EXTRACTION OF PERFUME OIL FROM LEMON PEELS
CHAPTER ONE
1.0 Introduction
A perfume is a liquid mixture of oils that emits a fragrant odor. (White and Eiserle, 1961). Natural
oils used to make ancient perfumes extracted from plants and animals through pressing and
steaming. In 18th century in France there was an inconceivable stench in cities. The streets stank
of manure, Sulphur rose which emanated from chimneys, caustic lye from tanneries and stench of
congealed blood from slaughter points. The oil was then burned to scent the air. The ancient
Egyptians were famous for luxury perfume and it was the center of production of many exotic and
luxury perfume. These could only be afforded by the royalty and upper class and applied to the
face to protect themselves from harsh sun, wind and dryness. (Briot E, 2011)
1.2 Problem statement
There is a high demand of perfume especially from the teenagers and women. In Zimbabwe there
is no cosmetic industry and many people are now making business by importing the cosmetic
products. There is an increasing percentage of people and local shop owners who are importing
Avon and Avoshlain products from South Africa which include facial products for ladies and most
importantly the perfumes. These products are very expensive and people from low income
background do not afford to buy. Due to high inflation rates in Zimbabwe those doing the business
are now affected because the exchange rates between South African Rands and Zimbabwean
dollars are high such that some of them are now operating at break-even point, and some abandon
the business due to high loses made. This high inflation rates causes the price of the products to
increase and this negatively affects both the importers and consumers.
1.3 Justification
This section highlights the importance of this project. It emphasizes on the economic and
environmental benefits of this project
Economically
Perfumes extracted from lemon peels can match and improve the commercially available products
at low cost. Theperfume would accommodate individuals from poor communities. The product
will be cheaper than the Avon and Avoshlain perfume as it is made from raw material which is
locally available. Lemon is a raw material and is found in Zimbabwe as an exotic plant and can
substitute expensive lavender, jasmine and roses. These plants are rare, they are found mainly in
Asia and India and the rarer the raw material is the more expensive it is. This project can lead to
rise of cosmetics industry in Zimbabwe and this can create employment as there is 95% level of
unemployment in Zimbabwe. The industry will make high profits and this can make the companies
offer some service to the communities like offering scholarships to students. These services offered
to the society reduces the government taxes that it imposes on industries and companies.
Environmentally
There is a significant amount of solid waste of lemon peels after extraction of juice. Lemon peels
are dumped to the surroundings and this leads to environmental pollution due to improper disposal.
This create environmental problems for communities due to the presence of biomaterials in lemon
peels, therefore this project can reduce land and water pollution as lemon peels are in high demand.
1.4 Aim
The main objective of this project is to extract perfume oil using lemon peels as a source of raw
materials.
1.5 Specific objectives
 To study properties and sources of perfumery oil
 To characterize perfumery oil from lemon peels and review its uses
 To study various technologies used in perfume oil extraction
 To investigate the amount of perfume oil extracted from lemon peels and the optimum
time required for maximum extraction.
1.6 Project approach
The project is organized into five chapters. Chapter one is the introduction. It describes the
background of the study and highlights the problem statement for the research.It states the general
and specific objectives of the study, comments on why the study is of significant importance and
lastly, discusses the organization of the project.
Chapter two presents the overview of relevant literature concerning the classification of perfume
oils and uses of perfume. It highlights the physical and chemical properties of valuable perfume
components from lemon oil and lastly describes the extraction techniques used in the extraction of
fragrant oil from lemon.
Chapter three is the methodology of the study which describes the principle of solvent extraction
technique in isolation of perfume oil from lemon peels.
Chapter four is analysis and discussion of results obtained from the experiments and the effects of
processing parameters.
Chapter five contains the summary of the key findings, conclusion and recommendations of the
project.
CHAPTER TWO
2.0 Perfume
A perfume is a liquid mixture of fragrant oils, compounds of high aroma, organic solvents and
fixatives. (Tananuwong and Lertsiri, 2010) It gives the human body and objects a pleasant odor
by covering the scent of the base product. It is a volatile liquid distilled from scented flowers which
include lavender, jasmine and roses. It is also extracted from roots and leaves of scented plants.
Perfumery products fall into two main categories which are household products and toiletries.
Toiletries include fine fragrances, cosmetics, personal care products, and deodorants. Household
products includelaundry products, air fresheners, and disinfectants. Perfumes influence emotions
and mood. It masks off human odor due to sweat. Human body uses the aromatic molecules
through olfactory receptor genes which are connected to the brain. This is where primal feelings
and emotions reside. Fragrant compounds of low molecular weight are absorbed through the
skin. (Sicard et al, 1985).
2.1 Components of perfume
A perfume is made up of four basic parts.
2.1.1Basics
These are essential oils in the perfume and make up the basic composition of the smell. Essential
oils are highly concentrated plant extracts and synthetic substances that have a fragrant
odor. (Sergeeva, 2016). They form the base of the perfume which can be modified by adding
different scents of higher volatilities to create a unique fragrance. Oils make up 10 % to 25% of
the perfume.They are stored in dark colored containersand tightly sealed because they are quickly
degraded by air, light and excess heat. Physical and chemical tests are conducted to determine the
purity of perfume essential oils. Test stages are:

The sensory evaluation whereby the scent, viscosity and color of the oil is assessed. Highly
volatile oils at room temperature are called adulterants.

The odor or smell test determines if the oil is accurately what is claimed to be. This test
also identifies adulterants.

Physical parameters are determined, such as specific gravity, refractive index and optical
rotation.

The oil is then subjected to Gas Chromatography – Mass Spectrometry (GC-MS)
evaluation. (Tamasi and Zsoldos, 2017). This approach is used for analysis of both natural
and synthetic fragrant substances. The cause of perfume allergy in contact eczema and
dermatitis patients is due to use of perfumed consumer products such as cosmetics and
toiletries. (Garioch, Forsyth and Chapman, 1989).
For the management of allergy, the
contents of fragrant allergens are analyzed using GC-MS. Patch-testing is then done on the
patient so as to avoid use of products which contain the sensitizing allergen.
2.1.2 Solvents
The solvent dissolves all the components of a perfume. They dilute the fragrant mixture and this
increases the surface area of application so that small amounts of the fragrance is used. (Shafique
et al., 2013). They also decrease the intensity of the fragrant solution which also reduces the price
of the perfume. The most widely used solvent is ethanol.
2.1.3 Fixactives
Fixatives are ingredients which prolong the odor effect of a perfume and regulate the rate of
evaporation of highly volatile notes of fragrant components. (Fisher and Dooms-Goossens, 1976).
They prevent spot residues on skin and clothes after perfume application. The components are
odorless. They are soluble in both polar and non-polar solutions and are of higher boiling point
temperature. The fixatives form hydrogen bonds with the fragrant molecules thus decreasing the
overall vapor pressure of theliquid mixture. (Phang, 1999).Fixactives retain a high concentration
of both the top and middle notes and release them slowly over a long period of time.The fixatives
blend all the perfume fragrant components so that their character do not change quickly as
individual ingredients evaporate.Examples of fixatives include ester extracts, glycol and diethyl
phthalate. Fragrances should be protected from excessive heat, light and oxygen so that they
remain fresh for about three years from the manufacturing date.
2.1.4 Carrier Oils
Perfume oil istoo strong and very expensive such that it cannot be used without dilution due to its
toxicity to the central nervous system. (Perfumery: Essential Oils and Volatiles, 1970). These
attributes are moderated by the use of carrier oils which dilute the fragrance. Carrier oils are
extracted from nuts, vegetable and animal oils and can also be pressed from commercially
produced crops. Carrier oils should be chemically inert and stable to oxidation. (Banthorpe, 1989).
They include oils from avocado, soybeans and sunflower. Carrier oils are usually 5 % by volume
of the total perfume.
2.2 Types of perfumes
Types of perfume are eau de toilette, eau de parfum, and parfum. (Stannard, 2014). They are
classified based on their concentration of oil, alcoholic solvents and water. The concentration
ranges are shown in the table below.
Table 1: Types of perfume
Types
Total volume %
Total volume %
Total volume %
Oil
Alcohol
Water
Parfum
15 - 30
63 - 80.75
4.25 - 7
Eau de parfum
8 - 15
68 - 82.8
9.2 - 17
Eau de toilette
4–8
73.6 - 86.4
9.6 - 18.4
2.3Classifications of scents of perfumes.
The performance of a scent within a fragrance is measured technically by its volatility or tenacity.
The scents are divided into three categories: top, middle and base notes.
Figure 1: Fragrance pyramid (Source: Liu and Hayashi, 2014)
2.3.1 Top Note
The top notes provide freshness to the perfume blend. These notes are not detected after 2 hours
after application due to high level of volatility. (White and Eiserle, 1961)
They are the first
components to vaporize from the fragrant mixture. The fragrance of top noteconstitutes the largest
initial impression of the perfume smell and therefore are a selling note of a perfume. Constituents
of top note oils are citrus oils. The consumer initially evaluates these scentswhen purchasing a
perfume.
2.3.2 Middle Note
Middle note oils are considered as the heart of the fragrance.These fragrances last for several hours
approximately 6 hours after application and are the most prominent within the fragrance. Middle
notes have moderate volatility. Examples of middle notes are heavy spices and floral or fruity oils
extracted from rose, pine, black pepper, rosemary and carrot seed. (Yu, Zhou and Parry, 2005)
2.3.3 Base Note
Base notes are the most important perfume oils as they act as fixatives for all scents. They have
the lowest volatility and lasts for very long periods on the skin. These notes can be detected from
a period of 8 to 72 hours. (Shiner, 2015) Constituents of base note perfume oils are musk oils,
lavender, sand wood, lavandin and jasmine.
2.4Classification of perfume oils.
Classification of perfumery oil may be based on the origin of ingredients, method of preparation,
chemical structure and functional groups.
2.4.1 According to origin of ingredients
 NATURAL PLANT EXTRACTS
Natural ingredients are derived straight from plants and are not subjected to any physical or
chemical modifications. They are a complex blend of molecules which are obtained in pure and
concentrated form from plants, herbs, fruits and seeds. These materials consist of ten to hundreds
of different individual molecules. Plants and animals produce odorous materials through
biosynthesis mechanism. The materials produced are primary and secondary metabolites. Primary
metabolites are divided into proteins, carbohydrates, nucleic acid and lipids. Secondary
metabolites are the perfumery ingredients which are derived through degradation of primary
metabolites. The categories of secondary metabolites which are perfume ingredients are
polyketides, terpenoids and alkaloids and are derived from glucose. (Gaich and Mulzer, 2005).
The quality of natural oils depends strongly on geographic origin and this is largely due to
diferences in cultivation conditions such as the type of soil, climate, genotype and on the extraction
process. However, they are very expensive due to their limited yield.Natural perfume oils are citrus
oil, lavender oil, eucalyptus oil and citronella oil and citrus oil used as top notes in perfumes. (de
Groot and Schmidt, 2016).
 MUSKS
Musks are extracted from animals and the major sources are musk and civet. Musk and civet are
extracted from the anal glands deer and the civet cat respectively. (VAN DORP, KLOK and
NUGTEREN, 1973) These extracts have a strong animalic odor character which arise 2-methylin-
dole compounds. The musk deer is commonly found in Asia and the civet cat is found in Africa
and Asia. Animalicordor is an entirely unpleasant note but it lays a rich, sweet character which
serve to ‘fix’ other notes due to the presence of Muscone (35) and civetone (36) compounds which
have good fixaction characteristics.
 SYNTHETIC INGREDIENTS
Synthetic ingredients are obtained by processes of enriching the fragrant essence with several
components. Most synthetics are derived from coal, tar and petroleum. These materials are
produced in a lab through a set of chemical reactions such as heating, enzymatic and microbial
reactions under specific temperature and pressure. These artificial perfumes undergo reasonable
evaporation to give acceptable scent. They leave behind them certain residue on skins or clothes
as spots which are absorbed by the skin causing skin irritations. Synthetic oils are galaxolide, lilial
and amyl cinnamic aldehyde.
2.4.2 According to method of preparation
Extracts of fragrant substances obtained from plants are divided into five classes based on the
preparation method.
 POMADES
Pomades consist of fatty material that contain fragrant molecules. They are produced by both hot
and cold enfleurage of flowers. (Tsering Shakya, 2000) Hot enfleurage preserves plant fragrance
substances. Flowers and fragrant bearing materials from plants are immersed in liquid or molten
wax. In cold enfleurage, the highly volatile components released into the surrounding are absorbed
fats and are retained for a very long period. The process of cold enfleurage was initially developed
in the 19th century in France for high grade industrial production of flower concentrates. Fresh
flowers are applied to alayer of fats which consist of a mixture of highly refined lard and beef
tallow, which is placed on a glass plate in a closed vessel so as to preserve volatile components.
(Ghani, Ismail and Asakawa, 2016)
 CONCRETES
Concretesare fresh plant material extracted using nonpolar organic solvents which include hexane,
toluene and petroleum ether. Solvents are then evaporated and the remaining residue contains a
large proportion of volatile fragrance materials and nonvolatile waxy compounds. Concretes are
highly stable and concentrated as compared to unmodified essential oils. Concretes are partially
soluble in alcohol and are employed in the scenting of soaps. They are prepared mainly from rose,
jasmine, lavender and violet leaves. (Anac, 1986)
 ABSOLUTES
Absolutes are prepared through a second process of ethanol or liquid carbon dioxide extraction of
concretes. Upon cooling some compounds precipitate and are then removed by the filtration
process. Ethanol is evaporated and a wax-free residue left behind is an absolute. Absolutes
completely dissolve in ethanol therefore they are freely used as perfume ingredients Oils produced
through liquid carbon dioxide extraction have high quality aroma and are 100% free of undesired
solvent residues and nonvolatile materials.
 RESINOIDS
Resinoids plant exudates such as frankincense, myrrh and amber extracted using hydrocarbon
solvents. Yield range from 50 to 95%. Resinoids are highly viscous substances and are often
diluted with phthalates or benzyl benzoate to improve their flow properties and for ease of
processing. (F. L. Herum, G. W. Isaacs and and R. M. Peart, 1966). Resinoids consist of a large
propprtion of nonvolatile compounds which have excellent fixative properties.
 TINCTURES
Tinctures are sometimes called infusions. They are alcoholic solutions that are prepared by treating
natural raw materials with ethanol or ethanol-water mixtures. They can also be obtained by
dissolving other plant extracts in alcohol.
2.4.3 According to functional groups
Compounds and aroma of perfume oils are terpene hydrocarbons and oxygenated
hydrocarbons.The terpenes are natural odorants which form the most common class of compounds
in the modern fragrance ingredients. These oils consist of mainly monoterpenes with chemical
formula C10H16 and molecular weight of 136, sesquiterpenes with chemical formula C15H24 and
molecular weight of 204. They are relatively unstable molecules with an aggressive odor due to
high degree of unsaturation. Myrcene, and farnesene are present in fruity oils andtheir use is
limited to perfumery. Oxygenated hydrocarbons are terpenoids which contain carbon, hydrogen
and oxygen.
Alcohols, aldehydes, ketones, esters and lactones are oxygenated compounds
frequently found in both natural and artificial fragrances. (Siek et al., 1971)
 ALCOHOLS
Acyclic terpene and sesquiterpene alcohols are found in many natural oils. These alcohols were
formerly isolated from oils in which they are major components. Currently there is large-scale
synthesis of terpenoids which are synthetic products. The odor qualities of synthetic products differ
from those of compounds isolated from natural sources since the desired natural product is not
separated from small amounts of compounds with similar physical properties but different odor
quality.The acyclic terpene alcohols geraniol, linalool, and citronellol are the most important
terpene alcohols used as fragrance and flavor substances. (Belsito et al., 2008)
 ALDEHYDES AND ACETALS
Among the acyclic terpene aldehydes, citral and citronellal are the key components of fragrance
and flavor chemicals. They are starting materials for the synthesis of other terpenoids.
Hydroxydihydrocitronellal is one of the most important fragrance materials. Lower acetals are
aldehyde derivatives which are used as fragrance materials. (Saito et al., 2017) They contribute to
the characteristic fragrance and aroma of alpha and beta sinensal in sweet orange oil.
 KETONES
The most important acyclic terpene ketones component in fragrances is Geranylacetone and
damascenone. Geranylacetone is an intermediate in the synthesis of some fragrance substances
and is mainly produced from linalool. It is also produced from the catalytic reaction of myrcene
and methyl acetoacetate using rhodium catalyst. It is used in perfumery in rose oil and in in soap
perfumes. Beta damascenone is an important component of Bulgarian rose oil.
 ACIDS AND ESTERS
Lower fatty acid esters particularly the acetates of the acyclic terpene alcohols geraniol, linalool,
and citronellol are extremely important contributors to the odor of many essential oils, these esters
are widely used as fragrances. The most widely used acetates are linalyl acetate, geranyl and neryl
Esters. (VIDARI et al., 2010)
 LACTONES
Lactones are naturally occurring organoleptic compounds. Most occurring lactones are saturated
and unsaturated γ- and δ-lactones and their occurrence reflects their ready formation from natural
acyclic precursors. Lactones are the intramolecular esters of the corresponding hydroxyl fatty
acids. They contribute to the scent of butter and various fruits. 15-Pentadecanolide is characteristic
for the musk-like odor of angelica root oil. Lactones can be synthesized by depolymerization of
the corresponding linear polyesters in large scale production. Various cyclic diesters are prepared
from long-chain α and β-dicarboxylic acids and glycols which are also valuable musk fragrances.
The γ-lactones are prepared to give high yield by radical addition of primary fatty alcohols to
acrylic acid and di-tert-butyl peroxide used as a catalyst. High yields are also obtained when the
reaction is carried out in the presence of alkali phosphates or alkali sulfates. There is high demand
for natural γ- and δ-lactones in the perfume industry therefore biosynthetic processes have been
developed for large scale production. Examples are γ-Octalactone which is a pale yellow liquid
with a fruity/coconut-like odor which is used in heavy blossom perfumes. γ- decalone is a colorless
liquid with an intensely fruity odor, reminiscent of peaches. (Yoshizawa et al., 1988) It is used in
perfumery for heavy, fruity flower particularly peach scent.
2.5 Perfume oil from lemon peels
Perfumery oil extracted from lemon peels is a very complex matrix containing numerous
compounds of different classes.It is a mixture of monoterpene and sesquiterpene hydrocarbons and
their oxygenated derivatives the aldehydes, ketones, acids, alcohols and esters. (Büchi, 1958)
Lemon peel oil is used as industrial deodorants to mask the unpleasant scent of industrial products
like rubber and plastic. Limonene is used as a biodegradable solvent in the manufacture of paint.
Toys are also scented. In textile industries they are used todisguise unpleasant smell during and
after dyeing process. Face wipes, notebooks and toilet paper, and are scented in paper making
industries.
The valuable components of lemon oil for perfumes are:

Limonene

Linalool

Pinene

Myrecene

Terpinene
2.5.1 Limonene
Limonene is a volatile monoterpene which is used as a fragrance material for perfuming household
products such as deodorants and bar soaps. It is a liquid substance with a lemon like odor.It has
high vapor pressure which predicts its high rate of vaporization.The (+) isomer in lemon peel oilis
present at a concentration of about 90%and is the precursor to main components of mint fragrance
such as carvone and menthol. Limonene is a very reactive compound which is easily oxidized.
Figure 2: Limonene structure
Chemical name
: (R)-1-methyl-4-(1 methylethenyl) cyclohexene
Molecular Formula
: C10H16
Molecular weight
: 136.23 g/mol
Boiling point
: 176 °C
Solubility
:Slightly soluble in water
Vapour pressure
: 190 Pascals at 20°C
2.5.2 Linalool
Linalool is a colorless liquid which has a fresh flowery odor and a slight citrus impression.
Together with its ester derivatives , linalool is the most widely used fragrant substances in
perfumes , bar soaps, hand lotion and air fresheners. (Arce, Marchiaro and Soto, 2003) It serves
as a natural and desirable top note in perfumes due to its high relative volatility.Linaloolisomerizes
in acids to give geraniol, nerol, and alpha terpineol. It is readily oxidized by chromic acid to citral
and with peracetic acid to give linalool oxides which are also used in perfumery. Hydrogenation
yields tetrahydrolinalool which is a stable fragrance material. Linalool used for fruity flowery
fragrance notes such as lily of the valley, neroli and lavender.
Figure 3: Linalool structure
Chemical name
: 3,7dimethyl octa-1,6-dien-3-ol
Molecular Formula
: C 10H18O
Molecular weight
: 154.25 g/mol
Boiling point
: 198 °C
Solubility
: insoluble in water
Vapour pressure
: 121 Pascals at 25 °C
2.5.3 Pinene
Pinene is a naturally occuring terpene hydrocarbon which exists either as α or β pinene with
varying ratios in lemon oil. Pure pinene is used as a fragrant substance which is used to improve
the ordor propeties of industrial products. It undergoes many reactions which yield fragrant
products.Hydrogenation of α-pinene gives pinane, which is an important starting material in the
industrial processes used in the fragrance and flavor industry such as the synthesis of terpineols
and camphor. Pyrolysis of α pinene yields a mixture of ocimene and alloocimene which is used to
improve odor of shaving creams and hair remover. α-Pinene can be isomerized to β-pinene with
high selectivity for β-pinene formation. (Hatakeyama et al., 1989)
Figure 4: Pinene structure
Chemical name
: 2,6,6-trimethylbicyclo(3.1.1) hept-2-ene
Molecular Formula
: C10H16
Molecular weight
: 136.24 g/mol
Boiling point
: 156 °C
Solubility
: 2.49mg/L in water at 25 °C
Vapour pressure
: 536 Pa at 25 °C
2.5.4 Myrecene
Myrecene is an unstable compound which has a slight aggressive odor due to high degree of
unsaturation.It is a colorless oil with a peppery, spicy and balsam odor.It is used in the perfume
industry but is not used directly as it tends to polymerise due to its chemical instability.In 1976,
Opdyke reported that the amount of myrecene used in fragrance industry in United States is
approximately 2000 pounds per year. It is an intermediate in the large scale commercial production
of terpene alcohols, geraniol, linalool and nerol which are used in large volume production of
fragrant chemicals. It is converted to mycenol a fragrant copund found in lavender throuhg
hydroamination of 1,3 –diene by diethylamine followed by hydrolysis. Myrecene is used as a
scenting agent in cosmetics, soaps and detergent.
Figure 5: Myrecene structure
Chemical name
: 2-Methyl-6-methylene-2,7-octadiene
Molecular Formula
: C10H16
Molecular weight
: 136.24 g/mol
Boiling point
: 167 °C
Solubility
Vapour pressure
: Insoluble in water
: 301 Pascals at 25 °C
2.5.5 Terpinene
Terpinene has a pleasant ordour whish is similar to liliac and is widely used in the manufactute
cosmetics, soaps and perfumes.
Figure 6: Terpinene structure
Chemical name
: p-mentha-1,3-diene
Molecular Formula
: C10H16
Molecular weight
: 136.24 g/mol
Boiling point
: 183°C
Solubility
: sparingly soluble in water
Vapour pressure
: 93.3 Pascals at 25 °C
CHAPTER THREE
3.0 Methodology
Heptane
added
Vessel
containing
lemon
peels
1. Preheating in
oven
2. Leaching
Methanol
added
Lemon oil
5.Evaporation
4. Solvent
extraction
Methanollemon oil
mixture
Figure 7: Block diagram for extraction process
3.1 Materials
-
2kg lemon peels
-
2 liters heptane
-
2 liters methanol
-
2*500ml flask
-
4 * 500ml beaker
3. Filtration
Heptane lemon
components
mixture
-
500ml separating funnel
-
Water bath
-
Thermometer
-
Iodine solution
3.2 Procedure
Fresh lemon peels were collected, sliced and washed with water to remove any particulate matter.
75g of lemon peels were measured on an electronic balance and placed in a plate. The peels were
preheated in an oven at a temperature of 45 degrees Celsius for 60 minutes. The peels were then
placed in a 500ml flask. 250 ml of heptane solvent was poured into the 500ml flask containing
lemon peels and stopped. The flask and its contents was allowed to stand for 24 hours. This was
done for complete extraction of the oil contents in the lemon peels.
Figure 8: Leaching lemon oil using heptane solvent
The lemon oil extracted was then decanted into another 500ml so as to separate the extract from
the solids. 200ml of methanol was added to extract the essential oil (myrecene, alpha and beta
pinene, limonene, and linalool) since these are the essential components for perfume which
dissolve in alcohols. The mixture was then transferred into a separating funnel so as to extract
valuable perfume components by liquid -liquid extraction process. The separating funnel contents
were allowed to stand for 60 minutes so that equilibrium is achieved. The mixture separated into
2 layers due to density differences, the lower layer which consisted of ethanol- valuable extract
mixture and upper layer which consisted of hexane. The two layers were collected into 2 separate
250ml beakers.
Figure 9: Liquid-liquid extraction process
The beaker which contained the ethanol extract mixture was placed in a water bath at 80 degrees
Celsius for 3 hours. This was done to evaporate methanol leaving the desired perfume oil only.
Methanol boils at 64.5 degrees Celsius. To ensure that all methanol was evaporated the mass of
the beaker and its contents was measured at regular intervals of 60 minutes until a constant mass
was obtained which showed that there was no more methanol left.
Figure 10: Evaporation using water bath
The yield of perfume oil extracted was determined by measuring the amount of extract in a
measuring cylinder.
3.2.1 Varying preheating temperature
The procedure was repeated with different preheating temperature of 55, 65, 75, 85, and 95
degrees Celsius for 60 minutes to get the optimum preheating temperature and the results were
tabulated.
3.2.2Varying the extraction time
The procedure was repeated using different extraction times of 20, 40, 60, 80, 100 and 120
minutes. 250 ml of heptane was used in each case and a constant solid to solvent ratio of 75 grams
of peels to 200 ml of methanol was maintained. Preheating temperature was maintained at 75
degrees Celsius for 60 minutes.
3.2.3 Varying the solid to solvent ratio
The procedure was repeated by varying the amount of solvent methanol from 140, 160, 180, 200,
220, 240 ml. 75grams of lemon peels were used and kept constant in each case. Preheating
temperature was kept constant at 75 degrees Celsius and extraction time maintained at 80 minutes.
3.2.4 Confirmation test
Iodine test: This test was done to characterize the presence of unsaturated compounds in a test
sample. 15ml of citrus oil extracted was prepared and placed in a test tube. 3 drops of iodine
solution were added to the test tube containing citrus oil and observations made and recorded.
CHAPTER FOUR
4.0 Experimental results analysis
The yield and quality of oil depends mainly on extraction technologies employed. In this research
operating parameters that is preheating temperature, extraction time and solid to solvent ratio were
the variables evaluated in order obtain the optimum yield for the extraction of perfume oil using
the liquid- liquid extraction process. The oil extracted was pale green in color as shown in the
figure below with a tinge citrus lemon odor. When the oil was left open for few days its color
changed from pale green to almost colorless and the odor faded as it evaporated into the
atmosphere.
Figure 11: Perfume oil from lemon peels
4.1 Investigating the effect of preheating temperature on oil yield
Table 2: Effect of Preheating temperature on lemon peels for perfume oil extraction
Run
Solid/Solvent
Temperature
Oil Extracted
% Yield
(g/ml)
(◦C)
(ml)
1
75/200
45
0.50
0.67
2
75/200
55
1.25
1.67
3
75/200
65
3.75
5.00
4
75/200
75
5.75
7.67
5
75/200
85
5.80
7.73
6
75/200
95
5.20
7.07
Figure 12: Graph of Preheating temperature against oil yield
Figure 12 above shows the effect of preheating temperature on oil yield. It is observed from the
figure that the increase in preheating temperature of lemon peels increases the oil yield until a
temperature of 85°C is reached when there is a maximum yield of 7.73 %. There is a sharp increase
in oil yield from a temperature of 55°C to a temperature of 75°C as indicated by a very steep
gradient. As the temperature is increased to 95°C the yield of oil decreases to 7.07%. This is due
to the fact that at higher temperature the lemon peels begin to char at the bottom of the dish as they
turn from green to yellow and finally brown in color. High temperature leads to thermal
degradation of the valuable chemical components within the peels hence yield is reduced.
4.2 Investigating the effect of extraction time on oil yield.
Table 3: Effect of extraction time
Run
Solid/Solvent
Extraction time
Oil extracted
% Yield
(g/ml)
(minutes)
(ml)
1
75/200
20
1.25
1.67
2
75/200
40
3.00
4.00
3
75/200
60
5.50
7.33
4
75/200
80
7.00
9.33
5
75/200
100
7.00
9.33
6
75/200
120
7.00
9.33
Extraction time against % oil yield
10
9
8
% OIl yield
7
6
5
4
3
2
1
0
0
20
40
60
80
Extraction time (minutes)
Figure 13: Graph of extraction time against oil yield
100
120
140
The effect of solvent extraction time on the yield of oil is shown on figure 13 above. From the
figure it is observed the yield of oil increases with increase in extraction time and is maximum at
80 minutes. There is a direct proportionality between extraction time and yield until an optimum
temperature is reached where there is a maximum yield of 9.33%. Further increase in extraction
time has no effect on the yield of oil as the yield remains constant at 9.33% after 80 minutes.
4.3 Investigating the effect of solid to solvent ratio on extraction time
Table 4: Effect of solid to solvent ratio
Run
Solid/Solvent
Heptane used
Oil extracted
% Yield
ratio
(ml)
(ml)
1
75/140
250
4.75
6.33
2
75/160
250
5.75
7.67
3
75/180
250
6.75
9.00
4
75/200
250
7.00
9.33
5
75/220
250
7.10
9.46
6
75/240
250
7.12
9.49
From figure 14 below it is observed that there is a direct relationship between solid to solvent ratio
and the oil yield. As the solid to solvent ratio is increased from 75/140 to 75/180 the yield also
increases from 6.33% to an optimum yield of 9.33%. Further increase in the ratio of solid to solvent
it is observed that there is a slight increase in the oil yield therefore we can assume that after an
optimum yield has been reached the solid- solvent ratio has no effect on the yield since the gradient
of the graph is almost zero.
Figure 14: Graph of solid/solvent ratio against oil yield
4.4 Confirmation test result
Figure 15: Iodine test
Upon addition of few drops of iodine solution, the pale green lemon peel oil changed color to red
brown as shown in the diagram above. The brown color is due to the reaction of iodine with
unsaturated lemon oil compounds which are alpha pinene, beta pinene, myrcene, limonene and
linalool.
CHAPTER FIVE
5.1 Conclusion
Environmental pollution is due to the disposal of lemon peels after juice extraction. This problem
may be overcome by solvent extraction of lemon peel oil which is a precursor for the formulation
of perfume in the fragrance industry. Citrus trees are grown extensively by the farmers in the
Eastern Highlands of Zimbabwe but the country is mostly importing cosmetics. It is important for
this project to be implemented so that we make use of the environmental waste of locally available
resource. There is a lot of demand for perfumes especially from ladies therefore production
targeting that market will be very profitable.
The optimum yield of 9.49 % which is 7.12ml of oil extracted per 75g of lemon peels used was
obtained at optimum extraction time of 80minutes, preheating temperature of 75°C and a solid to
solvent ratio of 75/240 (g/ml).
5.2 Recommendations
In this research, a water bath was used at a temperature of 80°C to evaporate methanol from the
valuable components and is a lengthy process as it took 4 to 5 hours for complete evaporation.
Other methods should be used for the recovery of the valuable components which include the use
of a pyro evaporator which speeds up the process. Also the long exposure of the mixture lead to
thermal degradation of the value components.
Soxhlet extraction technique should be used which allows the recovery of the methanol solvent as
there was a lot of solvent loss during evaporation in the water bath. There should also be techniques
to recover the heptane solvent which contained the lemon peel components which are insoluble in
methanol after the solvent extraction process.
Analytical methods which include Gas Mass Spectrometry should be done to analyze the chemical
compositionof each component in the value oil and physical tests done to evaluate the specific
gravity and refractive indexes of the components.
Various extraction methods like distillation and supercritical carbon dioxide extraction should be
done and the method which gives the highest yield of oil at relatively low cost determined.
Different solvents which include methanol, ethanol and hexanol should be used to determine which
solvent gives highest recovery. Experiments say the higher the length of the hydrocarbon chain
the lower the degree of separation.
More confirmation tests to be done which include Bromine test which characterizes the presence
of limonene which is present in larger quantities of approximately 90%.
Vermicomposting is a process of bacterial decomposition of organic matter to produce garden
manure. Residual lemon peels after the extraction process can be taken through the
vermicomposting process which is an environmentally friendly disposal method.
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