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FACULTY OF ENGINEERING

DEPARTMENT OF CHEMICAL ENGINEERING


FORMULATION OF PERFUME FROM ESSENTIAL OIL
EXTRACTED FROM LEMONGRASS

BY
SSENYUNJA NICHOLAS
14/1/327/D/627

FINAL YEAR PROJECT REPORT SUBMITTED TO THE DEPARTMENT OF


CHEMICAL ENGINEERING IN PARTIAL FULFILLMENT FOR THE
REQUIREMENTS FOR THE AWARD OF THE DEGREE OF BACHELORS OF
ENGINEERING IN CHEMICAL ENGINEERING OF NDEJJE UNIVERSITY

MAY, 2018

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DECLARATION

I SSENYUNJA NICHOLAS hereby declare that the information here in this project
report is full knowledge of my research and it has never been presented to any university
or institution as partial fulfillment for the award of a degree or diploma in any discipline.

Signature: ………………………. Date: …………………………

SSENYUNJA NICHOLAS
14/1/327/D/627

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APPROVAL

I hereby approve that this research report has been done by the mentioned person under
my guidance and in my opinion. This report is sufficient in terms of scope and quality so
it can be reviewed by an academic committee for purpose of assessing the students’
knowledge on final year project research.

Signature………………………. Date……………………………….

Mr. OGWENG GEORGE


PROJECT SUPERVISOR

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ACKNOWLEDGEMENT
Praise God, the most merciful and Compassionate, for giving me the strength in
completing this project.

First and foremost, I would like to express my deepest gratitude to the Faculty of
Engineering under Ndejje university at large for offering me an opportunity to pursue my
course of chemical engineering and to my supervisor Mr. Ogweng George for his tireless
advice, supervision, guidance, assistance and inspiration throughout my project work.

My great thanks and appreciation also goes to lab attendant of chemical engineering
laboratory, Ndejje university Mr. Natumanya Robert for his guidance rendered to me in
the practical work during the course of my project.

Last but not least I will not forget the timely effort and support extended to me by
Guardians Mr. Kaamu Mukasa David and family, not forgetting my grateful friends
Namuddu Cissy, Okello Raphael Obot, and Nabaka Maria Ngonzi for their assistance and
advice rendered to me through my project journey.

For those I have not physically mentioned I will always remain grateful and humbly
honored to extend the same to all, may Almighty bless you all

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DEDICTION
I dedicate this report to GOD Almighty, our creator, our strong pillar, source of
inspiration, wisdom, knowledge and understanding. He has been the source of my
strength throughout this program and on his wing only have I soared

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Table of Contents
DECLARATION......................................................................................................................................... ii
APPROVAL ............................................................................................................................................... iii
ACKNOWLEDGEMENT ......................................................................................................................... iv
DEDICTION ............................................................................................................................................... v
List of tables.............................................................................................................................................. viii
List of figures .............................................................................................................................................. ix
CHAPTER ONE: INTRODUCTION ....................................................................................................... 1
1.1 Background ........................................................................................................................................... 1
1.2 Problem Statement................................................................................................................................ 2
1.3 Objectives............................................................................................................................................... 2
1.3.1 General Objective .......................................................................................................................... 2
1.3.2 Specific Objectives ......................................................................................................................... 2
1.4 Justification ........................................................................................................................................... 2
CHAPTER TWO: LITERATURE REVIEW .......................................................................................... 3
2.1 Introduction ........................................................................................................................................... 3
2.2 Perfume Concentration ........................................................................................................................ 4
2.3 Perfume Notes ....................................................................................................................................... 4
2.3.1 Top Notes ........................................................................................................................................ 4
2.3.2 Middle Notes ................................................................................................................................... 5
2.3.3 Base Notes ....................................................................................................................................... 5
2.4 Sources Perfume.................................................................................................................................... 5
2.4.1 Aromatic sources ............................................................................................................................ 5
2.4.2 Synthetic source ............................................................................................................................. 6
2.4.3 Essential oil source ......................................................................................................................... 6
2.5 Lemongrass............................................................................................................................................ 6
2.5.1 Oil properties.................................................................................................................................. 7
2.5.2 Origin of lemongrass oil ................................................................................................................ 7
2.5.3 Extraction ....................................................................................................................................... 7
2.5.4 Chemical Composition................................................................................................................... 7
2.5.5 Uses of lemongrass oil .................................................................................................................... 7
2.6 Extraction of Essential oil..................................................................................................................... 8
2.6.1 Water Distillation ........................................................................................................................... 8

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2.6.2 Solvent-Extraction ......................................................................................................................... 8
2.6.3 Effleurage........................................................................................................................................ 9
2.6.4 Steam Distillation ........................................................................................................................... 9
2.7 Important Physical and Chemical properties of Essential oils ....................................................... 10
2.7.1 Physical properties ....................................................................................................................... 11
2.7.2 Chemical Constituents of Essential oils ..................................................................................... 11
2.8 Parameters Affecting Yield and Quality of Essential Oils .............................................................. 14
2.8.1 Mode of Distillation...................................................................................................................... 14
2.8.2 Improper Design of Equipment .................................................................................................. 14
2.8.3 Material of Fabrication of Equipment ....................................................................................... 15
2.8.4 Condition of Raw Material.......................................................................................................... 15
2.8.5 Time for Distillation ..................................................................................................................... 15
2.8.6 Loading of Raw Material and Steam Distribution.................................................................... 15
2.8.7 Operating Parameters ................................................................................................................. 16
2.8.8 Condition of Tank and Equipment............................................................................................. 16
2.8.9 Particle Size of the raw material loading to the chamber ........................................................ 16
2.9 Formulation of Perfume ..................................................................................................................... 16
CHAPTER THREE: METHODOLOGY ............................................................................................... 17
3.1 Sample Collection................................................................................................................................ 17
3.2 Sample Preparation ............................................................................................................................ 17
3.4 Oil Extraction Methods ...................................................................................................................... 18
3.4.1 Solvent Extraction Method ......................................................................................................... 18
3.4.2 Water Distillation ......................................................................................................................... 18
3.5 Components of the Water Extraction plant............................................................................ 19
3.5.1 Extraction Chamber ......................................................................................................... 19
3.5.2 Condenser ................................................................................................................................. 19
3.5.3 Separator .................................................................................................................................. 19
3.6 Determination of the Yield of lemongrass oil ................................................................................... 19
3.7 Characterization of Lemongrass Oil ........................................................................................... 20
3.7.1 Physicochemical properties of Lemongrass Oil .................................................................... 20
3.8 Formulation of Perfume ................................................................................................................. 23
CHAPTER FOUR: RESULT AND DISUSSION .................................................................................. 24
4.1 Determination of moisture contents .............................................................................................. 24

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4.2 Percentage yield .............................................................................................................................. 24
4.3 Factors affected the yield of extracted oil ..................................................................................... 25
4.3.1 Effect of extraction time on the yield of extracted oil with water distillation method ....... 25
4.3.2 Effect of particle size on the yield of extracted oil................................................................. 26
4.4 Physical properties .......................................................................................................................... 26
4.4.1 pH determination ..................................................................................................................... 26
4.4.2 Specific gravity determination ................................................................................................ 26
4.4.2 Viscosity determination ........................................................................................................... 26
4.4.3 Boiling point of lemongrass oil ................................................................................................ 27
4.4.4 Evaporation residue of lemongrass oil ................................................................................... 27
4.4.5 Flash point determination ................................................................................................ 27
4.4.6 Solubility of lemongrass oil ..................................................................................................... 27
4.5 Quality evaluation of the lemongrass oil ....................................................................................... 28
4.5.1 Acid value determination ........................................................................................................ 28
4.5.2 Saponification value determination ........................................................................................ 29
4.5.3 Iodine number determination ................................................................................................. 29
4.6 Formulated perfume ....................................................................................................................... 30
CHAPTER FIVE: CONCLUSION AND RECOMANDATION ......................................................... 31
5.1 Conclusion ........................................................................................................................................... 31
5.2 Recommendation................................................................................................................................. 31
References ................................................................................................................................................... 32
Appendix ................................................................................................................................................ 34

List of tables
Table 1: Perfume concentration fragrance ..................................................................................... 4
Table 2: Moisture content determination of lemongrass leaves ................................................. 24
Table 3: Yield percentage from oil extraction methods ............................................................... 24
Table 4: Value and unit of physical properties of lemongrass oil................................................. 28
Table 5: Chemical properties of lemongrass oil ........................................................................... 29

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List of figures
Figure 4.1: Effect of time on the yield of extracted oil with water distillation method ............... 25
Figure 4.2: Effect of time on the yield of extracted oil with solvent extraction method ............. 25
Figure 4.3: Effect of particle size on the yield of extracted oil .................................................... 26

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ABSTRACT

Perfume extraction refer to the extraction of aromatic compounds from raw materials, using

method such as distillation, solvent extraction, expression or effleurage. The extracts are either

essential oils, absolutes, concretes, or butters, depending on the amount of waxes in the extracted

product. Heat, chemical solvents, or exposure to oxygen in the extraction process denature the

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aromatic compounds, either changing their odor, character or rendering them odorless. In this

project water distillation and solvent extraction were used to extract essential oils from

lemongrass, 0.67% and 1.22% of essential oil respectively was produced. The extracted essential

oil was formulated into perfume using a fixative and carrier solvent.

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CHAPTER ONE: INTRODUCTION

1.1 Background
Perfume is a fragrant liquid made from an extract that has been distilled in alcohol and water.

The term perfume comes from the Latin word "per" meaning "through" and "fume," or "smoke."
Many ancient perfumes were made by extracting natural oils from plants through pressing and
steaming. The oil was then burnt to scent the air.

Making of perfume involves three key ingredients; essential oils, pure grain oil and water.
Techniques involved in perfume extraction from plants include; solvent extraction, steam
distillation and effleurage method. These methods tend distort the odor of the aromatic
compounds that are obtained.

Perfume can be formulated from essential oil extracted from many plant species such as
lemongrass, cocoa nut, groundnuts, eucalyptus and some species are mainly cultivated as
culinary and medicinal herbs because of their scent. Lemongrass essential oil is extracted from
Cymbopogon citratus of the Poaceae family. (M.A.Suryawanshi, 2016)

Perfume is categorized into two groups; pure perfume (any fragrance derived completely from
processed natural material like raw fruits, flowers, leaves, seeds, roots, without any artificial
components), and synthetic perfume (derive from artificial compound and materials belong to a
family of chemicals called petrochemical obtained from petroleum and natural gas). (Anne
Marie, 2007).

According to a study conducted by the environmental working group showed that, the perfume
industry employs over 3100 combination of synthetic compounds, with an average 29 perfume
sporting chemicals, half of which are not included on the ingredient label, some artificial
ingredients are not present in the umbilical cord blood of a newborn babies (Anne Marie, 2007).
This means that mothers wearing certain scent are actually passing toxins onto their children and
this can be linked to many allergic reaction, such as eczema, asthma attacks, disruption in
hormone and suppress the immune system. Unless someone happen to be allergic to one of the
ingredients, but all pure perfumes, made properly with essential oils, have no associated health
risk or negative side effects. (Anne Marie, 2007)

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1.2 Problem Statement
Majority of synthetic compounds used in formulation of perfume belong to a chemical family
called petrochemical derived from petroleum and natural gases. These have been linked to many
allergic reactions, such as eczema, asthma attacks, and disruption in hormone and suppress the
immune system (Anne Marie, 2007). This creates carcinogen which involve in the formation of
cancerous cell. According to the EU’s scientific committee on cosmetic products, 2% of people
suffer an allergic reaction in response to a synthetic fragrance. The abundant availability of
lemongrass in the country, it can also lay down a foundation for small-scale industries (Green,
june 1991).

1.3 Objectives
1.3.1 General Objective
To formulate perfume from essential oils extracted from lemongrass (CYMBOPOGON
FLEXUOSUS).

1.3.2 Specific Objectives


To extract essential oil from lemongrass (cymbopogon flexuosus).

To investigate the properties of extracted essential oils.

To formulate perfume from essential oils extracted.

1.4 Justification
The study will not only be stretching the limit of the resources by using lemongrass for other
purpose but also there will be production of a product that is commercially viable for places
where lemongrasses are cultivated in large quantities as weeds.

The success of this work will stimulate the development of the perfume industry locally because
of available cheap raw materials, hence job creation for those that will be engaged in
planting/cultivation of the lemongrass. This will lead reduction on the resources spent on
importation of lemongrass fragrance by end users.

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CHAPTER TWO: LITERATURE REVIEW

2.1 Introduction
Perfume is a mixture of fragrant essential oils or aroma compounds, fixatives and solvents used
to give human body, animal, food, and living space a pleasant scent.

Perfume was first used in Egypt, where Egyptians used it as a part religious ceremonies or burial
preparation and even in daily wear, they were more than 4000 years old. Cuneiform tablet from
mesopomia, dating back more than 3000 (Nyssen, 2009)

The earliest use of perfume battle is Egyptian and dates to around 1000 BC. The Egyptians
invented glass and perfume battles were one of the first common uses forms.

Persians and Arab chemist introduced the process of extracting oils from flowers by means of
distillation, the procedure most commonly used today. They first experimented with the rose.
Until his discovery, liquid perfumes consisted of mixtures of oil and crushed herbs or petals,
which made a strong blend. Rose water was more delicate, and immediately became popular.
Both the raw ingredients and the distillation technology significantly influenced western
perfumery and scientific developments, particularly chemistry (Al-Hassani, 2006).

The rise of Christianity however saw a decline in the uses of perfume much of the dark ages. It
was the world that kept the traditions of perfume alive during that time. According to the Book of
(Ullmann, 1986), written by Arab chemist (Al-Kindi) which contained more than a hundred
recipes for fragrant oils, salves, aromatic waters, and substitutes or imitations of costly drugs.
The book also described 107 methods and recipes for perfume-making and perfume-making
equipment, such as the alembic

The 16th century saw the popularity of perfume explode in France, especially among the upper
classes and nobles. Partly due to this patronage, the perfume industry developed. In 1693, Italian
barber Giovanni Paolo Feminis created a perfume water called Aqua Admirabilis, today best
known as eau de cologne (Wiedemann & Plessner, 1986)

With help from the perfume court, the court of Louis xv everything got perfumed say furniture,
gloves and other clothing.

The 18th century invention of eau de cologne helped the perfume industry to continue growing.

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2.2 Perfume Concentration
The perfume concentration depends on the percentage concentration of fragrance and this comes
in four levels of concentration. (Eau de cologne, eau de toilette, eau de parfum and parfum).

As the percentage of the aromatic compound decreases, so does the intensity and longevity of the
scent created. Different perfumeries of houses assign different amount oils to each of their
perfumes. Therefore, although the oil concentration of some perfumes dilution will be higher
than others like (eau de parfum EDP and eau de toilette EDT) form within the same range, the
actual amount can vary between perfume houses. In EDT from one house may be stronger than
EDP from other (Onyinyechi, 2012).

Table 1: Perfume concentration fragrance


Fragrance % aromatic compound Last time (hrs.)
Perfume extract 20-50 24
Eau de parfum 10-30 6
Eau de toilette 5-20 2-3
Eau de cologne 2-5 2

2.3 Perfume Notes


Perfume can be described in a musical metaphor as having three notes, making the harmonious
chord of the scent. The notes unfold overtime, with the immediate impression of the top note
leading to the deeper middle notes and the base notes gradually appearing as the final stage.
These notes are created carefully with the knowledge of the evaporation process of the perfume
(Lord, 1992).

2.3.1 Top Notes

The scents that are perceived immediately on application of a perfume. Top notes consist of
small light molecules that evaporate quickly. They form a person’s initial impression of perfume
and thus are very important in the selling of a perfume. The compounds that contribute to top
notes are strong in scent, very volatile, and evaporate quickly. Citrus and ginger scents are
common top notes. They are also called the notes usually last about five minutes.

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2.3.2 Middle Notes
The scent of the perfume that emerge after the top notes dissipate. The middle note s compounds
form the heart of perfume and are usually more mellow and rounded. Lavender and rose scent
are typically middle notes they are also called the heart notes and typically last about 10 to 60
minutes.

As a fragrance is more volatile components the top notes and middle notes evaporate the end
notes linger and carry the body of the fragrance.

All fragrances change as they dry down, and all fragrances are affected by each person’s unique
skin chemistry but the fragrance should remain true in character. Perfume use fixative (aromatic
ingredients that fix or prolong scent) in the perfume to ensure a scent longevity.

2.3.3 Base Notes


The scent of a perfume that appears after the departure of the middle notes. The base and middle
notes together are the main theme of perfume. Base notes bring depth and solidity to a perfume
and consist of large, heavy molecules that evaporate slowly. Compounds of this class of scent are
typically rich and deep and are usually not perceived until 30 minutes after the application of the
perfume or during the period of perfume dry down.

2.4 Sources Perfume


2.4.1 Aromatic sources
These mainly obtain from plant parts like flowers roots leaves and many others. They have been
in perfumery as a source of essential oil and aroma compounds. These aromatic compounds are
usually secondary metabolites produced by plants as protection against herbivores, infections, as
well as attract pollinators.

These sources may be derived from various parts of plants. A plant can offer more than one
source of aromatics for instance the aerial portions and seed of coriander from each other.
Orange leaves blossoms and fruit zest is the respective source of pettigram, neroil and orange
oils.

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2.4.2 Synthetic source
Many modern perfumes contain synthesized odorants. Synthetic can provide fragrance which is
found in nature. For instance, calone. A compound of synthetic origin imparts a fresh ozonous
metallic marine scent that is widely used in contemporary perfumer.

Synthetic aromatic is often used as an attractive source of compound that are not easily obtained
from and natural source. For example, linolool and coumarine are both naturally occurring
compounds that can be inexpensively synthesized from terpenes.

Orchid scent is usually not obtained directly from the plants itself but is instead synthetically
created to match the fragrance compound found in various orchids (J. Behboud, 2012).

2.4.3 Essential oil source


An essential oil is a concentrated, hydrophobic liquid containing volatile aroma compounds from
plants. Essential oils are also known as volatile, ethereal oils or aetherolea, or simply as the "oil
of" the plant from which they were extracted, such as oil of clove. Oil is "essential" in the sense
that it carries a distinctive scent, or essence, of the plant.

Essential oils are frequently referred to as the “life force” of plants. These "essential" oils are
extracted from flowers, leaves, stems, roots, seeds, bark, and fruit rinds. The amount of essential
oils found in these plants can be anywhere from 0.01 percent to 10 percent of the total. These oils
have potent antimicrobial factors, having wide range of therapeutic constituents. These oils are
often used for their flavor and their therapeutic or odoriferous properties, in a wide selection of
products such as foods, medicine, and cosmetics. Only pure oils contain a full spectrum of
compounds that cheap imitations simply cannot duplicate (Asaad A., 2014 ).

2.5 Lemongrass
Lemongrass is also known as cymbopogon which is a genus of Asian, African, Australian, and
tropical island plant in the grass family (Onyinyechi, 2012). Some species are mainly cultivated
as culinary and medicinal herbs because of their scent, resembling that of lemon (citrus linon).

Lemongrass essential oil is extracted from Cymbopogon citratus of the Poaceae family. It is
fresh smelling oil that can be used with success for fighting jet lag, cellulite, revitalizing a tired
body and mind, as well as keeping the family pet free of fleas and ticks.

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2.5.1 Oil properties
Lemongrass oil has a lemony, sweet smell and is dark yellow to amber and reddish in color, with
a watery viscosity.

2.5.2 Origin of lemongrass oil


It is a perennial fast-growing aromatic grass, growing to about 1 meter (3 feet) high with long,
thin leaves and originally was growing wild in India. It produces a network of roots and rootlets
that rapidly exhaust the soil (Esoteric oil ltd, 1998 - 2017).

In India it is known as 'choomana poolu' and is also referred to as 'Indian Verbena' or 'Indian
Melissa oil' and used in Ayurvedic medicine to help bring down fevers and treat infectious
illnesses. It is a valuable ingredient in perfumes and citrus-type soaps and is also an insect
deterrent.

2.5.3 Extraction
Lemongrass oil is extracted from the fresh or partly dried leaves by steam distillation, solvent
extraction, and influenza.

2.5.4 Chemical Composition


The main chemical components of lemongrass oil are myrcene, citronellal, geranyl acetate, nerol,
geraniol, neral and traces of limonene and citral. (N. E. Tajidin, 2012)

2.5.5 Uses of lemongrass oil


Lemongrass oil revitalizes the body and relieves the symptoms of jetlag, clears headaches and
helps to combat nervous exhaustion and stress-related conditions.

Lemongrass oil is a great overall tonic for the body and boosts the parasympathetic nervous
system, which is a boon when recovering from illness, as it also stimulates glandular secretions.

Lemongrass oil is useful with respiratory infections such as sore throats, laryngitis and fever and
helps prevent spreading of infectious diseases, and also helpful with colitis, indigestion and
gastro-enteritis.

Lemongrass oil helps tone the muscles and tissue, relieves muscle pains by making the muscle
suppler, correcting poor circulation and as an insect repellant and helps to keep pets clean of
fleas, ticks and lice.

Lemongrass oil is also used for clearing up oily skin and acne, as well as athlete's foot.

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2.6 Extraction of Essential oil
2.6.1 Water Distillation
In the manufacture of essential oils using the method of water distillation, the botanic material is
completely immersed in water and the still is brought to the boil. The main characteristic of this
process is that there is direct contact between boiling water and plant material. Distillation offers
better conditions for the osmosis of oil, because the higher temperature and the movement of
water, caused by temperature and pressure fluctuations within the still, accelerate the forces of
diffusion to such a point that all the volatile oil contained within the plant tissue can be collected.
A special case of water distillation it uses the practice of returning the distillate water to the still
after the oil has been separated from it so that it can be re-boiled. The principal behind it is to
minimize the losses of oxygenated components. Practical advantages of water distillation are that
the stills are inexpensive, easy to construct and suitable for field operation. These are still widely
used with portable equipment in many countries. This method protects the oils so extracted to a
certain degree since the surrounding water acts as a barrier to prevent it from overheating
(Basma A. Abdul-Majeed, (June 2013)).

2.6.2 Solvent-Extraction
In the Solvent-Extraction method of Essential Oils recovery, an extracting unit is loaded with
perforated trays of essential oil plant material and repeatedly washed with the solvent. A
hydrocarbon solvent is used for extraction. All the extractable material from the plant is
dissolved in the solvent. This includes highly volatile aroma molecules as well as non-aroma
waxes and pigments. The extract is distilled to recover the solvent for future use. The waxy mass
that remains is known as the concrete. The concentrated concretes are further processed to
remove the waxy materials which dilute the pure essential oil. To prepare the absolute from the
concrete, the waxy concrete is warmed and stirred with alcohol (ethanol). During the heating and
stirring process the concrete breaks up into minute globules. Since the aroma molecules are more
soluble in alcohol than the waxes, an efficient separation of the two results. This is not
considered the best method for extraction as the solvents can leave a small amount of residue
behind which could cause allergies and effect the immune system (Pandey D, 2007).

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2.6.3 Effleurage
This is one of the traditional ways of extracting oil from flowers. The process involves layering
fat over the flower petals. After the fat has absorbed the essential oils, alcohol is used to separate
and extract the oils from the fat. The alcohol is then evaporated and the Essential Oil is collected
(Trieste, 2008).
2.6.4 Steam Distillation
Steam distillation is a special type of distillation or a separation process for temperature sensitive
materials like oils, resins, hydrocarbons, etc. which are insoluble in water and may decompose at
their boiling point. The fundamental nature of steam distillation is that it enables a compound or
mixture of compounds to be distilled at a temperature substantially below that of the boiling
point(s) of the individual constituent(s). Essential oils contain substances with boiling points up
to 200 or higher temperatures (Pandey D, 2007). In the presence of steam or boiling water,
however, these substances are volatilized at a temperature close to 100, at atmospheric pressure.
Fresh, or sometimes dried, botanical material is placed in the plant chamber of the still and the
steam is allowing to pass through the herb material under pressure which softens the cells and
allows the essential oil to escape in vapor form. The temperature of the steam must be high
enough to vaporize the oil present, yet not so high that it destroys the plants or burns the essential
Oils. Besides the steam tiny droplets of essential Oil evaporates and travel through a tube into the
still's condensation chamber. Here Essential Oil vapors condense with the steam (Kabuba
Tshilenge John, 2009).
The essential oil forms a film on the surface of the water. To separate the Essential Oil from the
water, the film is then decanted or skimmed off the top. The remaining water, a byproduct of
distillation, is called floral water, distillate, or hydrosol. It retains many of the therapeutic
properties of the plant, making it valuable in skin care for facial mists and toners (A solution
containing chemicals that can change the color of a photographic print). In certain situations,
floral water may be preferable to be pure essential oil, such as when treating a sensitive
individual or a child, or when a more diluted treatment is required. Rose hydrosol, for example,
is commonly used for its mild antiseptic and soothing properties, as well as its pleasing floral
aroma (Satish, 2010).
A number of factors determine the final quality of a steam distilled essential oil. Apart from the
plant material, most important are time, temperature and pressure, and the quality of the
distillation equipment. Essential oils are very complex products. Each is made up of many,

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sometimes hundreds, of distinct molecules which come together to form the oil's aroma and
therapeutic properties. Some of these molecules are fairly delicate structures which can be
altered or destroyed by adverse environmental conditions. So, much like a fine meal is more
flavorful when made with patience, most oils benefit from a long, slow 'cooking' process.
It is possible that longer distillation times may give more complete oil. It is also possible
however, that longer distillation time may lead to the accumulation of more artifacts than normal.
This may have a curious effect of appearing to improving the odor, as sometimes when materials
that have a larger number of components are sniffed, the perception is often of slightly increased
sophistication, added fullness and character, and possibly, and extra pleasantness (Satish, 2010).

2.7 Important Physical and Chemical properties of Essential oils


The chemical properties of essential oils depend on the natural factors such as type of species,
the geographical origin and location of the plant, time of harvesting, plant parts from which the
oils are extracted, (Pant Chaitanya, 2011)
Essential oils component and percentage are different from oil to oil even for the same botanic
plant due to:

 Weather and planting time


Most of herbs are planted but small amount could also be wild grown or collected plants. By
means of example with spearmint, the oil percentage from a summer crop is double that from a
winter crop. The oil percentage from a given summer plant could be different from a previous
summer even from the same filed. The compound analysis of the oil could also be different from
one season to another,
 Soil elements
The B-phellanderene percentage increases in marjoram oil with the higher level of molybdenum
manganese, copper, calcium, zinc or iron in the soil.
 Irrigation
The highest yield of plant material results from increasing the leaf area. For example, this will
happen if a basil field is irrigated every 4 days. The essential oil is highest at medium level of
soil moisture.

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 Time of harvest
The peppermint oil yield increases as the herb approaches in the full bloom stage.
2.7.1 Physical properties
 Specific gravity
Specific gravity is an important criterion of the quality and purity of an essential oil. Values for
essential oils vary between the limits of 0.696 and 1.188 at 15 °C, in general, the specific gravity
is less than 1.000 (Guenther, 1960). Hence essential oil can be collected over (floating on) water.
 Solubility
Solubility in alcohol
Most essential oils are miscible with absolute alcohol. The solubility of oil may change with age.
Solubility in water
Most of essential oils of commercial interest are steam volatile, reasonably stable to action of
heat and practically insoluble in water and hence suitable for processing by steam distillation.
 Boiling range
In the case of isolates and synthetics, the boiling range is an important criterion of purity.
 Evaporation residue
An important criterion of purity is the evaporation residue; i.e., the percentage of the oil which is
not volatile at 100. It is important to study the odor of oil as it volatilizes during the heating.
 Flash point
The flash point may prove useful in the valuation of an essential oil. The flash point has value as
an indication of adulteration: additions of adulterants such as alcohol and low boiling mineral
spirits will greatly lower the flash point.
2.7.2 Chemical Constituents of Essential oils
Essential oil components are divided into terpenoids and non-terpenoids.
i. Non-terpenoids: This group contains short-chain aliphatic substances, aromatic
substances, nitrogenized substances, and substances with Sulphur. They are less
important than terpenoids in terms of uses and applications.
ii. Terpenoids: These are more important commercially and in terms of their properties.
Terpenes derive from isoprene units (C5) bonded in a chain. Terpenes are a type of
chemical substance found in essential oils, resins, and other aromatic plant substances,
(pines, citrus fruit). They are usually found in monoterpene oils (C15) and diterpenes
(C20). They may be aliphatic, cyclic, or aromatic (G. K. Oloyede, 2010).
11
According to their function group they can be:
 Alcohols (menthol, bisabolol) and phenols (timol, carvacrol)
 Aldehydes (geranial, citral) and cetones (camphor, thuyone)
 Esthers (bornile acetate, linalile acetate, methyl salicilate, anti-inflammatory compound
similar to aspirin)
 Ethers (1.8 - cineol) and peroxides (ascaridol)
 Hydrocarbons (limonene, pinene α and ß)
a) Monoterpenic hydrocarbons
These are the commonest compounds in essential oils, and precursors of the more complex
oxidized terpenes. Their names end in –ene. Limonene, for example, is the precursor to the main
components of mint essences (Mentha spp, Lamiaceae Family) such as carvone and menthol.
Limonene is also found in citric plants and in dill (Anethum graveolens, Apiaceae family).
Pinene α and ß are also widely present in nature, especially in trementine essence of the Pinus
genre (Pinaceae family).
b) Alcohols
Alcohols have the hydroxyl group (OH) bonded to a C10 skeleton. Their names end in –ol. They
are highly sought after for their aroma.

Linalool, for example, has two forms. R-linalool is found in roses and lavender and is the main
component of Mentha arvensis. S-linalool found in lavender oil at > 5% indicates adulteration.
Linalool gives tea, thyme, and cardamom leaves their taste. Menthol, another compound found in
this group, is responsible for the smell and taste of mint. Mint essence may contain up to 50% of
this component.
Geraniol, from scented geraniums (Pelargonium spp), citronelol, from roses (Rosa gallica),
borneol from rosemary, and santalol from sandalwood (Santalum album, Santalaceae family).

c) Aldehydes

12
Aldehydes are highly reactive compounds. Their names end in –al. Many of them, such as those
found in citrus fruits, match their respective alcohol. For example: geraniol – geranial, and
citronelol – citronelal. They are found in abundance in citrus plants, and are responsible for their
characteristic smell, particularly the isomers geranial (a citral) and neral (ß citral) known as citral
in combination. In addition to its characteristic aroma, citral has anti-viral, antimicrobiotic, and
sedative properties. But many aldehydes, including citral, cause irritation to the skin and cannot
be used externally. Another important group is the aromatic aldehydes, such as benzaldehyde,
main ingredient of bitter almond oil and cause of their typical aroma.
d) Phenols
They are only found in a few species but are very powerful and irritating. The most important are
timol and carvacrol, which are found in thyme (Thymus) and oregano (Origanus), both of the
Labiatae family. Another important phenol is eugenol, which is found in many species, for
example, clove essence. It is both a powerful bactericide and also anaesthetic, and is used in
dentistry.
e) Phenolic Ethers
These are the main components of species such as celery and parsley (apiol), aniseed (anetol),
basil (metilchavicol), and estragon (estragol). Safrol is a component which is used extensively in
the perfume industry and is found in the bark of the sassafras tree (Sassafras albidum Lauraceae
family).
f) Ketones
These are produced by the oxidisation of alcohols and are fairly stable molecules. They end in
one. Carvone is found in Mentha spicata. Tuyone -first isolated in Tuya- (Thuja occidentalis
Cupressaceae family) and pulegone are fairly toxic and should never be used during pregnancy.
Tuyone is found in plants of the Artemisia genus (Artemisia absinthium with which absinthe and
vermouth are made), and in salvia (Salvia officinalis). Pulegona was first isolated in Mentha
pulegium.
g) Ethers
Ethers or monoterpenic oxides are reactive and unstable. One example is bisabolol oxide found
in camomile (Matricaria chamomilla). Another common ether is 1.8 –cineol (also known as
eucaliptol), which is the main component of eucalyptus oil. It is an expectorant and mucolitic,
and the main component of cough medicines. The aroma of eucalyptus oil varies depending on

13
1.8 –cineol content: the oil with a high content (Eucalptus globulus) is used for medicinal
purposes, whereas that with a lower content (Eucaliptus radiata) is used in aromatherapy.
h) Esters
Most esters are formed from a reaction of a terpenic alcohol with an acetic acid. Their aroma is
characteristic of the oils in which they are found. Lavender oil, for example, contains linalool in
its Esther, linalile acetate. The relative abundance of both these components is a sign of good
quality. Methyl salicilate, a derivate of salicylic acid and methanol, is an anti-inflammatory
compound similar to aspirin and is found in a certain type of heather (Gaultheria procumbens
Ericaceae family). It is used externally in liniments (Onyinyechi, 2012).

2.8 Parameters Affecting Yield and Quality of Essential Oils


The yield and quality of essential oil is affected by the various process parameters. It is advisable
to keep them in mind while designing such systems. Some of the important parameters are being
listed below.
2.8.1 Mode of Distillation
The technique for distillation should be chosen considering the boiling point of the essential oil
and the nature of the herb, as the heat content and temperature of steam can alter the distillation
characteristics. For high boiling oils such as woody oils (e.g. sandalwood, cedar wood) and roots
(e.g. Cyperus), the oil should be extracted using boiler-operated steam distillation. Since the heat
content and temperature of steam depend upon its pressure, a change in steam pressure can alter
the distillation characteristics. High-boiling constituents of essential oils normally require high
pressure steam to distill over. For oil of rose and other florals, the material is generally immersed
in water, i.e. Hydro distillation, as flowers tend to aggregate and form lumps which cannot be
distilled using water and steam distillation or direct steam distillation.
2.8.2 Improper Design of Equipment
Improper designing of tank, condenser or separators can lead to loss of oil and high capital
investments. The design of the furnace and chimney affects the firing and heat control of the
distillation rates. Tank height: diameter ratio is important. Similarly, the use of a condenser with
an improper design and without calculating the heat transfer areas based on the steam generation
areas will lead to improper condensation and loss of oil.

14
2.8.3 Material of Fabrication of Equipment
Essential oils which are corrosive in nature should be preferably distilled in stills made of
resistant materials like aluminum, copper or stainless steel. The tank still can be made from a
cheaper metal like mild steel or galvanized iron, and the condenser and separator can be made
from a resistant material like stainless steel. As only vapor is present in the tank still, the rust and
other products of corrosion may not be carried over into the oil. This can result in considerable
savings in the capital cost of the equipment. Expensive, high-value essential oils like rose,
agarwood, kewda, sandalwood and lavender should be distilled in stainless steel systems.
Although copper was the most common material of fabrication of distillation stills since ancient
times, its availability is getting reduced and with the arrival of superior alloys like stainless steel,
it is slowly disappearing from the scene.
2.8.4 Condition of Raw Material
The condition of the raw material is important because some materials like roots and seeds will
not yield essential oil easily if distilled in their natural state. These materials have to be crushed,
powdered or soaked in water to expose their oil cells. Chopping of plants will also change the
packing density of the material when placed in the distillation still. One can pack up to 50%
more plant material in the same still after chopping of some aromatic herbs like mint. Air drying
and wilting the herb prior to distillation also has considerable effect on distillation. If required,
drying of the herbs prior to distillation should be done in shaded areas and the dried material
should not be kept in heaps.
2.8.5 Time for Distillation
Different constituents of the essential oil get distilled in the order of their boiling points. Thus,
the highest boiling fractions will be last to come over when, generally, very little oil is distilling.
If the distillation is terminated too soon, the high-boiling constituents will be lost. In many
aromatic plants, like vetiver, patchouli, chamomile, sandalwood and agarwood, these high
boiling fractions are valuable due to the quality of their aromas. Thus, the time of distillation
must be chosen with due care.
2.8.6 Loading of Raw Material and Steam Distribution
Improper loading of the herb may result in steam channeling, causing incomplete distillation.
The herb should be evenly and uniformly loaded in the tank without leaving any voids.
Excessive filling of plant material may also lead to formation of “rat holes” which may allow
steam to escape without vaporizing the oil. For powdered herbs, a proper stainless steel wire

15
mesh or muslin cloth should be put at the false bottom to prevent plant material from falling into
the tank base.
2.8.7 Operating Parameters
Proper control of injection rates and pressure in boiler-operated units is necessary to optimize the
temperature of extraction for maximal yield. Generally, high-pressure steam is not advisable for
the distillation of essential oils. The temperature of the condensate should not be high, as it can
result in oil loss due to evaporation. In directly fired-type FDUs, the firing of the furnace should
be well controlled as it can result in high flow rates and high condensate temperatures.
2.8.8 Condition of Tank and Equipment
The tank and other equipment should not be rusted. If rusted, the tank should be cleaned with
dilute caustic solutions. The perforated grids should not be corroded or have large gaps
permitting the plant material to settle to the bottom of the tank and emit a burnt odor. The
distillation tanks should be well steamed prior to distillation for multiple crop distillation
(Kabuba Tshilenge John, 2009)
2.8.9 Particle Size of the raw material loading to the chamber
The size of the leaves has its own contribution on the yield of the extract oil. The particle size
should be optimum in order to steam is distributed properly trough the chamber.

2.9 Formulation of Perfume


This explains why perfume formulation corresponds in fact to a conversation, interplay between
synthetic and natural perfumery materials. A natural raw material carries single information, and
usually is very linear. Its smell is uniform, clear, and faithful. Natural raw materials, on the
contrary, provide a strong, complex and generous image. While a synthetic material can be seen
as a single word.

To formulate a perfume is not to create a culinary recipe, with only dosing the ingredients in
well-balanced amounts, it rather means to flexibly knit materials together with a lively stitch,
meeting or repelling each other, building a pleasant form, which is neither fixed, nor solid, nor
rigid. A fragrance has an overall structure, which ranges from a clear sound, made up of stable,
unique, and linear items, to a background chat, comfortable and reassuring. But that does, of
course, not mean that there is only one way of creating a fragrance (Onyinyechi, 2012).

16
CHAPTER THREE: METHODOLOGY
The experimental work was done in the Chemical Engineering Laboratory of Ndejje University

3.1 Sample Collection


5kg of lemongrass leaves (Cymbopogon Citratus) were collected from Ndejje University
agricultural garden in the morning of the day, due the volatility of the aromatic compound in the
lemongrass leaves (Onyinyechi, 2012). This was because of the nature of conservation of the
garden. The leaves were then taken to the Chemical Engineering Laboratory of Ndejje
University.

3.2 Sample Preparation


The lemongrass leaves were cut freshly, with 5cm height from the root, in the morning of the
day, due to the high volatility of the components in the lemongrass (Cymbopogon Citratus), the
percentage essential oil yield for the partially dried leaves was found to be higher than that of the
fresh leaves (Onyinyechi, 2012). Thus, after collecting, the plant material were partially dried at
room temperature for maximum 4 days, then kept in a sealed plastic bag at ambient temperature
and protected from the light (Kidane, 2016). The lemongrass leaves (Cymbopogon Citratus)
were reduced in size by using a knife since extraction yield increase by decreasing the particle
size due to the higher amount of oil released as the leaves cells are destroyed as sizes are being
reduced. In order to improve the collection efficiency, the plant material was then soaked in
distilled water for 30min before the extraction performed.

3.3 Sample Analysis


3.3.1 Moisture Content determination
Different weights of the lemongrass leave (Cymbopogon Citratus) were weighed and dried in an
oven at 1030C, the weights of the leaves were measured and recorded for every after 2 hours.
The procedure was done repeatedly until a constant weight was obtained. The percentage
moisture in the leaves was calculated using the following formula:

𝑤1 − 𝑤2
𝑀𝑜𝑖𝑠𝑡𝑢𝑟𝑒 % = × 100
𝑤1

Where: w1 is original weight of the sample before drying; and w2 is weight of the sample after
drying.

17
3.3.2 Size Reduction and Sieve Analysis of the leaves

The moisture was removed by partial drying. The dried lemongrass leaves were crushed using
mortar for size reduction. The sample was sieved using set of sieves sizes arranged in descending
order 5mm, 8mm, 12.5mm and 20mm to obtain particular sizes of 5- 8mm, 8- 12.5mm and 12.5-
20mm. This was aimed to investigate the effect of particles size on yield.

3.4 Oil Extraction Methods


3.4.1 Solvent Extraction Method
300g of the dry sample of lemongrass (Cymbopogon Citratus) were weighed from the sliced
lemongrass sample and placed in a clean flat bottomed flask. 700ml of N-hexane solvent were
poured into the flask. The flask and content were allowed to stand for 36 hours (Pandey D,
2007), this was done to extract all the oil content in the lemongrass and for complete extraction.
After which the extract was decanted into another beaker. 250ml of ethanol were added to extract
the essential oil since essential oil is soluble in ethanol. The mixture was then transferred to
100ml separating funnel and separated by a process called liquid-liquid separation process. The
content of the separating funnel was allowed to come to equilibrium, which separated into two
layer (depending on different density). The lower ethanol extract and the upper hexane layer
were collected into two separate 250ml beaker and were placed in a water bath at 780C. This was
done to remove the ethanol leaving only the natural essential oil (Pandey D, 2007). The yield of
oil was determined by weighing the extract on an electronic weighing balance. The different
between the final weight of the beaker with extract and the initial weight of the empty beaker
gave the weight oil essential oil.

3.4.2 Water Distillation


300g of fresh leaves of lemongrass (Cymbopogon Citratus) were placed into a necked round
extraction flask and soaked with 700ml of water. The flask was fitted with a rubber stopper
connected to a condenser and heated using heating hot plate. Water and leaves, were mixed and
allowed to boil. Water and extracted lemongrass oil evaporated. The water at 00C flowed counter
currently through the condenser to condense the ensuring steam. When the lemongrass
(Cymbopogon Citratus) got heated up, the essential oil that was extracted from the leaves mixed
with the water vapor. Both passed through the condenser and the vapor was condensed into
liquid. With the use of cold water, cooling was made possible and volatilization of the essential
oil was avoided. The condensate was directly collected using a 500ml beaker and the poured into
18
a separating funnel. This formed two layers of oil and water. The tap of the separating funnel
was opened to let out the water while the oil was immediately collected into a 100ml stoppered
bottle. The bottle was closed tightly to prevent vaporization of the essential oil. The oil was
collected and the volume of oil obtained was weighed. (Basma A. Abdul-Majeed, (June 2013))

3.5 Components of the Water Extraction plant


3.5.1 Extraction Chamber
This served primary as a container and as a vessel in which the water contacts the plant material
and vaporize its oil. The plant material was packed in the extraction chamber so that distillation
commences. Proper charging was very important otherwise the steam channel through the plant
material and low yield results. The first load was contact to the set-up and establishes the
determine processing parameters.

3.5.2 Condenser
A counter-current flow condenser was used to convert all the steam and the accompanying oil
vapors from the extraction chamber into liquid. Water was feed to the overhead reservoir and this
permitted the water to trickle over the entire length of the condenser tube. It was noted that the
condenser tube sloped downward slightly, to ensure the proper drainage of the condenser oil and
steam. The cooling medium used in this device was cooling water drawn from a running tap.

3.5.3 Separator
Essential oil extracts and water condensate were known to have different densities and also from
an immiscible two liquid phases mixture at low room temperature conditions. The separation of
essential oils from the condensation hence utilize the density and immiscibility advantage for the
two be isolated each other. This phenomenon was the oil extract float on the water layer due to
being less dense than water. In separation the water from the oil, the water layer is carefully run
out from the bottom of decanter by opening the tap until its meniscus was just at the calibration
mark. The contents that remained inside the decanter are the oil layer and the water between the
tap bridge and the bottom of the calibration mark.

3.6 Determination of the Yield of lemongrass oil


𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑜𝑖𝑙 × 100
%𝑎𝑔𝑒 𝑦𝑖𝑒𝑙𝑑 𝑜𝑓 𝑜𝑖𝑙 =
𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑙𝑒𝑚𝑜𝑛𝑔𝑟𝑎𝑠𝑠 𝑙𝑒𝑎𝑣𝑒𝑠

19
3.7 Characterization of Lemongrass Oil
3.7.1 Physicochemical properties of Lemongrass Oil
Physical characterization is determining the physical properties of the extracted oil. Some of
these properties are specific gravity, evaporation residue, viscosity etc. Chemical properties of
lemongrass oil are such as acidic value, saponification value, iodine number. Physicochemical
properties were used to determine the quality of oil extracted. All parameters were determined
according to method of European Pharmacopeia (European Pharmacopoeia Commission, 2001)
and (Panda, 2009)

 pH
2g of the lemongrass oil was poured into a clean dry 25ml beaker, next 13ml of distilled water
was added in the beaker and stirred slowly. It was then cooled in a cold-water bath to 250C. the
pH electrode was standardized with buffer solution then the electrode was immersed into the
sample finally the pH value was read and recorded.

 Specific gravity
A tube (pycnometer) (w) was first filled with the lemongrass oil and then with water and their
respective weight w1 and w2 was determined. Then, the specific gravity was calculated using the
following formula:

𝑤1 − 𝑤
𝑆𝑝. 𝑔𝑟 =
𝑤2 − 𝑤

 Viscosity
35ml of lemongrass oil was poured into a test tube and a viscometer was used to measure the
viscosity at a temperature of 190C.

 Boiling temperature
25ml of lemongrass oil was placed into borosilicate glass and a thermometer was inserted and
placed on the heating mantal, it was observed that the oil in the borosilicate started circulating
leading to boiling of oil and the temperature on the thermometer was then recorded.

20
 Evaporation residue
20g of lemongrass oil was placed into borosilicate glass, put it on the heater and then
thermometer was inserted into the borosilicate glass until it reads the temperature of 100oC to
determine volatile matter.

𝑤2
𝑝𝑒𝑟𝑐𝑒𝑛𝑡𝑎𝑔𝑒 𝑜𝑓 𝑡ℎ𝑒 𝑜𝑖𝑙 = × 100%
𝑤1

Where:

W1 is the weight before evaporation and w2 is weight after evaporation

 Flash point of lemongrass oil


The flash point of lemongrass oil was measured by adding 25ml of sample into borosilicate glass

and then put it on heater next thermometer was immersed into the glass containing the sample to

read the minimum temperature of first flame. Finally, the temperature was read and then

recorded.

 Solubility
The solubility of lemongrass oil has been seen by adding 2g of lemongrass oil sample into 10
milliliters of alcohol and water.

 Acid value determination

2g of lemongrass oil was accurately weighted and dissolved in 10ml of 95% ethanol and 2-3
drop of phenolphthalein indicator was added. The free acid was then titrated with standard 0.1
normality of aqueous sodium hydroxide solution by adding the alkali drop-wise at a uniform rate
of about 30 drops per minute. The content of the flask was continuously agitated. The primary
manifestation of the red coloration that did not fade with 10sec was considered the end point.
Afterward, the acid value was determined using the following equations (Boukhatem N, 2014).

5.61 × (𝑛𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑚𝐿 𝑜𝑓 0.1𝑁 𝑁𝑎𝑂𝐻)


𝐴𝑐𝑖𝑑 𝑣𝑎𝑙𝑢𝑒 =
𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑡ℎ𝑒 𝑠𝑎𝑚𝑝𝑙𝑒 𝑖𝑛 𝑔𝑟𝑎𝑚

Where N is Normality

21
 Saponification value

1g of lemongrass oil was accurately weighed and dissolved in 10ml of 2.5 Normality potassium
hydroxide solution was added.

This procedure was performed together with blank experiment which was also perfumed
omitting the oil. The mixture was refluxed for two (2) hours then cooled. The unreacted KOH
was titrated with standard 0.5 Normality of oxalic acid by adding 2-3 drops of phenolphthalein
indicator until became colorless. After that, the saponification value was determined using the
following equation:

56(𝑣1 − 𝑣2 )
𝑆𝑎𝑝𝑜𝑛𝑖𝑓𝑖𝑐𝑎𝑡𝑖𝑜𝑛 𝑣𝑎𝑙𝑢𝑒 =
2×𝑊

Where W is the weight of oil, V1 is the volume of 0.5 normality of oxalic acid for blank; V2 is the
volume of 0.5 normality of the oxalic acid for sample (Boukhatem N, 2014).

 Iodine number

2g of lemongrass oil was dissolved in 10ml of chloroform. Then 25ml of iodobromide solution
was added and allowed to stand for 30 minutes in dark. Again 30ml of 1 N potassium iodide and
100ml of distilled water were added and the liberated iodine was titrated with 0.1 Normality
solution of sodium thiosulphate with constant shaking. When iodine color became quite pale,
1ml of 1% starch solution was added and the titration was continued until the blue color was
discharged. A blank test was also carried out parallel under identical conditions. The iodine
number was determined using the formula:

(𝑉1 − 𝑉2 )
𝐼𝑜𝑑𝑖𝑛𝑒 𝑛𝑢𝑚𝑏𝑒𝑟 = 1.269
𝑊

Where

W is the weight of sample,

V1 is the number of ml of thiosulphate by the blank; and

V2 is the number of ml of thiosulphate consumed by the test sample (Boukhatem N, 2014)

22
3.8 Formulation of Perfume
15ml of carrier oil (olive oil) were first placed in a clean and sterilized beaker to avoid
unexpected reactions (Salari, (2006)), followed by 42%vol vodka (25ml). 15 drops of lavender
were added as the base note in the beaker, then 25 drops of lemongrass oil as the middle note
were also added and lastly 10 drops of sandalwood as top note. The beaker containing mixture
was covered and placed in a cool dark place for 3 weeks to allow the scent to mingle and become
stronger. Then 10ml of distilled water were added to keep the evaporation of perfume a little
low. The sample product was then placed in a bottle using a funnel, covered and placed in a cool
dark place (because light can adversely affect their chemical properties) for 5 weeks in order to
marry and mature. (Onyinyechi, 2012)

23
CHAPTER FOUR: RESULT AND DISUSSION
4.1 Determination of moisture contents
The fresh leaves of lemongrass were collected on February, 2018 after drying by taking 35.48g,
43.4g, and 46.49g the moisture content of the sample was obtained in the following table.

Table 2: Moisture content determination of lemongrass leaves


Time for drying Moisture
Sample 0 2 4 6 8 10 12 content
weight (%)
(g) 35.48 35.07 35.04 35.02 34.97 34.95 34.95 1.494
43.4 42.98 42.97 42.94 42.93 42.92 42.92 1.106
46.49 45.92 45.88 45.87 45.83 45.82 45.82 1.441

The moisture content of the lemongrass leaves of 35.48, 43.4 and 46.49grams was 1.494, 1.106,
and 1.441% respectively. The average moisture content of the three samples was 1.347%.

4.2 Percentage yield


The amount of essential oil obtained by solvent extraction method was 3.67g of essential oil per
300g of dry lemongrass sample. This gave about 1.22% yield of essential oil per 300g of dry
lemongrass. The temperature used was 780C i.e. the boiling point of ethanol. The volume of oil
was measured at every 3hr interval to determine the oil yield at varying time. As the time
increase the ethanol solvent reduces thereby leaving the essential oil in the mixture.

The result of water distillation process was 2.01g weight of 300g of lemongrass sample giving
0.67% yield of oil

Table 3: Yield percentage from oil extraction methods


Method of extraction % yield
Solvent extraction 1.22%
Water distillation 0.67%

24
4.3 Factors affected the yield of extracted oil
4.3.1 Effect of extraction time on the yield of extracted oil with water distillation method

water distillation method


2.5

2
weight (g) of oil

1.5

0.5

0
0 50 100 150 200
time (min)

Figure 4.1: Effect of time on the yield of extracted oil with solvent extraction method

solvent extraction method


4
weight (g) of oil

3
2
1
0
0 10 20 30 40
time (hour)

Figure 4.2: Effect of time on the yield of extracted oil with solvent extraction method
Extraction time plays a great role on the percentage yield of lemongrass oil using both solvent
extraction and water distillation in figures (4.1 and 4.2) show that as contact time increase the oil
yield also increased the oil yield also increase till transfer of oil from leaves to steam attain zero.
When the maximum amount of extractable oil is obtained, the oil yield level remains invariable
even by extending the reaction time. So that the maximum oil yield could be finding at an
extraction time of 36 hours for solvent extraction and 3 hours for water distillation.

25
4.3.2 Effect of particle size on the yield of extracted oil

solvent extraction method


4
weight of essental oil (g)

0
5 6 7 8 9 10 11 12 13
particle size (mm)

Figure 4.3: Effect of particle size on the yield of extracted oil


The effect of increasing and decreasing particle size on oil yield has been shown on figure 3
above. It was quite clear that there was an increase in the oil yield to a maximum value due to
reduce in particle size and a further increase in particle size results in a drop in oil yield. In this
figure 3, it was observed that the minimum particle size has had maximum oil yield whereas the
maximum particle size has had minimum oil yield.

4.4 Physical properties


4.4.1 pH determination
the pH of the lemongrass oil was measured by pH and its value was recorded as 6.21.

4.4.2 Specific gravity determination


𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑝𝑦𝑐𝑛𝑜𝑚𝑒𝑡𝑒𝑟(𝑊)𝑎𝑡 25℃ = 103.0𝑔

𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑝𝑦𝑐𝑛𝑜𝑚𝑒𝑡𝑒𝑟 𝑤𝑖𝑡ℎ 𝑙𝑒𝑚𝑜𝑛𝑔𝑟𝑎𝑠𝑠 𝑜𝑖𝑙 𝑎𝑡 25℃ = 111.9𝑔

𝑤𝑒𝑖𝑔ℎ𝑡 𝑜𝑓 𝑝𝑦𝑐𝑛𝑜𝑚𝑒𝑡𝑒𝑟 𝑤𝑖𝑡ℎ 𝑤𝑎𝑡𝑒𝑟 (𝑊) 𝑎𝑡 25℃ = 113.1𝑔

𝑤1 − 𝑤 111.9 − 103.0
𝑓𝑟𝑜𝑚 𝑠𝑝𝑒𝑐𝑓𝑖𝑐 𝑔𝑟𝑎𝑣𝑖𝑡𝑦 = =
𝑤2 − 𝑤 113.1 − 103.0

= 0.881

4.4.2 Viscosity determination


The dynamic viscosity (𝜇) of lemongrass oil was measured using viscometer at 250C. the value
was found to be 2.069 mili Pascal seconds (mpas).

26
4.4.3 Boiling point of lemongrass oil
The boiling point of lemongrass was measured by the procedure described on the methodology.
The value was 2200C

4.4.4 Evaporation residue of lemongrass oil


The percentage of lemongrass oil which does not evaporated at 1000C was 97.5% shows
evaporation residue measurement i.e. mass of lemongrass oil evaporated at temperature of 1000C
is 2.5%

𝑤2
%𝑎𝑔𝑒 𝑜𝑓 𝑜𝑖𝑙 𝑛𝑜𝑡 𝑣𝑜𝑡𝑖𝑙𝑒 𝑎𝑡 100℃ = × 100
𝑤1

19.5
= × 100 = 97.5%
20.0

4.4.5 Flash point determination

The flash point of lemongrass oil was measured as 730C

4.4.6 Solubility of lemongrass oil


The lemongrass oil was soluble in alcohol and insoluble in water.

27
Generally, the physical properties of lemongrass oil extracted were summarized in the table 4.1.

Table 4: Value and unit of physical properties of lemongrass oil


Physical Results unit Standards
properties
pH at 250C 6.21 -
Specific gravity 0.881 0.890 – 0.906
Dynamic 2.069 mPa.s-1 -
viscosity at
250C
0
Flash point 73 C >66
0
Boiling point 220 C 224
Evaporation 97.5 %
residue
Color Brownish yellow liquid Brownish yellow liquid
Odor Very strong and stimulating Very strong and stimulating
characteristic lemon odor characteristic lemon odor
Solubility in Soluble soluble
alcohol
Solubility in Insoluble Insoluble
water

4.5 Quality evaluation of the lemongrass oil


4.5.1 Acid value determination
The acid was determined from;

56.1(𝑣𝑜𝑙𝑢𝑚𝑒 𝑜𝑓 𝑎𝑙𝑐𝑜ℎ𝑜𝑙𝑖𝑐 𝑠𝑜𝑑𝑖𝑢𝑚 ℎ𝑦𝑑𝑟𝑜𝑥𝑖𝑑𝑒 𝑠𝑜𝑙𝑢𝑡𝑖𝑜𝑛 × 𝑛𝑜𝑟𝑚𝑎𝑙𝑖𝑡𝑦)


𝐴. 𝑉 =
𝑚𝑎𝑠𝑠 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒

56.1(2.167𝑚𝑙 × 0.1)
= 12.155𝑚𝑙/𝑔
1𝑔

28
4.5.2 Saponification value determination
The saponification of lemongrass oil was calculated from;

𝑉1 − 𝑉2
𝑆𝑉 = 56 ( )
2×𝑤

56(11.5 − 11)
= = 14𝑚𝑙/𝑔
2 × 1𝑔

4.5.3 Iodine number determination


The iodine number calculated from;

𝑉1 − 𝑉2
𝐼. 𝑁 = 1.269 ( )
𝑊

(10.5 − 8)
= 1.269 = 31.725𝑚𝑙/𝑔
0.1

Table 5: Chemical properties of lemongrass oil

Chemical properties Value unit

Acid value 12.155 ml/g

Saponification value 14.00 ml/g

Iodine number 31.725 ml/g

29
4.6 Formulated perfume

Five experiments of perfume were carried out each with different amount of lemongrass oil
and fragrance oils (sandalwood and lavender oils), five people were selected at randomly
from Ndejje university to select the best blended experiment among all according to each
one. Marks were awarded from the five people to each experiment and the average mark was
calculated the one with the highest mark was taken as the best.

From the equation:

𝑡𝑜𝑡𝑎𝑙 𝑚𝑎𝑟𝑘𝑠 𝑜𝑏𝑡𝑎𝑖𝑛𝑒𝑑


=
𝑛𝑢𝑚𝑏𝑒𝑟 𝑜𝑓 𝑝𝑒𝑜𝑝𝑙𝑒

84
=
5

= 16.8

Experiment 2 had the highest average mark (16.8) and was selected as the best in all after
getting response from five people

30
CHAPTER FIVE: CONCLUSION AND RECOMANDATION

5.1 Conclusion

In this work, extraction of lemongrass oil was carried out. Extraction time and particle size were
considered as factors to see their effects on the yield of lemongrass oil extracted. The volume or
mass of lemongrass oil increase as extraction time increased and particle size decreased. The
maximum yield was found at extraction time of 36 and 3 hours using solvent extraction and
water distillation respectively, with particle size range from 5 to 8mm for water distillation and
the maximum yield is 1.22% for solvent extraction and 0.67% for water distillation. All these
methods of extraction are special type of separation process used for heat sensitive materials like
essential oils, resins, hydrocarbons, etc. which are insoluble in water and may decompose at their
boiling point. The formulation of perfume from extracted essential oil was carried out. Finally,
extraction of essential oil from lemongrass can also be used on industrial scale to make various
finished product like body oils, cosmetic lotions, baths, hair rinse, soap etc.

5.2 Recommendation

In this work, the effect of temperature, pressure and chemical compounds of lemongrass
oil were not studied due to the lack appropriate equipment. Therefore, further study is
need on these effects.
Study can be carried on converting the residue or the waste valuable product and using
the hydrosol as integrated small scale industry.
The temperature in water distillation must be high enough to vaporize the essential oil
present, yet not destroy or burns the essential oils.

31
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33
Appendix
Laboratory equipment’s and samples photos

water distillation column


Lemongrass leaves

Sieve plates Partially dried lemongrass of different sizes

Extracted lemongrass oil Fresh cut lemongrass leaves

34
Micro oven Determining boiling and flash point of lemongrass oil

Determining Acidic value

35