME in diesel.
Amongst all blends tested, the B5 is found to give better BTE a value of 24.70%. Higher BTE
for B5 may be occurred due to effective trade-off between less viscous, higher energy content
energy diesel fuel and oxygenated fuel SOME.
When compared with petro-diesel the BTE with SN blends is slightly less. This may be due
to higher viscosity of blends resulting in poorly formed fuel sprays and the air entrainment
affecting the combustion in the engine and due to lower volatility of vegetable oils.
5.8.2 Effect on SFC at varying loads for SOME-Diesel Blends
The SFC for blends operation of each fuel is found in the tune with BTE. Decreased SFC is
seen for diesel and increased SFC for blends appeared as percentage of SOME increases. The
fig. 5.14 shows variation of SFC with varying load.
0.6
0.5
SFC (kg/kwh)
0.4 Diesel
0.3 B5
0.2
B10
B20
0.1
B30
0
0 5 10 15 20
Load (kg)
Fig 5.16 Specific fuel consumption v/s load for different blends
This may be due to lower calorific value and higher density of Soapnut oil. Among the blends
SFC for B5 is lowest at 15 kg load. Hence from SFC point of view SN5 may be
advantageous.
Chapter 6
Conclusions
The current work was aimed to investigate the Soapnut seeds as a potential feedstock for
biodiesel production to establish optimized parameters for getting maximum oil yield during
oil extraction by using Soxhelet extraction unit and optimized transesterification process for
Soapnut oil using different types of homogenous and heterogeneous catalysts. The study
involved the following;
Oil extraction:
 Getting out kernels from Soapnut seeds to extract oil from it.
 Grind kernel into fine pieces of 1 mm, 2 mm, and 3 mm.
 Use Soxhelet extraction unit to extract oil
 Measurement of oil properties
Transesterification process:
 Extraction of oil from seeds kernels.

 Transesterification with different homogenous catalyst.
 Biodiesel washing
 Measurement of biodiesel properties
Current work was aimed at studying performance characteristics of diesel engine with
biodiesel prepared from Soapnut seed crude oil. Initially, experiments were conducted on
diesel under variable load conditions and standard operating conditions to establish reference
for comparison. Soapnut oil methyl ester was blended with diesel in a proportion to obtain
B5, B10, B20 and B30. These blends were tested at varying loads.
Based on the extensive experimental study, following conclusions have been deduced.
Oil Extraction:
1. After the study of effect of different parameters on oil yield it has been found that the
parameter seeds size has the major effect on oil yield rather than other parameters such as
reaction temperature, reaction time and volume of solvent.
2. The percentage contribution of each parameter during oil extraction is given below,
 Seeds size - 86
 Reaction temperature - 2.78
 Reaction time – 8.7
 Volume of solvent – 2.45
3. From S/N ratio analysis, the maximum yield of oil can be achieved when the process
parameters are optimized to 1mm seeds size, 75°C reaction temperature, 3 hours of
reaction time and 400 ml volume of solvent.
4. Study of effect of type of solvent on oil yield reveals that n-hexane gives greater oil yield
than methanol. Therefore n-hexane is considered as the better solvent for oil extraction
process.
Transesterification Process (using homogenous catalyst)
1. After the study of different parameters on SOME yield it has been found that the effect of
parameter oil to methanol ratio has the major impact on transesterification process rather
than other parameter such as catalyst type, catalyst concentration and reaction
temperature.
2. The percentage contribution of each parameter during transesterification process is given
below,
 Oil to methanol ratio - 91.50
 Catalyst type – 7.08
 Catalyst concentration – 1
 Reaction temperature – 0.42
3. From S/N ratio analysis, the maximum yield of SOME can be achieved when the process
parameters are optimized to 1:12 oil to methanol ratio, KOH as catalyst, 0.5 wt% catalyst
concentration, and 70°C reaction temperature.
Transesterification process (using heterogeneous catalyst)
1. After the study of different parameters on SOME yield it has been found that the effect of
parameter oil to methanol ratio has the major impact on transesterification reaction rather
than other parameters such as stirrer speed, catalyst concentration and reaction
temperature.
2. The percentage contribution of each parameter during transesterification reaction is given
below
 Oil to methanol ratio – 72.32
 Stirrer speed – 24.15
 Catalyst concentration – 2.5
 Reaction temperature – 1.08
3. From S/N ratio analysis, the maximum yield of SOME can be achieved when the process
parameters are optimized to 1:12 oil to methanol ratio, 800 rpm stirrer speed, 1.5 wt%
catalyst concentrations, 60°C reaction temperature.
Study of effect of type of catalyst on SOME yield reveals that the heterogeneous catalyst
gives better yield as compared to homogeneous catalyst. The separation of heterogeneous
catalyst from crude biodiesel is much easier as compared to homogeneous catalyst. Hence it
is recommended to use heterogeneous catalyst for SOME production.
Performance testing of CI engine with SOME and its Blends with Diesel
The brake specific fuel consumption increased and brake thermal efficiency decreased with
increase in the proportion of biodiesel in the blends.
Among the Soapnut oil methyl ester blends tested, BD5 gave the best performance. The brake
thermal efficiency of the engine with BD10 blend at 100% load was 26.86% which is the
closer to diesel operation. From these findings, it is concluded that Soapnut biodiesel could
be safely blended with diesel up to 5% without significantly affecting the engine performance
(BSFC, BTE,) and thus could be a suitable alternative fuel for diesel. A blend of SOME with
diesel could be used in CI engines in rural areas for agriculture, irrigation and electricity
generation. On the whole, it was observed that engine operation was smooth with SOME and
its blends.
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ent=firefoxb&tbm=isch&tbo=u&source=univ&sa=X&ved=0ahUKEwijjsuX_uLUAhUEr
48KHXy3CrIQ7AkIMQ&biw=1366&bih=659#imgrc=DwLLfcZQ9s314M
Appendix 1
Specifications of the engine
Make and Model Kirloskar, TV1
No. of Cylinders One
Orientation Vertical
Cycle 4 Stroke
Ignition System Compression Ignition
Bore X Stroke 87.5mmX 110mm
Displacement Volume 660 cc
Compression Ration 17: 1
Arrangement of valves Overhead
Combustion Chamber Open Chamber(Direct Injection)
Rated Power 3.5 kW(7 HP) @1500 rpm
Cooling Medium Water cooled

Appendix 2
Specifications of the dynamometer
Make SAJ, Pune
Model ED -1
Type Eddy current

Power 7.5 kW
Volts Max75 V (DC)
Amps 2 A (Max)
Speed 3000 rpm

Appendix 3
Reading Table
Input Data: Inj. Timing: 23°BTDC, Compression ratio: 17, Fuel Used: Diesel
Load (kg) 0 5 10 15
RPM 1534 1491 1467 1448
Manometer (mWC/60) 0.0769 0.0714 0.0684 0.0645
Fuel (kg/hr) 0.3578 0.6134 0.9202 1.0224
EGT (°C) 123 195 275 373
Input Data: Inj. Timing: 23°BTDC, Compression ratio: 17, Fuel Used: B5
Load (kg) 0 5 10 15
RPM 1534 1491 1467 1450
Manometer (mWC/60) 0.0789 0.0731 0.0684 0.0647
Fuel (kg/hr) 0.3578 0.6646 0.9713 1.3802
EGT (°C) 115 194 294 385
Load (kg) 0 5 10 15
RPM 1531 1492 1469 1447
Manometer (mWC/60) 0.0775 0.0714 0.0685 0.0649

Fuel (kg/hr) 0.3578 0.7157 1.0024 1.4314
EGT (°C) 123 216 296 346
Load (kg) 0 5 10 15
RPM 1531 1493 1471 1454
Manometer (mWC/60) 0.0773 0.0724 0.0685 0.0645
Fuel (kg/hr) 0.3578 0.7668 1.0735 1.4825
EGT (°C) 117 212 302 390
Load (kg) 0 5 10 15
RPM 1529 1494 1473 1452
Manometer (mWC/60) 0.0776 0.0725 0.0689 0.0654
Fuel (kg/hr) 0.409 0.7668 1.1246 1.5847
EGT (°C) 121 205 296 388
Important Equations for calculation of performance of CI Engine,
1. Torque (N-m):
T = W x R x 9.81
Where,
W = load in kg
R = Radius of Dynamometer arm length
2. Mean Effective Pressure (bar):
MEP =
Where,
nc = 2 for 4 stroke engines
T = Torque in N-m
Vd = Displacement volume (m3)
3. Brake Power (KW):
B.P =
Where,
N = RPM of engine
T = Torque in N-m
4. Brake Thermal Efficiency (%):
BTE =
BP = brake power in kw
mf = fuel flow rate in kg/sec
Cv = Calorific Value in KJ/kg
5. Specific Fuel Consumption (kg/KWhr):
SFC =
mf = fuel flow rate in kg/hr

BP = brake power in kw
Appendix 4
Result Table
Fuel Used: Diesel
Load RPM Torque (N-m) MEP BP (KW) BTE (%) SFC

(kg) (bar) (kg/KWhr)
0 1534 0 0 0 0 ----
5 1491 9.08 1.724646 1.41772 19.809 0.43269348
10 1467 18.15 3.447392 2.78827 25.973 0.33001095
15 1448 27.22 5.170138 4.12748 34.603 0.24770565
Fuel Used: B5

0 1534 0 0 0 0 -----
5 1491 9.08 1.724646 1.41772 18.286 0.46875127
10 1467 18.15 3.447392 2.78827 24.606 0.3483449
15 1450 27.22 5.170138 4.13318 25.667 0.33394138
Fuel Used: B10

0 1531 0 0 0 0 ----
5 1492 9.08 1.724646 1.41868 16.991 0.50447071
10 1469 18.15 3.447392 2.79207 23.875 0.35901648
15 1447 27.22 5.170138 4.12463 24.7 0.34702757
Fuel Used: B20

0 1531 0 0 0 0 ----
5 1493 9.08 1.724646 1.41963 15.869 0.54014231
10 1471 18.15 3.447392 2.79587 22.323 0.38396584
15 1454 27.22 5.170138 4.14458 23.963 0.35769104
Fuel Used: B30

0 1529 0 0 0 0 ----
5 1494 9.08 1.724646 1.42058 15.879 0.53978077
10 1473 18.15 3.447392 2.79968 21.338 0.40170376
15 1452 27.22 5.170138 4.13888 22.386 0.38288606

Appendix 5
Uncertainty Analysis
The errors associated with various measurements and in calculation of performance

parameters are computed in this section. Mass of fuel consumption and the applied load are
the two measured quantities, where there are chances of error. Mass of fuel consumptions and
the brake are the two calculations from where errors can be reflected to BTE and BSFC. The
accuracy of the instruments used for the measurement of fuel flow and brake are listed below.
Sr. No Measuring Instruments Scale Range Accuracy
1 Fuel Flow Measurements ---- 0.5%
2 Eddy Current Dynamometer 0-20 kg 0.125 kg
Uncertainty Calculations
Standard procedure of uncertainty calculations is adopted for calculations percentage

uncertainty in BTE and BSFC. The governing equations of BTE and BSFC are formulated in
terms of their respective measures. Mass of fuel flow and the load are the two measures,
which are used in the calculations of BTE and BSFC. So, the equations are formed as the
function of time and load.
1. Brake Thermal Efficiency:
BTE = % (1)
Power = watt
The engine set up unit is computerised fuel flow rate is directly generated in data sheet
through transmitters by the data acquisition system in cc/min.
mf = x ρ x 10-6 (2)
Therefore the equation (1) becomes,
BTE = %
Time required for fuel consumption is constant as 60 seconds and the fuel volume is variable
and mf must be in kg/sec (hence mf is divided by 60)
Where,
Constant =
Therefore,
BTE = constant x (3)
Where,
mf = Mass of fuel consumption
CV = Calorific value of fuel
N = Speed of the engine
r = Radius of output shaft
ρ = Density of fuel
W = Load applied
v = per unit fuel flow rate
Now, Uncertainty in BTE by standard deviation is given as,

Uuncertainty = √( ) ( ) (4)
Where,
Percentage Uncertainty is,
U%= x 100, % (5)
dW = Accuracy in measurement of load = 0.125 kg

dv = Accuracy in measurement of fuel flow rate = 0.5% = 0.005
Solving equations (3) and (4) we get uncertainty in BTE. Following tables gives uncertainty
in BTE, percentage.
Table 1 Uncertainty in BTE for single cylinder diesel engine

Fuel Used – Diesel
Load N (rpm) dBTE/dw dBTE/dv U% BTE BTE BTE

(kg) (min) (max)
5 1491 0.04054 -0.01689 0.025589 19.78341 19.809 19.809256
10 1467 0.02659 -0.01478 0.012803 25.9602 25.973 25.973128
15 1448 0.02362 -0.01772 0.008538 34.59446 34.603 34.603085
Fuel Used – SN 5

(kg) (min) (max)
5 1491 0.03751692 -0.01443 0.025649 18.26035 18.286 18.286256
10 1467 0.02525628 -0.01329 0.012832 24.59517 24.608 24.608128
15 1450 0.01756698 -0.00976 0.008557 25.66044 25.669 25.669086
Fuel Based – SN 10

(kg) (min) (max)
5 1492 0.03473495 -0.01241 0.025557 16.96544 16.991 16.991256
10 1469 0.02393965 -0.01197 0.012536 23.86246 23.875 23.875125
15 1447 0.01684366 -0.00902 0.008526 24.69147 24.7 24.700085
Fuel Used – B20

(kg) (min) (max)
5 1493 0.03236332 -0.01079 0.025495 15.84351 15.869 15.869255
10 1471 0.02277602 -0.01085 0.012756 22.31024 22.323 22.323128
15 1454 0.01630238 -0.00843 0.008506 23.95449 23.963 23.963085
Fuel Used – B30

(kg) (min) (max)
5 1494 0.03219223 -0.01073 0.025344 15.85366 15.879 15.879253
10 1473 0.02164072 -0.00984 0.012679 21.32532 21.338 21.338127
15 1452 0.01513898 -0.00733 0.008455 22.37755 22.386 22.386085

2. Brake Specific Fuel Consumption (BSFC)
Likewise, governing equation for BSFC is formulated as below,

We have,
BSFC = (6)
( )
BSFC
Therefore
BSFC (7)
Now, uncertainty in BSFC is given as,
UBSFC = √( ) ( ) (8)
(9)
= (10)
Solving equation (9) and (10), the uncertainty in percentage is given as,
% Uncertainty (BSFC) = x 100 (11)
Table 2 Uncertainty in BSFC for single cylinder diesel engine
Fuel Used – Diesel
Load N dBSFC/dv dBSFC/dw U % BSFC BSFC BSFC

(kg) (rpm) min max
5 1491 1.40596E- -3.3743E- 0.0001 0.432692 0.432693477 0.432695
06 06 62
10 1467 5.3586E-07 -9.6455E- 8.12E- 0.33001 0.330010954 0.330012

07 05
15 1448 4.98523E- -9.0641E- 0.0001 0.247705 0.247705647 0.247707

07 07 01
Fuel Used – SN 5

(kg) (rpm) min max
5 1491 1.52679E- -3.9697E- 0.0001 0.46875 0.4687513 0.468753
06 06 63
10 1467 5.66993E- -1.0773E- 8.14E- 0.348349 0.3483499 0.348351

07 06 05
15 1450 6.73697E- -1.6536E- 0.0001 0.333948 0.3339494 0.33395

07 06 01
Fuel Used – SN 10

(kg) (rpm) min max
5 1492 1.64511E- -4.6063E- 0.0001 0.504469 0.5044707 0.504472
06 06 63
10 1469 5.96739E- -1.1935E- 8.31E- 0.359016 0.3590165 0.359017

07 06 05
15 1447 7.00939E- -1.7842E- 0.0001 0.347027 0.3470276 0.347029

07 06 01
Fuel Used - SN 20

(kg) (rpm) min max
5 1493 1.76567E- -5.297E-06 0.0001 0.540141 0.5401423 0.540144
06 63
10 1471 6.27226E- -1.3172E- 8.17E- 0.383965 0.3839658 0.383967

07 06 05
15 1454 7.24212E- -1.9093E- 0.0001 0.35769 0.357691 0.357692

07 06 01
Fuel Used - SN 30
(kg) (rpm) min max
5 1494 1.77505E- -5.3252E- 0.0001 0.539779 0.5397808 0.539782
06 06 64
10 1473 1.77505E- -1.4523E- 8.22E- 0.401703 0.4017038 0.401705

06 06 05
15 1452 7.79866E- -2.1978E- 9.71E- 0.401703 0.4017038 0.401705

07 06 05
Authors Bio-data
Name Moon Vaibhav Harichandra
Email ID moon.vaibhav878@gmail.com
Contact No. 9975109434/70385458654
Date of Birth 7th April 1989
Branch Thermal and Fluid Engineering
University Dr. Babasaheb Ambedkar Technological University, Lonere
Permanent Address C/O Chandan Wasudeo Gawande, Ward no. 5, Vidyanagri,

Gadchandur, Ta: Korpana, Dist: Chandrapur Maharashtra
Pin 442908

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Optimization of Oil Extraction and Transesterification

Processes and Preliminary Tests on CI Engine with

Under the Guidance of

Department of Mechanical Engineering,

The project report entitled “Optimization of oil extraction and transesterification

Dr. Madhukar S. Tandale Dr. M Sadaiah

I sincerely thanks to Dr. Mudigonda Sadaiah, the Head of Mechanical Engineering

Date: Vaibhav H. Moon

Keywords- Biodiesel, Soapnut, Soapnut oil methyl ester (SOME), Transesterification,

2.4.4.1.2 Acid catalyzed

2.4.4.1.3 Enzyme catalyzed

2.4.4.2 Non catalytic transesterification methods

2.4.4.2.2 Microwave assisted

2.4.4.2.3 Ultrasound assisted

2.5 Review of Oil Extraction and Transesterification Process

3. Oil Extraction and Preparation of Biodiesel

4. Experimental Set-up and Plan of Experiment

Appendix 1 Specifications of the engine

Figure Title Page

2.1 Manual and Automatic oil expeller 12

2.2 Schematic representation of Soxhelet extractor 13

2.3 Process of Enzymatic extraction 14

2.4 Supercritical fluid extraction 15

2.5 Microwave assisted extraction 16

2.6 Process flow chart of non-edible seeds to produce biodiesel 17

2.7 Basic transesterification technology 19

2.8 Transesterification reaction of triglycerides 19

2.9 Mechanism of alkali catalyzed transesterification of vegetable oil 22

2.10 Mechanism of acid catalyzed transesterification 23

2.11 Soapnut seeds and Kernels 34

3.1 Mechanism of transesterification reaction 41

3.2 Experimental Soxhelet extraction unit 42

3.3 Schematic diagram of biodiesel production setup 43

3.4 Biodiesel production set up 43

3.5 Flow chart of biodiesel production from crude Soapnut oil 44

3.6 Settling and Seperation 45

4.1 Schematic of engine set up 47

4.2 Overall view of engine set up 48

5.1 Effect of seeds size on oil yield 54

5.2 Effect of reaction temperature on oil yield 55

5.3 Effect of reaction time on oil yield 56

5.5 Effect of type of solvent on oil yield 57

5.6 Effect of molar ratio on SOME yield (Homogenous catalyst) 58

5.7 Effect of catalyst type on SOME yield (Homogenous catalyst) 59

5.8 Effect of catalyst concentration on SOME yield (Homogenous catalyst) 60

5.9 Effect of reaction temperature on oil yield (Homogenous catalyst) 60

5.10 Effect of molar ratio on SOME yield (Heterogeneous catalyst) 61

5.11 Effect of stirrer speed on SOME yield (Heterogeneous catalyst) 62

5.12 Effect of catalyst concentration on SOME yield (Heterogeneous 63

5.13 Effect of reaction temperature on SOME yield (Heterogeneous 64

5.14 Effect of type of catalyst on SOME yield 64

5.15 Brake thermal efficiency v/s load for various blends 69

5.16 Specific fuel consumption v/s load for different blends 70

2.1 Comparison of the standards for diesel and biodiesel based on 8

2.3 Estimated oil yields of various non-edible vegetable oil resources 11

2.4 Comparison of oil yields between common oil seeds crops 34

2.5 Major fatty acid composition of Soapnut and popular seeds 35

4.2 Comparison of the standards for diesel and biodiesel based on 49