Extraction of Essential Oil from Orange Peel

ADIGRAT UNIVERSITY
COLLEGE OF ENGINEERING DEPARTMENT OF

CHEMICAL ENGINEERING
THESIS TITLE: EXTRACTION OF ESSENTIAL OIL FROM ORANGE PEEL USING

STEAM DISTILLATION
A Thesis Submitted to departments of Chemical Engineering in Partial Fulfilment of the Degree

of Bachelor of Science in Chemical Engineering.
By:
NAME OF STUDENTS ID NO
1. Haftom Weldegebriel 0724/06

2. Tesfu Gidey 1501/06
3. Zeray Zenfo 1705/06
Advisor
Instructor Tsegaluel k. (MSc)
Adigrat, Tigray, Ethiopia
JUNE 2018
EXTRACTION OF ESSENTIAL OIL FROM ORANGE PEEL USING STEAM
DISTILLATION
DECLARATION
This is to declare that the thesis entitled, “Extraction of Essential oil from orange peel by using
steam distillation” submitted by Haltom W/Gabriel, TesfuGidey and ZerayZenfo in partial a
fulfillment of the requirements for the award of Bachelor of Science Degree in Chemical
Engineering at Adigrat University is an authentic work carried out by our self under the
supervision and guidance instructor Tsegaluel.K (lecturer).
Name Signature
4. Haftom weldegebriel.......................................................
5. Tesfu gidey......................................
6. Zeray zenfo...................................................
The thesis titled Extraction of essential oil from orange peel using steam distillation was
submitted by this thesis group member has been accepted as satisfactory in partial fulfilment of
the requirement for the degree of Bachelor of Science in Chemical engineering.
Approved by
.......................... ……………………. ……………………
Advisor Signature Date
………………… …………………. …………………

Examiner Signature Date
………………… …………………… …………………

Chairman Signature Date
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Department of chemical engineering(ADU)
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Acknowledgment
Praise God, the Most Merciful and Compassionate, for giving us strength in completing this
thesis research. Next and for most, we would like to express our deepest gratitude to our advisor
Tsegalaul(lecturer) from department of Chemical Engineering for his tireless advice, supervision,
guidance and patience throughout our research work. Our great thanks and appreciation also goes
to department of chemical engineering for the provision of chemical and equipment support so as
to accomplish our project work, all laboratory assistant members in Chemical Engineering
Department Mr. HaftayMulaw , Mr. G/hiwetTadese(lab assistances) others who were helping us
throughout the work. We also would like to say thank you to Quality control members in Addis
Pharmaceutical Factory of Adigrat Mr. K/Mariam, Mr. Eyob and lab assistants of department of
Chemistry for their help on characterization of the raw material and the sample. Last but not
least, we want to acknowledge our family who were on our side in the whole our life in
education in general and our graduate studies in Adigrat University in particular.
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Abstract
Acknowledging the importance of plants and its medicinal value, extraction of Essential Oil had
been done using Steam Distillation method. In different projects Steam Distillation was used to
extract oil from different plant materials like eucalyptus leaves, vegetable leaves, hibiscus leaves,
lemon leaves, marigold flowers, rose flowers, orange peels etc. Research has confirmed centuries
of practical use of essential oils, and we now know that the 'fragrant pharmacy' contains
compounds with an extremely broad range of biochemical effects. Essential oils are so termed as
they are believed to represent the very essence of odor and flavor. The recovery of Essential Oil
(the value added product) from the raw botanical starting material is very important since the
quality of the oil is greatly influenced during this step. There are a variety of methods for
obtaining volatile oils from plants. Steam distillation method was found to be one of the
promising techniques for the extraction of essential oil from plants as reputable distiller and
preserve the original qualities of the plant. The distillation was conducted in Clevenger apparatus
in which boiling, condensing and decantation was done. The effect of different process
parameters, such as particle size, extraction temperature and extraction time on the extraction
yield was investigated. The parameters taken up for the study like the extraction time were found
to significantly affect the extraction yield and quality of the essential oil. Increase in yield was
observed when increase the extraction time of 60 minutes. The optimum essential oil yield was
found 5.33% from 150 gram of orange peel and 1500 ml of distilled water under optimum
particle size, temperature and extraction time of< 200𝜇𝑚, 93.5℃ and one hour respectively.
During laboratory investigation of material balance, the total input of material was 1650 gram,
from this we have got two percent of essential oil by mass using separating funnel, which is
much lower result when we compared to the feed composition of powder peel and amount of
water due to nature of the material, inefficiency of equipment relatively and lack of pressure
control mechanism. Industrially, the processing unit operations of essential oils are not numerous
and complex; it‟s simple and profitable investment with low value of payback period of 3 years
and net profit of dollar 96,351.9942/yr
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Table of content
DECLARATION ........................................................................................................................................... i
Acknowledgment .......................................................................................................................................... ii
Abstract ........................................................................................................................................................ iii
Table of content ........................................................................................................................................... iv
List of figures ............................................................................................................................................. viii
List of table .................................................................................................................................................. ix
List of acronym and abbreviations ................................................................................................................ x
CHAPTER ONE ........................................................................................................................................... 1
INTRODUCTION ........................................................................................................................................ 1
1.1Backgrounds of the Study .................................................................................................................... 1
1.2 Problem statement ............................................................................................................................... 2
1.3 Objectives ........................................................................................................................................... 3
1.3.1 General objective ......................................................................................................................... 3
1.3.2Specific objectives ........................................................................................................................ 3
1.4 Significance of study........................................................................................................................... 3
CHAPTER TWO .............................................................................................................................................. 5
LITERATURE REVIEW ..................................................................................................................................... 5
2.1Essential Oils ........................................................................................................................................ 5
2.1.1 Chemical constituents of Essential oils ................................................................................. 5
2.1.2 Aldehydes ............................................................................................................................. 5
2.1.3 Esters ..................................................................................................................................... 5
2.1.4 Ketones ................................................................................................................................. 6
2.1.5 Lactones ................................................................................................................................ 6
2.1.6 Hydrocarbon: ........................................................................................................................ 6
2.1.7 Terpenes ................................................................................................................................ 6
2.1.8 Monoterpene [C10 H16]: ............................................................................................................. 6
2.1.9 Diterpenes: ............................................................................................................................ 7
2.1.10 Sesquiterpene ............................................................................................................................. 7
2.2 Advantages of essential oil ........................................................................................................... 7
2.2.1Aromatherapy ................................................................................................................................... 7
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2.2.2 Pharmaceutics .............................................................................................................................. 7

2.2.3Antiseptics......................................................................................................................................... 8
2.3 Expectorants and diuretics .................................................................................................................. 8
2.3.1 Spasmolytic and sedative ................................................................................................................. 8
2.3.2 Food ................................................................................................................................................. 8
2.3.3 Cosmetics and Perfumes .................................................................................................................. 8
2.4 Major importing countries .................................................................................................................. 9
2.5 Major exporting countries ................................................................................................................. 10
2.6 Availability of citrus peel waste around the world ........................................................................... 10
2.6.1 Amount of citrus waste produced by the top five producers of orange juice................................. 10
2.7 Orange peel waste composition and value ........................................................................................ 11
2.7.1 D-limonene and orange oil:............................................................................................................ 12
2.8 Methods of extraction ....................................................................................................................... 12
2.8.1 Solvent-Extraction ......................................................................................................................... 12
2.8.2 Maceration ..................................................................................................................................... 13
2.8.3 Cold Pressing ................................................................................................................................. 13
2.8.4 Effleurage....................................................................................................................................... 13
2.8.5 Super Critical CO2 Extraction ....................................................................................................... 13
2.8.6 Steam Distillation Extraction ......................................................................................................... 14
2.8.6.1 Extraction of Essential Oils Using Steam distillation Method .................................................... 14
2.8.9 Advantages of using Steam Distillation ......................................................................................... 15
2.8.10 Methods for Distillation ............................................................................................................... 15
2.9 Parameters Affecting Yield and Quality of Essential Oils................................................................ 18
2.9.2 Improper Design of Equipment...................................................................................................... 18
2.9.3 Material of Fabrication of Equipment ............................................................................................ 18
2.9.4 Condition of Raw Material ............................................................................................................ 18
2.9.5 Time for Distillation ...................................................................................................................... 19
2.9.6 Loading of Raw Material and Steam Distribution ......................................................................... 19
2.9.7 Operating Parameters ..................................................................................................................... 19
CHAPTER THRE ....................................................................................................................................... 20
MATERIALS AND METHOD .................................................................................................................. 20
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3.1 Materials ........................................................................................................................................... 20

3.2 Chemicals.......................................................................................................................................... 20
3.3 Raw Material preparation ................................................................................................................. 20
3.4 Procedures ......................................................................................................................................... 21
Iodine test:........................................................................................................................................... 23
3.5 Characterization of the extracted orange peel essential oil ............................................................... 23
3.5.1 Determination of physical properties ............................................................................................. 23
3.5.2 Determination of the chemical properties ...................................................................................... 25
CHAPTER FOUR....................................................................................................................................... 29
RESULTS AND DISCUSSIONS ............................................................................................................... 29
4.1 Determination of physical properties .......................................................................................... 29
4.1.1entage of orange pPerceel essential oil extracted ............................................................................ 29
4.1.2 Determination of Specific gravity .................................................................................................. 29
4.1.3 Moisture Content ........................................................................................................................... 29
4.1.4 PH value of essential oil ................................................................................................................ 30
4.2 Determination of the chemical properties ......................................................................................... 30
4.2.1 Acid value ...................................................................................................................................... 30
4.2.2 Percentage of free fatty acid (% FFA) ........................................................................................... 30
4.2.3 Determination of Saponification value .......................................................................................... 30
CHAPTER FIVE ........................................................................................................................................ 32
MATERIAL AND ENERGY BALANCE ................................................................................................. 32
5.1 Material balance at laboratory........................................................................................................... 32
5.1.1 Steam distillation ........................................................................................................................... 32
5.1.2 Separating funnel ........................................................................................................................... 32
5.2 Material and energy balance at the industrial scale .......................................................................... 33
5.2.1 Material balance ............................................................................................................................. 33
5.2.1.1Decanter ....................................................................................................................................... 33
5.2.1.2 Material balance on condenser .................................................................................................... 33
5.2.1.3 Material balance on expansion tank ............................................................................................ 34
5.2.1.4 Material balance on mixer........................................................................................................... 34
5.2.2 Energy balance ............................................................................................................................... 35
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5.3.2.1 Energy balance on drier .............................................................................................................. 35

5.3.2.2 Energy Balance for Milling......................................................................................................... 36
5.3.2.3 Energy balance on condenser ...................................................................................................... 37
CHAPTER SIX ........................................................................................................................................... 40
FINANCIAL EVALUATION AND SITE SELECTION .......................................................................... 40
6.1 Market Study..................................................................................................................................... 40
6.1.1 Present Demand and Supply .......................................................................................................... 40
6.1.2 Projected Demand .......................................................................................................................... 41
6.1.3 Pricing and Distribution ................................................................................................................. 41
6.2 Plant Capacity ................................................................................................................................... 42
6.2.1 Production Program ....................................................................................................................... 42
6.2.2 Plant location and Source of Raw Materials .................................................................................. 42
6.3.1 Working capital .............................................................................................................................. 43
6.3.2 Capital investments ........................................................................................................................ 43
6.3.3 Fixed capital investment ................................................................................................................ 43
6.3.4 Machinery and Equipment ............................................................................................................. 44
6.4 Estimation of Fixed Capital Investment............................................................................................ 44
6.4.1 Estimation of direct and indirect cost ............................................................................................ 45
6.4.2 Estimation of Total Production Cost (TPC) ................................................................................... 46
6.5 Economic and Social Benefits and Justification ............................................................................... 50
6.5.1 Profit Generation ............................................................................................................................ 50
6.5.2 Tax Revenue .................................................................................................................................. 51
6.5.3 Import Substitution and Foreign Exchange Saving ....................................................................... 51
6.5.4 Employment and Income Generation ............................................................................................ 51
CHAPTER SEVEN .................................................................................................................................... 52
CONCLUSION AND RECOMMENDATIONS ........................................................................................ 52
7.1 Conclusion ........................................................................................................................................ 52
7.2 Recommendation .............................................................................................................................. 52
REFERENCES ........................................................................................................................................... 53
APPENDIX ................................................................................................................................................. 56
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List of figures
Figure 1: Top five importers share of world essential oils exports. -------------------------------------------------- 9
Figure 2: Top 5 exporter’s shares of world essential oils exports --------------------------------------------------- 10
Figure 3: Main compounds of interest present in orange peel and their occurrence (wt. % dry basis)…..12
Figure 4: D – Limonene structure. ------------------------------------------------------------------------------------------ 12
Figure 5: process flow chart for preparation of orange peel ---------------------------------------------------------- 21
Figure 6: Separation of essential oil from distilled water using separating funnel ------------------------------ 23
Figure 7: conformation test for limonene ---------------------------------------------------------------------------------- 23
Figure 8: titration of ethanol-ether solution with sodium hydroxide ------------------------------------------------ 26
Figure 9: Process diagram of essential oil extraction ------------------------------------------------------------------- 28
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List of table
Table 1:Estimated amounts of WOP produced in main citrus producing countries for the 2013-2014
harvesting season. --------------------------------------------------------------------------------------------------------------- 11
Table 2:Values and unit of physical properties of orange peel oil. -------------------------------------------------- 30
Table 3: chemical properties of essential oil extracted using steam distillation. --------------------------------- 31
Table 4: Projected Demands for Essential Oil ---------------------------------------------------------------------------- 41
Table 5: Machinery and Equipment----------------------------------------------------------------------------------------- 44
Table 7: Estimation of cost ---------------------------------------------------------------------------------------------------- 45
Table 8: Fixed Operating Costs ---------------------------------------------------------------------------------------------- 47
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List of acronym and abbreviations
AFNOR………………………………………………. AgenceFrançaise de Normalisation

CIF……………………………….…..…………….….cost, insurance and freight
EO……………………………………………..………Essential Oil
EU…………………………………….……………….European union
GGPP………………………………………………….GeranylGeranyl pyrophosphate
GRAS…………………………………………………Generally Recognized as Safe
NAFTA………………………………………………..North American Free Trade Area.
SADC………………………………………………….Southern African Development
Community UK…………………………………………………......United Kingdom
USA……………………………………...……………United States of America
USD……………………………………...……………United States Dollar
WOP…………………………………………………...Waste Orange Peel
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CHAPTER ONE
INTRODUCTION
1.1Backgrounds of the Study
Oranges are one of the most ubiquitous crops in the world, grown throughout Asia, the
Mediterranean, Africa, and both South and North America. The United States and Brazil are the
world’s leading producers; most U.S. grown fruit is consumed within the country, while the bulk
of Brazil’s output is exported. In the United States, top orange growing states are Florida,
California, Texas, and Arizona. Florida continues to lead the charge. Oranges are believed to
have originated from a wild variety in the Southern China/Northern India region, although these
cultivars can no longer be found. Originally valued for medicinal purposes, oranges were
brought to the Mediterranean region by Italian traders in the 1400s, and then were introduced
around the globe by Portuguese explorers. The Spanish brought oranges to South America and to
missions in Arizona and California, and the French brought oranges to what is now Louisiana. In
the 1800s, orange groves were planted in Florida to much success. Oranges are some of the most
commonly utilized fruits in the world due to its pleasant taste. Because of the huge consumption
of orange juice throughout the world, a large amount of wet solid waste is produced. This waste
mainly includes orange peels. [1] Orange juice is one of the most widely-consumed beverages
today in Ethiopia. Approximately 50-60% of the processed fruits are transformed into citrus peel,
which is composed of peels, seeds and membrane residues. With the increase in production of
processed fruit wastes generated is increasing enormously. A large amount of these wastes poses
the problem of disposal without causing environmental pollution. These wastes can be
effectively disposed by manufacturing useful by products from them. The peels contain
numerous oil bearing glands that enclose significant amounts of citrus oil. The oil gland present
in orange peels. Orange peel oil has been chosen for extraction because it provides a great
potential for further commercial form. Peel of citrus fruit has numerous glands that contain oil
that is typically recovered as major by product. Each citrus fruit has its own characteristic set of
compounds that comprise the oil and that are responsible for its flavor and aroma to products
such as carbonateddrinks, ice-creams, cakes, air-fresheners and perfumes. In this thesis, for scale
up processing orange peel wastes to be collected separately from the awash agro processing
industry which is located Merti/ Oromia National Regional State and for tasting the samples the
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orange fruits are available from fruit super markets to enjoyment the outer coverage. Recently
developed extraction methods like supercritical carbon dioxide extraction, steam distillation,
solvent-extraction, maceration, and cold pressing and effleurage methods have been used for oil
extraction. The basic parameters influencing the quality of an extract are the solvent used for
extraction, the manufacturing process (extraction technology) used with the type of equipment
employed. The use of appropriate extraction technology, plant material, manufacturing
equipment, extraction method and solvent and the adherence to good manufacturing practices
certainly help to produce a good quality extract. In this thesis, direct steam distillation assisted
extraction of oil of orange peel has been chosen because it processes many advantages over
conventional methods in terms of costing, yielding and time and reproducing better natural
aroma of orange essential oil. It 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 Oil contains components
with boiling points up to 200°C or higher temperatures. In the presence of steam or boiling
water, however, these substances are volatilized at a temperature close to 100°C, at atmospheric
pressure. [2]
1.2 Problem statement

The orange peels after treated as waste materials may create environmental problems for local
communities. Most of the times the local essential oil demand is fulfilled by importing from
foreign producers this may minimize and affect the country economy in its own side and also our
country Ethiopia never attempt to construct such like project plants for the production of
essential oil. In addition to this the country unemployed number is large, this will affect the
country growth by making the productive human powers independence. Currently, extraction of
essential oil from orange peel has remained unexploited. Its application in antioxidant,
aromatherapy, perfumery, soap and other related industries are limited due to lack of adequate
research on the chemical and biological potential of its raw materials. The orange peel content,
which is not well known about its valuable uses, orange peel is one of the most useful materials
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and so far, its many uses are not discovered. Therefore, to solve those all listed problems we
should introduced new plant site in out county.
1.3 Objectives
1.3.1 General objective
 The general objective of this project work is to extract the essential oil from orange peels
by steam distillation.
1.3.2Specific objectives
 To determine the optimum effect of time of heating, particle size and temperature to
extract essential oil from orange peel for the highest yield and quality by using steam
`distillation.
 To know the maximum amount of extracted essential oil at the distillate.
 To determine and identify the optimum yield of essential oil in different conditions. Such
as temperature, particle size, and time of heating.
 To characterize the physical and chemical properties of essential oil. Scope of study
The scope of study is to solve the problem of disposal orange peels as waste materials which will
cause to the environmental problems. Thus we were evaluate the effect of different operating
temperatures, time of heating and the effect of particle size of the essential oil from orange peels.
1.4 Significance of study

Essential oil when produced from orange peel locally can benefit the country for reasons as
stated below;
 Effective solid waste management is one of the most essential elements for an industry to
achieve a sustainable development. Improper treatment of waste will affect peoples'
health and the environment. For the citrus processing industry the disposal of fresh peels
has become a major concern for many years. Orange peels are the major solid by-product
of the overall process. This study can avoid this problem greatly.
 The oil can be a substitute for the imported oil used for multipurpose usage. It can reduce
the importation of oil into the country.
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 Locally produced essential oil means more chance of exporting high quality essential oil,
considering the increase in value of an essential oil in overseas markets it will have great
export potential.
 This project, however, can be really useful for unemployed communities by creating the
work opportunities in their life as it can provide village councils with revenue earning
opportunities as well as making the youths be more working productive for their future
development.
 It attracts the investors to invest in this area with cheap man powers, good climate
conditions, and better profits by providing satisfy utilities and peace.
 The by-products, such as the orange pith and residue can be recover for the another
inputs.
 The erection of the plant will provide essential oil for the industries demand for its flavor
and aroma to products such as carbonated drinks, ice-creams, cakes, air-fresheners,
pharmaceuticals, cosmetics and perfumes.
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CHAPTER TWO
LITERATURE REVIEW
2.1Essential Oils
The term essential oil dates back to the sixteenth century and derives from the drug Quinta
essentia, named by Paracelsus von Hohenheim of Switzerland [4]. Essential oils or “essences”
owe their name to their flammability. Numerous authors have attempted to provide a definition
of essential oils. The French Agency for Normalization: AgenceFrançaise de Normalisation
(AFNOR) gives the following definition “The essential oil is the product obtained from a
vegetable raw material, either by steam distillation or by mechanical processes from the epicarp
of Citrus, or “dry”” distillation. The essential oil is then separated from the aqueous phase by
physical means [5]. This definition encompasses products obtained always from vegetable raw
material, but using other extraction methods, such as using non-aqueous solvents or cold
absorption. Thus, we can define three types of products [6]. Essential oils are soluble in alcohol,
and ether, but insoluble in water. They have a characteristic odor, are usually liquid at room
temperature and have a density less than unity.
2.1.1 Chemical constituents of Essential oils

An Essential Oil contains more than 200 chemical components, but some are many times more
complex. Essential oils consist of chemical compounds which have hydrogen, carbon and
oxygen as their building blocks. [7] They can be essentially classified into two groups: these are
volatile fraction (90 – 95%) and non-volatile residue (1 – 10%).
2.1.2 Aldehydes
Aldehydes are found in lemon-scented oils such as Melissa, lemon verbena, citronella etc. and
include citral, citronellal and neral. They generally have sedative qualities with specific
antiseptic properties. Other known aldehydes include benzaldehyde, cinnamicalderhyde and
perillaldehyde. Essential oils containing aldehydes are helpful in treating inflammation, Candida
and viral infections. [8]
2.1.3 Esters
Esters are formed through the reaction of alcohols with acids. Essential oils containing esters are
used for their soothing, balancing effects. Because of the presence of alcohol, they are effective
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antimicrobial agents. Medicinally, esters are characterized as antifungal and sedative, with a
balancing action on the nervous system. They generally are free from precautions with the
exception of methyl salicylate found in birch and wintergreen which is toxic within the system.
Examples are linlyl acetate in bergamot and lavender and Geranylformate in geranium. [9]
2.1.4 Ketones
Ketones found in plants are used for upper respiratory complaints. They assist the flow of mucus
and ease congestion. Essential oils containing ketones are beneficial for promoting wound
healing and encouraging the formation of scar tissue.
2.1.5 Lactones
Lactones are known to be particularly effective for their anti-inflammatory action, possibly by
their role in the reduction of prostaglandin synthesis and expectorant actions. Lactones have an
even stronger expectorant action than ketones.
2.1.6 Hydrocarbon:
Building blocks of Essential Oil are hydrogen and carbon.
2.1.7 Terpenes
These components generally have names ending with “ene”.Some of them are limonene, pinene,
piperene, camphene etc. These components act as an antibacterial, antiviral, anti- inflammatory,
antiseptic, antiviral and bactericidal. These are further categorized intomonoterpene,
sesquiterpene and diterpenes. When two of theisoprene units are joined head to tail, the result is a
monoterpene, when three are joined;it’s a sesquiterpene and similarly four linked isoprene units
are diterpenes. [10]
2.1.8 Monoterpene [C10 H16]:

Monoterpene are naturally occurring compounds, the majority being unsaturated hydrocarbons
(C10). But some of their oxygenated derivatives such as alcohols, Ketones, and carboxylic acids
have known as monoterpenoids. Two isoprene units are present in these branched-chain C10
hydrocarbons and are widely distributed in nature with more than 400 naturally occurring
monoterpenes.
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2.1.9 Diterpenes:
Isoprene has been an integral part in most of the components as there are four isoprene units in
Diterpenes. By Stem Distillation method we cannot detect Diterpenes as this molecule is too
heavy to allow for evaporation, so it is rarely found in distilled Essential Oils. In a similar
manner to monoterpenes, Diterpenes arise from metabolism of geranyl pyrophosphate (GGPP).
Therapeutically Diterpenes have limited importance and are used in certain sedatives (coughs) as
well as in antispasmodics and anxiolytics.
2.1.10 Sesquiterpene
Sesquiterpenes are biogenetically derived from farensyl pyrophosphate and in structure may be
linear, monocyclic or bicyclic. They constitute a very large group of secondary metabolites,
some having been shown to be stress compounds formed as a result of disease or injury. These
are having properties like anti-inflammatory, anti-septic, analgesic and anti-allergic.
2.2 Advantages of essential oil
2.2.1Aromatherapy
Aromatherapy is a form of alternative medicine that uses volatile plant materials, known as
essential oils, and other aromatic compounds for the purpose of altering a person's mood,
cognitive function or health. Science has discovered that our sense of smell plays a significant
role in our overall health. [11] Since ancient times Essential Oils have been used in medicine
because of their medicinal properties, for example some oils have antiseptic properties. In
addition, many have an uplifting effect on the mind, though different essential oils have different
properties. When Essential Oil is inhaled it goes directly from olfactory system to limbic system
of the brain. Brain responds to the particular scent affecting our emotions and chemical balance.
Essential Oils also absorbed by the skin and carried throughout the body via the circulatory
system to reach all internal organs. We can be benefited by choosing carefully the desired and
suitable oils which can promote overall health. Benefits depend upon the unique nature of each
person’s response to an aromatic stimulus. [1]
2.2.2 Pharmaceutics
Essential Oils have versatile applications in pharmaceutics. Some of the applications are listed
below.
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2.2.3Antiseptics
The antiseptic properties of Essential Oil make them active against wide range of bacteria as on
antibiotic resistant strains. In addition to this they are also against fungi and yeasts. The most
common sources of essential oils used as antiseptics are: Cinnamon, Thyme, Clover, Eucalyptus,
Culinsavory, and Lavender. Citral, geraniol, linalool and thymol are much more potent than
phenol. [1]
2.3 Expectorants and diuretics

When used externally, essential oils like (L‟essence de terebenthine) increase microcirculation
and provide a slight local anesthetic action. Till now, essential oils are used in a number of
ointments, cream and gels, whereby they are known to be very effective in relieving sprains and
other articular pains. Oral administration of essential oils like eucalyptus or pin oils, stimulate
ciliated epithelial cells to secrete mucus. On the renal system, these are known to increase
vasodilation and in consequence bring about a diuretic effect.
2.3.1 Spasmolytic and sedative

Essential oils from the Umbellifereae family, Mentha species and verbena are reputed to
decrease or eliminate gastrointestinal spasms. These essential oils increase secretion of gastric
juices. In other cases, they are known to be effective against insomnia.
2.3.2 Food
EOs is used for flavoring in food and is accepted by the Food and Drug Administrations as
additives in certain type of foods. Citrus oils are used for food and beverages and they are
Generally Recognized as Safe (GRAS), being a good starting point for the use of EOs as
antimicrobials within the food industry. Recently, a study was carried out to evaluate the
inhibitory potential of EOs extracted from the orange peels of citrus by steam distillation
process.
2.3.3 Cosmetics and Perfumes

Mixtures of volatiles and EOs isolated from plants represent the „essence‟ or odoriferous
constituents of the plants. They have been used since early days because of pharmaceutical
properties and also as flavoring agents in the manufacture of perfumes and cosmetics.
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2.3.4 Detergent
Citrus EOs is processed into various formulations for industrial cleaning applications and as
sustainable alternatives to traditional solvents.
2.4 Major importing countries

Quite a few countries dominate the world’s import market in essential oils. Figure 2.1 shows
five countries that are leading importers. The US is leading with a 14% share or US$390.9m
worth of imports in the world. France, the UK and Germany are not only leaders in the EU but
also amongst the five largest world importers. As it has been indicated above, essential oils
products are mainly used in developed countries as their consumers are more sophisticated
compared to other consumers in other parts of the world. Added to this is their purchasing power.
Other regions such as Oriental lands, China and Japan mainly use essential oils for reasons other
than conventional ones although the proliferation of western culture has had a huge impact in
changing the usage of essential oils products. In Asia essential oils are also used for cultural and
religious purposes. [12]
Figure 1: Top five importers share of world essential oils exports.
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2.5 Major exporting countries
Figur.2 shows the leading five exporters of essential oils in the world. Together they exported
US$936.3m worth of essential oils product representing about 40% of world exports. Again the
US is a major exporter with US$351.7m worth of exports or 17% share of world total exports.
The US is followed by France, India, the UK, and Brazil. The leading export destination for three
of the five countries is the EU (France, UK and US). Brazil and India export mainly to NAFTA,
with 43% and 32% worth of exports destined to that region in 2005, the equivalent of US$45.3m
and US$53.1m, respectively. The SADC region exports less that 1% of essential oils products on
average to these countries. Only 2% of exports from SADC are destined for the UK with France
and India each importing about 1% in 2005. [12]
Figure 2: Top 5 exporter’s shares of world essential oils exports
2.6 Availability of citrus peel waste around the world
2.6.1 Amount of citrus waste produced by the top five producers of orange juice
Citrus fruits are extensively cultivated around the world. They are considered as a commodity
product, similar to coffee and tea in terms of international trade. They include oranges, lemons,
limes, grapefruits and tangerines. Globally, 51.8 million metric tons of orange fruits were
produced for the 2013-2014 harvesting season, 40% of which was grown for the sole purpose of
being processed into juice. [13] The processing industry creates a large amount of waste
byproduct in the form of peel, seeds, rag (the membranes between the citrus segments) and pulp
(juice sacs), representing ~ 50-60% of the whole fruit being discarded after juicing. [14]
Assuming 50% of the weight of a citrus fruit is discarded in the form of peel when processed, the
corresponding amounts of waste orange peel arising from the processing of orange fruits have
been estimated based on the latest report published by the United States Department of
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Agriculture. The data can be found in the table below. The data reported in the table show that of
the top five orange processing nations, three are also the largest orange fruit growing nations. It
should be noted that the data does not take into account either “off spec” orange fruits disposed
of prior to processing or fruits destined for human consumption but destroyed to regulate the
selling price (which is a regular practice in Spain for example). These fruits could also be used
for valorization purposes. The numbers show how citrus peel and more specifically orange peel,
which is a by-product of the juicing industry, represent a high volume waste stream occurring on
both hemispheres of the globe. [15]
Table 1:Estimated amounts of WOP produced in main citrus producing countries for the 2013-
2014 harvesting season.
[13]
Country Amount of orange fruits produced for processing Associated amounts of waste orange
purposes (metric tons) peel produced following processing
(metric tons)
Brazil 10,935,000 5,467,500

U.S.A 5,423,000 2,711,500
E.U 1,069,000 534,500
Mexico 1,350,000 675,000
China 600,000 300,000
Total 19,377,000 9,688,500
2.7 Orange peel waste composition and value
Orange peel is of particular interest given the variety of compounds it contains (see Figure). It
has been recognized as an interesting source of dietary fiber, natural antioxidants, food colorants
and flavors. D-limonene and pectin both have applications in the food and cosmetic industries
amongst others; as a fragrance compound and a thickener respectively.[16] The sequential
extractions of those compounds for valorization purposes in the food and chemical sectors
amongst others, represents an interesting research avenue, from both academic and economic
angles. The main components present in orange peel are summarized in Figure below together
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with their associated weight percentage on a dry basis. WOP can contain up to 80% water. [17,
18]. In the following section, the current commercial extraction process used will be described.
Figure 3: Main compounds of interest present in orange peel and their occurrence (wt. % dry
basis).[19, 20]
The peel is mainly composed of pectin, hemicelluloses and cellulose (50-70%). Lignin typically
represents less than 10% of the peel on a dry weight basis. [21]
2.7.1 D-limonene and orange oil:

D-limonene can be obtained from whole fruits if the harvest is dedicated to oil production or as a
by-product of juice production. By D-limonene, the material referred to often corresponds in the
literature to the peel oil, or essential oil obtained by steam distillation. [22]
Figure 4: D – Limonene structure.
2.8 Methods of extraction

The following are the methods of extraction of Essential Oil and their drawbacks.
2.8.1 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. 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 waxy mass that remains is
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known as the concrete. 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. [23]
2.8.2 Maceration
Maceration actually creates more of “infused oil” rather than an Essential Oil. Plant matter is
soaked in vegetable oil, heated and strained at which point it can be used for massage. This
method is not desirable because it changes the composition of oil. [24]
2.8.3 Cold Pressing

This method is used to extract the Essential Oils from citrus rinds such as orange, lemon,
grapefruit and bergamot. This method involves the simple pressing of the rind at about 120
degrees F to extract the oil. The rinds are separated from the fruit, are ground or chopped and are
then pressed. The result is a watery mixture of essential oil and liquid which will separate given
time. Little alteration from the oil's original state occurs – these citrus oils retain their bright,
fresh, uplifting aromas like that of smelling a wonderfully ripe fruit. The drawback of this
method is, oils extracted using this method have a relatively short shelf life. [25]
2.8.4 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.
[26]
2.8.5 Super Critical CO2 Extraction

Supercritical CO2 extraction involves carbon dioxide heated to 87 degrees F and pumped
through the plant material at around 8,000 psi, under these conditions; the carbon dioxide is
likened to a 'dense fog' or vapor. With release of the pressure in either process, the carbon
dioxide escapes in its gaseous form, leaving the Essential Oil behind. The usual method of
extraction is through steam distillation. After extraction, the properties of a good quality essential
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oil should be as close as possible to the "essence" of the original plant. The key to a 'good'
essential oil is through low pressure and low temperature processing. High temperatures, rapid
processing and the use of solvents alter the molecular structure, will destroy the therapeutic value
and alter the fragrance. [27]
2.8.6 Steam Distillation Extraction

Distillation is suitable for hard-to-extract or coarse plant material, such as bark, roots, and seeds.
In this process, the plants soak in water and steam is circulated through this plant and water
mixture. Throughout the entire process, the same water is continually recycled through the plant
material. This method allows faster extraction of essential oils from hard-to-extract plant
materials. [24]
2.8.6.1 Extraction of Essential Oils Using Steam distillation Method

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°C or higher temperatures. In the presence of steam or boiling water, however,
these substances are volatilized at a temperature close to 100°C, at atmospheric pressure. Fresh,
or sometimes dried, botanical material is placed in the plant chamber of the still and the steam is
allows 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. 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. [28] It is possible that longer distillation times may
give more complete oil.
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2.8.9 Advantages of using Steam Distillation

The advantage of Steam Distillation is that it is a relatively cheap process to operate at a basic
level, the availability and the properties of oils produced by this method are not altered. As steam
reduces the boiling point of a particular component of the oil, it never decomposes in this
method. This method apart from being economical, it is also relatively faster than other methods.
[29].
2.8.10 Methods for Distillation

There are three types of distillation for isolating essential oils from plant materials:
A. Water distillation
B. Water and steam distillation
C. Direct steam distillation
A. Water Distillation
In this method, the material is completely immersed in water, which is boiled by applying heat
by direct fire, steam jacket, closed steam jacket, closed steam coil or open steam coil. The main
characteristic of this process is that there is direct contact between boiling water and plant
material. When the still is heated by direct fire, adequate precautions are necessary to prevent the
charge from overheating. Water distillation possesses one distinct advantage, i.e. that it permits
processing of finely powdered material or plant parts that, by contact with live steam, would
otherwise form lumps through which the steam cannot penetrate. Other 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. The main
disadvantage of water distillation is that complete extraction is not possible. Besides, certain
esters are partly hydrolyzed and sensitive substances like aldehydes tend to polymerize. Water
distillation requires a greater number of stills, more space and more fuel. It demands
considerable experience and familiarity with the method. Oil components like esters are sensitive
to hydrolysis while others like acyclic monoterpene hydrocarbons and aldehydes are susceptible
to polymerization (since the pH of water is often reduced during distillation, hydrolytic reactions
are facilitated).
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 Oxygenated components such as phenols have a tendency to dissolve in the still water, so
their complete removal by distillation is not possible.
 As water distillation tends to be a small operation (operated by one or two persons), it
takes a long time to accumulate much oil, so good quality oil is often mixed with bad
quality oil.
 The distillation process is treated as an art by local distillers, who rarely try to optimize
both oil yield and quality.
 Water distillation is a slower process than either water and steam distillation or direct
steam distillation.
B. Water and Steam Distillation
In water and steam distillation, the steam can be generated either in a satellite boiler or within the
still, although separated from the plant material. Like water distillation, water and steam
distillation is widely used in rural areas. Moreover, it does not require a great deal more capital
expenditure than water distillation. Also, the equipment used is generally similar to that used in
water distillation, but the plant material is supported above the boiling water on a perforated grid.
In fact, it is common that persons performing water distillation eventually progress to water and
steam distillation. It follows that once rural distillers have produced a few batches of oil by water
distillation, they realize that the quality of oil is not very good because of its still notes (subdued
aroma). As a result, some modifications are made. Using the same still, a perforated grid or plate
is fashioned so that the plant material is raised above the water. This reduces the capacity of the
still but affords a better quality of oil. If the amount of water is not sufficient to allow the
completion of distillation, a cohobation tube is attached and condensate water is added back to
the still manually, thereby ensuring that the water, which is being used as the steam source, will
never run out.
Advantages
 Higher oil yield.

 Components of the volatile oil are less susceptible to hydrolysis and polymerization (the
control of wetness on the bottom of the still affects hydrolysis, whereas the thermal
conductivity of the still walls affects polymerization).
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 If refluxing is controlled, then the loss of polar compounds is minimized.

 Oil quality produced by steam and water distillation is more reproducible.
 Steam and water distillation is faster than water distillation, so it is more energy efficient.
Disadvantages
 Due to the low pressure of rising steam, oils of high-boiling range require a greater
quantity of steam for vaporization - hence longer hours of distillation.
 The plant material becomes wet, which slows down distillation as the steam has to
vaporize the water to allow it to condense further up the still.
 To avoid that the lower plant material resting on the grid becomes waterlogged, a baffle
is used to prevent the water from boiling too vigorously and coming in direct contact with
the plant material.
C. Direct Steam Distillation
As the name suggests, direct steam distillation is the process of distilling plant material with
steam generated outside the still in a satellite steam generator generally referred to as a boiler. As
in water and steam distillation, the plant material is supported on a perforated grid above the
steam inlet. A real advantage of satellite steam generation is that the amount of steam can be
readily controlled. Because steam is generated in a satellite boiler, the plant material is heated no
higher than 100 and, consequently, it should not undergo thermal degradation. Steam distillation
is the most widely accepted process for the production of essential oils on large scale.
Throughout the flavor and fragrance supply business, it is a standard practice. An obvious
drawback to steam distillation is the much higher capital expenditure needed to build such a
facility.
Advantages
 Amount of steam can be readily controlled.

 No thermal decomposition of oil constituents.
 Most widely accepted process for large-scale oil production, superior to the other two
processes.
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Disadvantage
 Much higher capital expenditure needed to establish this activity than for the other two
processes.
2.9 Parameters Affecting Yield and Quality of Essential Oils

The yield and quality of essential oil from steam distillation is affected by the various process parameters.
2.9.1 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. Cyprus), 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.
2.9.2 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.
2.9.3 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.
2.9.4 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.
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2.9.5 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 agar wood, these
highballing fractions are valuable due to the quality of their aromas. Thus, the time of distillation
must be chosen with due care.
2.9.6 Loading of Raw Material and Steam Distribution

Improper loading of the material may result in steam channeling, causing incomplete
distillation. The material 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.
2.9.7 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.
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CHAPTER THRE
MATERIALS AND METHOD
3.1 Materials
 Round bottom flask
 Basket heater
 Distillation unit
 Thermometer
 Measuring cylinder
 Glass bowl
 Conical flask
 Beaker
 Separating funnel
3.2 Chemicals
 Iodine
 Diethyl ether
 Phenolphthalein
 Ethanol
 Potassium hydroxide (KOH)
 Sodium hydroxide (NaOH)
3.3 Raw Material preparation

To begin the experiment, the raw materials should be prepared. The orange peels were collected
from any juice house of Adigratcity and we have bought the normal orange fruit from the market
and peeled the orange covers manually and dried the peels by exposed to the sun for 2 or 3
consecutive days. Finally ground the material by using rotary mortal grinder (model: CE261).
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Collection of
orange peels
Washing
Weighing
Drying
Weighing
Grinding
Packaging
Figure 5: process flow chart for preparation of orange peel
3.4 Procedures
I. Pretreatment of the collected orange peel by using tap water
The collected orange peels were infected by various conditions, such as during storage,
transportation and other conditions. For high quality extraction of essential oil the orange peels
had been washed or treated by water in order to avoid the dirty materials.
II. Weighing the pretreated orange peel by using electronic balance
After pretreatment of the orange peels, estimation of weight of the orange peels was considered
to know the moisture content for the further estimation investigation.
III. Drying the orange peel for two or three days by exposing at the sun
The completion of weighing the moisture content guides to the drying process until the
maximum drying process achieved.
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IV. Weighing the dried peel by using electronic balance

The weighing process is the same as before drying condition by using electronic balance after
complete drying of the orange peel. Finally we have estimated here the moisture content of
orange peel.
V. Grinding the dried orange peel by using mortar grinder
The dried orange peel is conducted to size reduction by using mortar grinder for 5 – 8 minutes.
VI. Making sieve analysis to know the effect of particle size within the extraction
The ground orange peels must be sieved in order to carry out different particle sizes by using
710,500, 250 and 200𝜇𝑚 mesh sizes to know their effects during extraction.
VII. Final we have conducted the extraction process by using steam distillation.
The Distillation set up is arranged. It consists of distillation flask, Basket heater, horizontal
condenser and a conical flask. 150g of pre-treated orange peels sample is taken in a distillation
flask. To that 1500ml of water is added. Heat is supplied to the distillation unit by temperature
controlled basket heater.
 At the initial stage, experiment was carried out at a Temperature of 88 for 36 min. time
period. The distillate is collected in a conical flask. After the extraction the distillate
layers were observed, one dense layer and other less dense layer. This was then separated
using a separating funnel. The less dense upper layer is the citrus oil. This oil is then
stored in a glass bottles.
 The experiments were continued keeping distillation time and solid to solvent ratio
constant varying the temperature of distillation at an interval from 88℃ to 93.5° . Here,
the optimum distillation temperature was conducted as 93.5℃ .
 In the next phase, experiments are carried out keeping the distillation temperature and
solid to solvent ratio constant by varying the distillation time at an interval of 15 min.
Finally, 60 minute was investigated as optimum.
 In the final phase, experiments are carried out keeping distillation time and temperature
constant by varying the solid particle size. The experiment was done by four type of mesh
size sieve analysis; these are 710, 500, 250 and< 200𝜇𝑚 . From the laboratory analysis
we have got maximum product <200𝜇𝑚 , which is 8.0 gram of oil sample. But with the
similar procedure of this project, we have got the literature that was extracted from 50
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gram of peel powder and 750 gram of water with 80 minute heating time and at the
temperature of 100℃ has been extracted 0.5 gram of oil. [31] This result is differing from
our analysis due to the effect of raw material proportion, geographical location, particle
size and variety of orange peel and operating conditions.
Figure 6: Separation of essential oil from distilled water using separating funnel
Iodine test:
A dilute iodine-water solution was prepared and taken in a test tube. To that citrus oil extracted
from orange peels is added. If limonene is present in the oil extracted, the color of the iodine -
water gets changes from red brown to pale yellow. This is because of the fact that the iodine
present in the iodine – water solution occupies the space between the two double bonds present
in limonene. The conformation test for Limonene is shown below.
Figure 7: conformation test for limonene
3.5 Characterization of the extracted orange peel essential oil

The yield of essential oil, pH value, the acid value, Saponification value, ester value, Percentage
of free fatty acid (% FFA) of waste orange peel essential oil were performed and compared with
literatures.
3.5.1 Determination of physical properties

Specific gravity
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𝑀𝑎𝑠𝑠𝑜𝑓𝑠𝑎𝑚𝑝𝑙𝑒𝑙
Sp.gr =𝑀𝑎𝑠𝑠𝑜𝑓𝑎𝑛𝑒𝑞𝑢𝑎𝑙𝑣𝑜𝑙𝑢𝑚𝑒𝑜𝑓𝑤𝑎𝑡𝑒𝑟……………………………………………….. (3.1)
Moisture Content Determination

600 gm. moist waste orange peel was weighed and dried at the sun and the weight was measured
every 6 hrs. The procedure was done repeatedly until a constant weight was obtained. The
percentage moisture in the peel was calculated using the following formula;
𝑊1−𝑊2
Moisture content (%) = 𝑋100 …………………………………………………….. (3.2)
𝑊1
Where:
W1 = original weight of the sample before drying; and
W2 =weight of the sample after drying.
Size reduction and Sieve analysis of the peel

The moisture was removed by full sun drying. The dried orange peels were crushed in mortar
grinder mill. The sample was sieved using set of sieves sizes arranged in ascending order 200 ,
250 , 500 and 710m to obtain particular sizes. This was aimed to investigate the effect of
particles size on yield.
Percentage of orange peel essential oil extracted

The percentage yield of essential oil was calculated using two formulas, i.e. percentage of oil
yield and percentage of extraction yield.
𝑀𝑎𝑠𝑠𝑜𝑓𝑜𝑖𝑙
Percentage of oil yield =𝑀𝑎𝑠𝑠𝑜𝑓𝑜𝑖𝑙𝑝𝑒𝑟𝑐𝑒𝑛𝑡𝑖𝑛𝑡ℎ𝑒𝑜𝑟𝑎𝑛𝑔𝑒𝑝𝑒𝑒𝑙 𝑥100………………………… (3.3)
PH value of essential oil

2g of the sample was taken and putted in a clean dry 25ml beaker and distilled water was added
to the sample in the beaker and stirred slowly. [32]
Procedures
Three major steps are involved in the experiment. They are
 Preparation of Reagents
 Calibrating the Instrument
 Testing of Sample
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Preparation of reagents
 Buffer Solution of pH 2.0
 Buffer Solution of pH 7.0
 Buffer Solution of pH 9
Calibrating the instrument

Using the buffer solutions calibrate the instrument to check the known value of PH.
Testing of sample
 In a clean dry 25 ml beaker take the water sample and place it in a magnetic stirrer, insert
the Teflon coated stirring bar and stir well.
 Now place the electrode in the beaker containing the oil sample and check for the reading
in the pH meter. Wait until you get a stable reading.
 The pH of the given oilsampleis 5.73.
3.5.2 Determination of the chemical properties

Acid value:is the mass of potassium hydroxide (KOH) in mg that is required to neutralize one
gram of chemical substance. [33]
Method and procedure
Reagents
 Phenolphthalein indicator: Weighed 1 g of phenolphthalein and dissolved in 100 ml
of ethanol.
 Sodium hydroxide titrant: Weighed accurately 4.0 g of sodium hydroxide and place it
in a 1000-mL volumetric flask. Make up to the mark with water.
 Ethanol-ether solution: Prepared a mixture of ethanol and diethyl ether (1:1, v/v).
Neutralize with sodium hydroxide titrant and added 1.0 ml of phenolphthalein
indicator until pink coloration is observed. Freshly prepare the solution.
Titration of test solution

Unless otherwise specified, weighed accurately a quantity of the essential oil being examined
and placed it in a 250-mL conical flask, then add 50 ml of ethanol-ether solution.Shaked it well.
If necessary, reflux the mixture gently until the substance is completely dissolved. Titrate the
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solution with sodium hydroxide titrant until pink coloration can be observed which persists for
30s. Measured the volume of sodium hydroxide titrant used.
Figure 8: titration of ethanol-ether solution with sodium hydroxide
56.1𝑥(𝑣𝑜𝑙𝑢𝑚𝑒𝑜𝑓𝑎𝑙𝑐𝑜ℎ𝑜𝑙𝑖𝑐𝑣𝑎𝑙𝑢𝑒𝑠𝑜𝑑𝑖𝑢𝑚ℎ𝑦𝑑𝑟𝑜𝑥𝑖𝑑𝑒𝑥𝑛𝑜𝑟𝑚𝑎𝑙𝑖𝑡𝑦)
Acid value = ……………………. (3.4)
𝑊𝑒𝑖𝑔ℎ𝑡𝑜𝑓𝑠𝑎𝑚𝑝𝑙𝑒𝑖𝑛𝑔𝑟𝑎𝑚
Determination of Saponification value

The Saponification value is the number of mg of potassium hydroxide required to saponify
1gram of oil.
Materials
 1 gram essential oil
 Solvent (equal volumes of 95% ethanol and ether)
 Alcoholic KOH (0.5 mol/liter)
 Reflux condenser.
 Boiling water bath.
 Phenolphthalein.
 Hydrochloric acid (0.5 mol/liter)
 Burettes (10 ml and 25 ml)
 Conical flasks (250ml)
Procedures
 Accurately weighed 1g of oil in a small beaker and dissolved it in about 3ml of the
solvent.
 Quantitatively transferred the contents of the beaker to a 250 ml conical flask by rinsing
the beaker three times with further milliliters of solvent.
 Added 25ml of alcoholic KOH and attached to a reflux condenser.
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 Set another reflux condenser as blank with everything present except the oil.
 Heated both flasks on a boiling water bath for 30 min.
 Leave to cool to room temperature and titrated with 0.5mol/liter HCl and used
phenolphthalein as indicator. Until the pink color disappears.
 Recorded the readings as T ml for test and B ml for blank.
Calculations
The difference between the blank and the test reading gives the number of milliliters of KOH
required to saponify 1g oil.
You can use this formula to calculate the saponification value:
1ml (0.5 N HCl) = 28.05 mg KOH
(B-T) = S
(𝐵−𝑇)𝑋28.05
Saponification value=𝑊𝐸𝐼𝐺𝐻𝑇 𝑂𝐹 𝑂𝐼𝐿=mgKOH/1gm………… (3.5)
Percentage of free fatty acid (% FFA)

Free fatty acid was determined using the following equation:
Where: K = Constant (0.503)
AV = is acid value of the oil
% FFA = 0.503 AV……………………………………………………………………….. (3.6)
Ester value
The determination of the ester content is of great importance in the evaluation of many essential
oils. Most esters, which occur as normal constituents of essential oils, are esters of monobasic
acids. Ester value may be defined as "the number of milligrams of potassium hydroxide required
to neutralize the acids liberated by the hydrolysis of esters present in 1g of the essential oil
materials”. The value of ester can be calculated as follow:
Ester value = saponification value – acid value…………………………………………….. (3.7)
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Water
Pneumatic
Milling Scrubber
Drier Orange peel
Energy Energy
Storage
tank Decanter
Water Condenser oil
Expansi
Mixer on tank Water
Conveyer
Pump To biogas plant
Figure 9: Process diagram of essential oil extraction
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CHAPTER FOUR
RESULTS AND DISCUSSIONS
4.1 Determination of physical properties
4.1.1entage of orange pPerceel essential oil extracted

The percentage yield of essential oil was calculated using two formulas, i.e. percentage of oil
yield and percentage of extraction yield.
𝑀𝑎𝑠𝑠 𝑜𝑓 𝑜𝑖𝑙
Percentage of oil yield =𝑀𝑎𝑠𝑠 𝑜𝑓 𝑜𝑖𝑙 𝑝𝑒𝑟𝑐𝑒𝑛𝑡 𝑖𝑛 𝑜𝑟𝑎𝑛𝑔𝑒 𝑝𝑒𝑒𝑙 𝑥100
8.0𝑔𝑚
= 150 𝑔𝑚 × 100 =5.33
4.1.2 Determination of Specific gravity

𝑀𝑎𝑠𝑠 𝑜𝑓 𝑠𝑎𝑚𝑝𝑙𝑒
Sp.gr =𝑀𝑎𝑠𝑠 𝑜𝑓 𝑒𝑞𝑢𝑎𝑙 𝑣𝑜𝑙𝑢𝑚 𝑜𝑓 𝑤𝑎𝑡𝑒𝑟
Density = 𝑉𝑜𝑙𝑢𝑚 𝑜𝑓 𝑜𝑖𝑙
0.001𝑘𝑔 𝑜𝑓 𝑜𝑖𝑙
Density = 0.0000011905𝑚3
Density = 839kg/
𝜌𝑜𝑖𝑙
Specific gravity =𝜌𝑤𝑎𝑡𝑒𝑟 = 0.839
The Specific gravity is < 1, this indicates that the oil can suspended on the surface of water.
4.1.3 Moisture Content

𝑤1−𝑤2
Moisture content (%) = 𝑥100
𝑤1
Where:
W1 = 600gm. (before drying)
W2 = 150 gm. (after drying)
600−150
Moisture content (% = 𝑥100 =75%
600
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4.1.4 PH value of essential oil

The pH of orange peel essential oil was measured by pH meter. Its value was recorded as 5.73.
Table 2:Values and unit of physical properties of orange peel oil.
Physical properties Results

Molecular weight 136.2 gm./mol
Molecular formula C10H16
Class/ family Hydrocarbon
Specific gravity 0.839
Density 839 ⁄𝑚3
Percentage of oil 5.33%
Moisture content 75%
Color Pale yellow
Odor Characteristics odor
Melting point 74.0℃
Boiling point 176℃
Solubility in water Insoluble
Solubility in alcohol Soluble
PH. Value 5.73
4.2 Determination of the chemical properties

4.2.1 Acid value
56.1𝑥(.1𝑥10𝑚𝑙)
Acid value= = 28.05 ml/gm
2𝑔𝑚
4.2.2 Percentage of free fatty acid (% FFA)

Free fatty acid was determined using the following equation:
Where: K = Constant (0.503)
AV = is acid value of the oil
% FFA = 0.503 AV
= 0.503x 28.05 = 14.11
4.2.3 Determination of Saponification value
The saponification value is the number of mg of potassium hydroxide required to saponify 1
gram of oil/fat.
0.1 𝑁×𝐾𝑂𝐻𝑚𝑙×51
Saponification value (S)= =mgKOH
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0.1×19𝑀𝐿×51
S= 1𝐺𝑀
= 96.9 ml/gm
4.2.4 Determination of ester value
Ester value = (96.9 – 28.05) = 69 ml/gm.
Table 3: chemical properties of essential oil extracted using steam distillation.

Chemical properties Results Units
Acid value 28.05 mL/gm.
Percentage of free fatty acid (% FFA) 14.11 ---
Saponification value 96.9 mL/gm.
Ester value 69 mL/gm.
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CHAPTER FIVE
MATERIAL AND ENERGY BALANCE
5.1 Material balance at laboratory
5.1.1 Steam distillation

Assumptions:
I. No consumption
II. No generation
III. Reference temperature = 25oc
IV. Heat loss is negligible
V. Complete condensation on the distillation,
VI. Unsteady state condition.
F=1650g Distillation 250gm (distilled water +

1500gm distilled water+150g essential oil)
Orange peel powder
Overall material balance; (x) Sludge

Inlet = outlet
1650 gm = 250gm + sludge
Sludge(X) = 1400 gm.
5.1.2 Separating funnel

8.0gm oil
Separating funnel
250gm (distilled water +essential oil)
Unknown (X), Water (98%)
In = out
250gm = X+ 8.0gm
X = 242 gm
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5.2 Material and energy balance at the industrial scale
5.2.1 Material balance

Assumption:
 The feed rate in to washer = 185kg/hr. of wet orange peels.
 Basis of calculation = 1 hour
 The feed rate to the decanter input is 98 percent of water
 2 percent output of essential oil
 0.1percent of loss of powder during transportation from milling to mixer
5.2.1.1Decanter
Oil (18.18 kg/hr.)

Decanter
Unknown(X)
Waste water (890.82 kg/hr.)
Inlet = outlet
X = 18.18 kg /hr. + 890.82 kg /hr.
X = 909 kg/hr.
5.2.1.2 Material balance on condenser

V=?
Qc
L=? 909 Kg/hr (distillate)
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Inlet = outlet
V = L + 909 kg/hr.; but the reflex ratio is given as 2.5; this means:-
R =𝐷𝐿 = 2.5
L/ distillate = 2.5 => L = 2.5* 909kg/hr.
L = 2272.5kg/hr.
V = L+ D
Then V = 2272.5 kg/hr. + 909 kg/hr. => V = 3181.5kg/hr.
5.2.1.3 Material balance on expansion tank

Assume the sludge is 89% of output.
(X) kg/hr (X) kg/hrOil + water (3,181.5 kg/hr.)

Expansion
Tank
Sludge = 2,831.5 kg/hr.

Overall balance
In = out
(X) kg/hr. = 3,181.5 kg/hr. + 0.89*3,181.5 kg/hr
(X) kg/hr. = 6,013 kg/hr.
5.2.1.4 Material balance on mixer

Distilled water(X)
6,013kg/hr.
Orange peel powder Mixer
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Inlet = outlet
Orange peel powder from storage tank to the mixer is 41.615kg/hr.
Orange peel powder + distilled water = 6,031 kg/hr.
41.625kg/hr. + distilled water(X) = 6,031 kg/hr.
Distilled water(X) = 5,989.375 kg/hr.
5.2.2 Energy balance

Assumptions:
 Steady state conditions,
 No heat lost through the walls of the condenser.
 Reference temperature = 25°c,
 Complete condensation on the distillation,
 Feed of temperature of distillation =35℃

 Drying temperature = 120oc
Basic data: We have the following basic information from vapor equilibrium data.
 Boiling point of essential oil= 176℃
 Heat of capacity for essential oil = 23 kJ/kg .k
 Heat of capacity for water = 4.2kJ/kg .k
 Heat of capacity for sludge = 3.671KJ/Kg.K
 Latent heat of essential oil @ 176℃ = 29,882 kj/kg
 Latent heat of water at 176℃ = 2256.9kj/kg.
 XOF= mass fraction of essential oil at the feed
 XWF = mass fraction of water at the feed.
5.3.2.1 Energy balance on drier

Assume: after drying the raw material mass reduced by 75%.
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Feed = 185kg/hr. Pneumatic drier TOUT = 30℃

Air + fuel
Tin = 120℃
The energy required is Q = m Cp ΔT

Where m =mass of wet orange peel = 185 kg/hr.
After drying = 46.25 kg/hr.
Cp = specific heat of orange peel = 3.9kj/kg.
ΔT = Tf- Ti
Xf = mole fraction of orange peel = 10%
Xw = mole fraction of water = 90%
Ein=Eout
MinCp ΔT=Eout
Cp = Cpf*Xf+ Cpf *Xw = = 3.90*0.1 + 4.2*0.9 = 4.17 j/kg
Qout = mCp ΔT =185 kg/hr.*4.17kj/Kg.K* (120 - 30) k = 69,430.5kj/hr.
5.3.2.2 Energy Balance for Milling

Assume: there is 0.1% loss of orange peel during milling.
Mdp = 46.25 kg/hr.

T = 25℃. Milling T = 60℃
Mm = 41.625 kg/hr.
Mm = 41.625 kg/hr.
Where:
Mdp = mass of dried orange peel
Mm = mass of orange peel after milling
Cp = specific heat of orange peel = 3.9kj/kg
ΔT = Tf- Ti
From material balance the mass flow rate is 46.25kg/hr.
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Q = mCp ΔT = 46.25 kg/hr*3.9kj/Kg.K* (60 -25) ◦k = 6,313.125kj/hr.
5.3.2.3 Energy balance on condenser

From material balance Mass of vapor = 634.13 kg/hr.
Hv=?
QC =?
HL =? HD
From vapor equilibrium data; Boiling point of essential oil of orange peel = 1760C
At steady state
Input = Out put
HV= QC + HD + HL; But HL= HD = 0
Then; HV= QC
HV = Latent + Sensible heat = mv*ʎv + Mv*Cp*ΔT,
Here Mv = V = 909 kg/hr.
ʎv = (0.98*2,256.9kj/kg.) + (0.02*29,882kj/kg) = 2809.402 kj/kg
Cp = 0.98(4.2KJ/Kg.K) + 0.02(23kJ/Kg.K) = 4.576 KJ/Kg.K
HV = V (ʎv + *Cp*ΔT) = 909 kg [2809.402 kj/kg + 4.576KJ/Kg.K (176 - 25)K]
HV = 3,181,843.602 KJ
QC = HV = 3,181,843.602KJ
To determine the flow rate of cooling water;
QC = ṁH2O* ʎH2O
ṁH2O= Qc/ ʎH2O = 3,181,843.602 / 2256.9kj/kg
ṁH2O = 1409.829Kg of water is required to remove 3,181,843.602 KJ of heat
𝑄𝑐
Mass flow rate of water = 𝐶𝑃𝑤×∆𝑇
3,181,843.602
= 2256.9×68.5
= 20.58Kg/sec
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Take the system boundary including re-boiler and condenser to determine the re-boiler heat. Qbis
determined from complete system.
HD
QC
HF Distillation QR=?
XOF = 0.02
Unit
XWF = 0.98
F = 6,013 kg/hr HB
D = 0.02*6013 kg/ hr = 120.26 kg/hr.
F=B+D
B = F – D = 6,013 kg/hr – 120.26 kg/hr.
B = 5,892.74 kg/hr.
𝑘𝑔 𝑘𝑔
3,181,843.602 ℎ𝑟 5,892.74 ℎ𝑟
Xoil = 𝑘𝑔 = 0.02 X water = 𝑘𝑔 = 0.98
2256.9×68.5ℎ𝑟 6,013 ℎ𝑟
CP mix = CP oil * X oil + CP water * X water
CP mix = 23kj/Kg.K * 0.02 + 4.2 kj/Kg.K*0.98
CP mix = 4.576 kj/Kg.K
HF + QR = HD + HB +QC
QR = HD + HB + QC – HF, But HD =0 (due to the same temperature)
HF = mass of feed * CP mix *∆𝑇
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HF = 6013 kg/hr.*4.576 (93.5-25) k
HF = 1,884,810 kj/hr.
HD = Moil*CpD*∆T = 0
HB = mass of the sludge *CpB*∆T; But CpB = 3.671KJ/Kg.K
Then; HB = mass of the sludge*CpB*∆T
HB = 5892.74 Kg*3.671KJ/Kg.K *(90-25) K
HB = 1,406,096.1 kJ.
QR = 1,406,091.1KJ + 0KJ + 3,181,843KJ – 6,013KJ = 4581921.7KJ
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CHAPTER SIX
FINANCIAL EVALUATION AND SITE SELECTION
6.1 Market Study

6.1.1 Present Demand and Supply
Currently industrial demand for essential oil is met through import. There is also Essential Oils
Research Centre that has its head office and the main laboratory in Addis Ababa and an
agricultural research station, laboratory and a small-scale production unit at Wando Genet,
(about 267 km south of Addis Ababa). In addition to this, some firms are engaged in processing
and export of some specific types of essential oil. This includes Ariti Herbal Private Company,
Aromabyssinia Plc. and Cheleleka Edible Oil Factory. On the other hand various types of
essential oil are imported to Ethiopia which can be categorized under some major groups
according to their application. These are for: Perfumery, Pharmaceutical, Cosmetics, Toiletries,
and Confectionery industry. *However, detail data of essential oil for each sub section could not
be obtained. But it can be asserted that much of the demand is derived from the toiletries, and
confectionery industries given the relatively more production in these sectors. Nonetheless, the
supply of essential oil is derived from import mainly from India, Germany, Ireland, Italy, South
Africa, Great Britain and China (Customs Authority, various years). The total import demand for
the oil is presented in the following table. [34]
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Table 4: Projected Demands for Essential Oil
Year (E.C) Import (in ton)

1997/98 ton) 1997/98
1998/99 339.5
1999/2000 335.7
2000/2001 301.2
2001/2002 332.9
2002/2003 448.4
2003/2004 532.3
2004/2005 590
2005/2006 738.3
2006/2007 914.2
2007/2008 952.7
2008/2009 981
Source: Customs Authority, (various years)
The above table shows that annual demand for essential oil has increased by almost three fold
within the last ten years under consideration. Such huge increase is a result of expansion of the
industrial sector that makes use of essential oil.
6.1.2 Projected Demand

The future demand for essential oil very much depends on the growth of the industrial sector.
However, since all industrial production processes do not use essential oil, the growth of the
sector as a whole could not be used. But, since the growth of industrial outputs that make use of
essential oil (such as food industry, soap industry, etc.) is related with the growth of the urban
population growth rate, population based forecast can be made.
6.1.3 Pricing and Distribution

The CIF value of essential oil has been on average Birr 80 per kg in 1997/98 and has grown to
Birr 137 in 2006/07. The price charged by local distributers is further higher as duties; inland
transportation etc. will be added on the CIF value. In order to compete with imported products
and in view of the capacity of the envisaged plant, the whole sale price of the product has been
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estimated at Birr 66 per litter. The product will be distributed directly to the firms that use
essential oil in their production as the numbers of firms that demand the product are limited.
6.2 Plant Capacity

Given the projected demand presented earlier, and the planned technology, the envisaged plant is
set to produce 120 tons of essential oil annually that would be used mainly by the soap industry
and other toiletry products. This capacity is about 11.5% of the demand projected in 2009/10 and
it further decreases as time goes by.
6.2.1 Production Program

The program is scheduled based on the consideration that the envisaged plant will work 330 days
in a year in 2 shifts, where the remaining days will be holidays and for maintenance. During the
first year of operation the plant will operate at 40 percent capacity and then at to 60 percent in
the 2nd year and 80 percent in the 3rd year. The capacity will grow to 100 percent starting from
the 4th year. This consideration is developed based on the assumption that market and logistics
barriers would take place for the first three years of operation.
6.2.2 Plant location and Source of Raw Materials

Essential oil industry is an agro based industry. Accordingly, the envisaged orange peel waste as
the main raw material. This is available in large quantity in awash agro industry processing
(Arsi/merti wereda of oromia). And the location of plant is hospitable at the area of Arsi wereda,
which can minimize transportation cost and it has best climate condition for processing product.
6.3 Estimate the total capital requirement
It is essential that the chemical engineer be aware of the many different types of costs involved
in manufacturing processes. Capital must be allocated for direct plant expenses, such as those
for;
 Raw materials
 Labor
 Equipment
Total capital investment is the sum of working capital investment for the project, manufacturing
fixed capital investment and non-manufacturing fixed capital investment.
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6.3.1 Working capital

The working capital for an industrial plant consists of the total amount of money invested in:
1. Raw materials and supplies carried in stock,
2. Finished products in stock and semi-finished products in the process of being manufactured.
3. Accounts receivable,
4. Cash kept on hand for monthly payment of operating expenses, such as salaries, wages, and
raw-material purchases,
5. Taxes payable.
6.3.2 Capital investments

The capital needed to supply the necessary manufacturing and plant facilities is called the
fixedcapital investment, while that necessary for the operation of the plant is termed the working
capital. The sum of the fixed-capital investment and the working capital is known as the total
capital investment. The fixed-capital portion may be further subdivided into manufacturing
capital investment and nonmanufacturing capital investment.
6.3.3 Fixed capital investment

Manufacturing fixed-capital investment represents the capital necessary for the installed process
equipment with all auxiliaries that are needed for complete process operation. This is also called
direct cost. Like
 Purchased equipment
 Purchased equipment installation
 Expenses for piping
 Instrumentations and controls including insulation
 Service facilities
 Site preparations are typical examples of costs included in the manufacturing cost.
The nonmanufacturing fixed-capital investment (indirect cost) includes
 Engineering and Supervision
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 Construction expanses
 Contractor’s Fee
6.3.4 Machinery and Equipment

The machineries and equipment required for producing essential oils are detailed in table 4
below.
Table 5: Machinery and Equipment
Year (E.c) Imported (in ton)

2009/2010 1041
2010/2011 1071
2011/2012 1104
2012/2013 1138
2013/2014 1172
2014/2015 1207
2015/2016 1243
2016/2017 1380
2017/2018 1319
2018/2019 1358
Source: Customs Authority, (various years)
The forecasted result indicates that demand for essential oil will be higher than 1000 tons
beginning from 2009/10 and points out the importance of local production that can relieve to
some extent the import demand.
6.4 Estimation of Fixed Capital Investment

Fixed capital investment = direct cost + indirect cost
Construction period one year
Work in progress six days/week
Source of finance =30% of equity
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=70%of loan
Bank interest =5%
The finance analysis of our plant project is based on the current raw material cost tabulated and
the diagrammatic relationship of different cost shown below;
6.4.1 Estimation of direct and indirect cost

Table 6: Estimation of cost
Direct cost(DI) Range% Selected percentage Estimated cost ( $)

Purchased equipment 174,000
cost(PEC)
Purchased equipment 25-55PEC 30 52,200
installation, insulation
and painting
Instrumentation and 6-30PEC 18 31,320
control
Piping (installed) 10-80PEC 40 69,600
Electrical (Installed) 10-40PEC 25 43,500
Building (including 10-70PEC 13 22,620
services)
Service facility and 40-100PEC 40 69,600
yard improvement
Land 4-8PEC 10 10,440
Total direct cost 299,280
Indirect cost(IDC)
Engineering and 5-30DC 17.5 52,374
supervision
Construction expenses 6-30DC 15 44,892
& contractor fee
Contingency 5-15DC 10 29,928
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Total indirect cost 127,194

Fixed capital investment =direct cost + indirect cost
FCI = DC +IDC
FCI = $299,280 + $127,196
Fixed capital investment = $426,474
Working Capital investment (WCI) = 15% of TCI
Total Capital Investment (TCI) = FCI + WC
TCI =FCI+0.15TCI
TCI - 0.15TCI = FCI
TCI = FCI/0.85
= $426,474/0.85
= $501,734
From the above two equations:
WC = $75,260.1
6.4.2 Estimation of Total Production Cost (TPC)

Total production cost = Manufacturing cost + General expenses
Manufacturing cost = direct production cost + indirect production cost
Direct production cost (DPC): is the summation of all the following costs
 Raw material cost = 10%TPC

 Operating labor = 15%TPC
 Direct supervisory and clerical labor = 10%OL = 0.015TPC
 Utility = 15%TPC
 Maintenance and repairs = 6%FCI = $426,474*0.06 = $25,588.44
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 Operating supplies=15%maintenance and repair=0.15*$25,588.44 = $ 3,838.266

 Laboratory charges = 15% of operating labor = 15% (0.15%TPC) = 0.0225TPC
 Patent and royalties = 3%TPC
DPC= 0.1TPC+0.15TPC+ (0.1*0.15) TPC+0.15TPC+$93146.76+$25,588.44 + $3,838.266 +
(0.15*0.15) TPC+0.03TPC
DPC = 0.4675TPC+$29,426.7………………….…………………… ……………….…… (1)
Fixed Operating Costs/Fixed charges:
Fixed operating costs are generally incurred in full whether or not the plant is producing at full
capacity. These costs include labor and various overhead items.
Table 7: Fixed Operating Costs
SN Item Factor Cost(US ,$)

1 Depreciation 0.1FCI 0.1FCI 42,647.4
2 Local taxes 0.02FCI 0.02FCI 8,529.48
3 Insurance 0.005FCI 0.005FCI 2,132.37
4 Rent 0.006(Land and Building) 62.64
Total fixed charge = $53,371.9
Plant overhead cost =10%TPC……………………………………………..………………. (2)
Manufacturing cost (MC) = Direct product cost + Fixed charges + Plant overhead cost
MC =0.4675TPC+$29,426.7 + $53,371.9 + 0.1TPC
MC =0.5675TPC +$82,798.6…………………………………………………………...…. (3)
General expense cost:
 Administrative cost = 3%TPC

 Distribution and selling = 6%TPC
 Research and development = 5%TPC
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Then, General expenses = 0.03TPC+0.06TPC+0.05TPC = 0.14TPC…………………….. (4)
Total product cost (TPC) = MC + general expenses.
TPC= 0.5675TPC + $82,798.6 + 0.14TPC = 0.7075TPC+$82,798.6
TPC (1- 0.7075) = $82,798.6
0.2925TPC = $82,798.6
TPC= $283,072.13
Total product cost (TPC) = $283,072.13
From equation (1)
Direct production cost (DPC) = 0.4675TPC + $29,426.7
= $161,762.9
From equation (2), Plant overhead cost =10%TPC = 0.1*283,072.13= $28,307.213
From equation (4), General expenses = 0.14TPC = 0.14*283,072.13 = $39,630.1
Gross earnings cost
Basis: -working hour = 24hr/day
Working day = 330day /yr.
Product per year is = 120,000kg/yr.
Unit sell price = $3/L.
To know the amount production of essential oil in litter per year:
1,2000,000 𝑘𝑔/𝑦𝑟
V = (𝑚𝑎𝑠𝑠𝑜𝑖𝑙)/(𝑑𝑒𝑛𝑠𝑖𝑡𝑦𝑜𝑖𝑙) = = 143.027 m3/yr. = 143,020 L/yr.
839𝑘𝑔/𝑚3
Total selling price per year = unit selling price*total volume per year.
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= $3/L * 143,020 L/yr.
=$ 429,060/yr.
Gross income= Total selling price per year – Total Product Cost
= $ 429,060/yr. - $283,072.13/yr.
=$ 145,987.87/yr.
Depreciation = $ 42,647.4
Plant life (n) = 10 year, MAR= 15% Let the Tax rate be 34% (common)
Net Profit (NP):
Net Profit (NP) = Gross income - Taxes = Gross income× (1- Tax rate)
NP= $145,987.87× (1- 0.34) = $ 96,351.9942/yr.
Rate of Return on Investment (ROI):
Rate of return= (Net profit/ Total Capital Investment) ×100
= ($96351.9942/ $501,734) ×100% = 19%
This shows that the project is feasible because ROI is greater than minimum acceptable rate of
return (Mar). I.e. 19% >15%
Payback Period (PBP):
Project life is assumed 10 years and we use straight line method
Vs = salvage value of property at end of service life assume that = 0
𝑻𝒐𝒕𝒂𝒍𝒇𝒊𝒙𝒆𝒅𝒄𝒂𝒑𝒊𝒕𝒂𝒍𝒊𝒏𝒗𝒆𝒔𝒕𝒎𝒆𝒏𝒕−𝒔𝒂𝒗𝒊𝒏𝒈𝒗𝒂𝒍𝒖𝒆 $𝟒𝟐𝟔.𝟒𝟕𝟒−𝟎
PBP = =($𝟗𝟔,𝟑𝟓𝟏+$𝟒𝟕,𝟔𝟒𝟕.𝟒) = 3.08yr ≈ 3yr
𝑵𝑷×𝑫𝒆𝒑𝒓𝒊𝒄𝒊𝒕𝒊𝒐
Payback Period Reference (PBPREFF):-
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𝑻𝒐𝒕𝒂𝒍𝒇𝒊𝒙𝒆𝒅𝒄𝒂𝒑𝒊𝒕𝒂𝒍𝒊𝒏𝒗𝒆𝒔𝒕𝒎𝒆𝒏𝒕 $𝟒𝟐𝟔,𝟒𝟕𝟒
Ratio = = 0.8500≈0.85%
𝑻𝒐𝒕𝒂𝒍𝒄𝒂𝒑𝒊𝒕𝒂𝒍𝒊𝒏𝒗𝒆𝒔𝒕𝒎𝒆𝒏𝒕 $𝟓𝟎𝟏,𝟕𝟑𝟒
0.85 0.85
PBPref = = 0.15+0.85/10 =0.85/0.235 = 3.62, this shows that the project is feasible
𝑀𝑎𝑟+0.85/𝑛
because PBP is less than PBPref .That is 3 years 3.62 years ≈ 4 years.
Net present worth (NPW) NPW = ∑10

1 (1 + 𝑖)
−𝑛
(NPj + dj +recj) – TCI
Recovery value = (salvage value + working capital)(1 + 𝑖)−10 = (0+$75,260.1) (1.15)−10
= $ 18,603.1457/yr.
Annual cash flow (R) =NP +Dj = $96,351.9942+ $42,647.4
= $139,026.4
𝑅(1+𝑖)𝑁 −1
NPW = + recovery value – TCI
𝑖(1+𝑖)𝑁
$139,026.4(1+.15)10
NPW = + $ 18,603.1457- $501,734=$14,686,046.7
0.15(1+0.15)10
Where i = MAR= 15%
NPW = $ 14,686,046.7 since the value is positive the project is feasible.
6.5 Economic and Social Benefits and Justification

The envisaged project possesses wide range of benefits that help promote the socio - economic
goals and objectives stated in the strategic plan of the Oromia National Regional State. It also
boosts inter sectarian linkage between the agricultural and industrial sectors. At the same
time,therefore, it helps diversify the economic activity of the region. The other major benefits are
listed as follows:
6.5.1 Profit Generation

The project is found to be financially viable and earns on average a profit of dollar 96,351.9942
thousand per year and dollar 9h63, 519.942 within the project life. Such result induces the
project promoters to reinvest the profit which, therefore, increases the investment magnitude in
the region.
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6.5.2 Tax Revenue
In the project life under consideration, the region will collect about $49,635.8758 from corporate
tax payment alone (i.e. excluding income tax, sales tax and VAT). Such result creates additional
fund for the regional government that will be used in expanding social and other basic services in
the region.
6.5.3 Import Substitution and Foreign Exchange Saving

Based on the projected figure we learn that in the project life an estimated amount of USD dollar
963,519.942 will be saved as a result of the proposed project. This will create room for the saved
hard currency to be allocated to other vital and strategic sectors.
6.5.4 Employment and Income Generation

The proposed project is expected to create employment opportunity to several citizens of the
region. That is, it will provide permanent employment as well as support staff.
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CHAPTER SEVEN
CONCLUSION AND RECOMMENDATIONS
7.1 Conclusion
This study showed that different factors had different effects on the yield of orange peel
essential oil product. The effects of treatment on the product also differ with in the treatment.
The effect of temperature, heating time and particle sizes were significant on the yield of
essential oil. It rapidly increases the yield when the temperature rise from 30℃ up to 93.5℃ but
when the temperature beyond 93.5℃ the yield of the essential oil became decrease. When the
extraction time rise from 36 min. up to 1 hr. the yield also increase rapidly but further increase
the time would gradually decrease the yield. The yield obtained at 1:10 material ratio was higher
than the yield obtained at 1:5 material ratios. As we have seen from the analysis the highest
yield, 5.33%, obtained at the treatment of the temperature 93.5 ℃ , residence time at the
treatment of 1 hour and the ratio of orange peel powder with solvent (distilled water) at 1:10
ratio. From the laboratory investigation, we have considered that the loading amount of raw
material affect the extraction temperature, energy consumption, and time of heating.
7.2 Recommendation
 In this project work, the effects of pressure and viscosity were not studied due to the lack
of appropriate equipment. Therefore, further study is need on these effects.
 A further study can also be conducted in focusing on the quality of the orange peel
essential oil obtained at each operating conditions. This will provide alternative to
manufacturers on the minimum conditions required to get a specific quality of essential
oil with minimum capital.
 The project groups also can’t did on the characterization of some of the behaviors of the
essentialoil. Such as: characterization of viscosity, peroxide value, refractive index, and
some others should be conducted to investigate and come up with the qualified product.
 The extraction process has much amount of residue of sludge of orange peel powder,
which is very vital feed stock for fertilization and biogas processing. Therefore the
consideration should be taken in account for the environmental protection.
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REFERENCES
1. Agricultural Marketing Resource Center, Purdue University Center for New Crops & Plant
Products, USDA.
2. Extraction and Characterization of Essential Oil from Rosemary Leaves, Solomon Haile
Mariam Addis Ababa, Ethiopia October,2016
3. Essential oil/ http://www.wikipedia.org
4. Guenther, E. The Essential Oils; D. Van Nostrand Company Inc.: New York, NY, USA,
1948; p. 427.
5. Association Française de Normalisation (AFNOR). Huiles Essentielle, Tome 2, Monographies

Relatives Aux Huiles Essentielle, 6th ed.; AFNOR, Association Française de Normalisation:
Paris, France, 2000.
6. Carette Delacour, A.S. La Lavande et son Huile Essentielle. Ph.D. Thesis, University Lille 2,
Lille, France, 2000
7. http://www.buzzle.com/editorials/7-3-2006-101131.asp
8. http://www.cherylinskintherapy.co.uk/chemical-constituents-essential-oils-may.pdf
9. M. Josip, O. Politeo and I. Jerković Contribution to the Analysis of the Essential Oil of
Helichrysum italicum (Roth) G. Don. – Determination of Ester Bonded Acids and Phenols,
Department of Organic Chemistry, Faculty of Chemistry and Technology, Department of
Biochemistry.
10. http://www.healingdeva.com/selena2.htm
11. http://lmkinteriorsltd.wordpress.com/2010/04/18/what-is-that-wonderful-scent/
12. SADC trade, trade information brief, essential oils, Australian government.
13. Citrus: World Markets and Trade for January 2014, United States Department of Agriculture
2014. 14. J. A. Siles Lopez, Q. Li and I. P. Thompson, Critical Reviews in Biotechnology, 2010,
30, 63-69.
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15. R. P. Bates, J. R. Morris and P. G. Crandall, in Principles and practices of small and medium
scale fruit juice processing, Food & Agriculture Organization, 2001, vol. 2014, Ch. 11.
16. M.-C. Ralet, E. Bonnin and J.-F. Thibault, in Polysaccharides and Polyamides in the Food
Industry: Properties, Production, and Patents, eds. A. Steinbüchel and S. Ki Rhee, Wiley-VCH,
2005, vol. 1.
17. R. J. Braddock, Handbook of Citrus By-Products and Processing Technology,

WileyInterscience, 1999. 18. G. Dugo and A. D. Giacomo, eds., Citrus- The genus Citrus, Taylor
& Francis, London, 2002.
19. F. R. Marin, C. Soler-Rivas, O. Benavente-Garcia, J. Castillo and J. A. PerezAlvarez, Food

chemistry, 2007, 100, 736-741.
20. M. Pourbafrani, G. Forgacs, I. S. Horvath, C. Niklasson and M. Taherzadeh, Bioresource

Technology, 2010, 101, 4246-4250.
21. V. A. Bampidis and P. H. Robinson, Animal Feed Science and Technology, 2006, 128, 175-
217.
22. Lucie Anne Pfaltzgraff (2014), the study & development of an integrated & additive-free
waste orange peel biorefinery.
23. Pandey D. and Virendra Rao P.S, Extraction of essential oil from Eucalyptus leaves (Btech
project), NIT Rourkela.
24. Kumar K.satish, 2010 extraction of essential oil using steam distillation: National Institute of
Technology, Rourkela.
25. Li Y. et al., (2014). Essential Oils: From Conventional to Green Extraction: Essential Oils as
Reagents in Green Chemistry, SpringerBriefs in Green Chemistry for Sustainability, DOI
10.1007/978-3-319-08449-7_2
26. H. Mukhtar, M. Khalid Shabbiri, R. Nadeemi, A. Farooq, and W. Mumtazi 1Department of

Chemistry, physico chemical analysis and determination of various chemical constituents of
essential oil in Rosa cent folia, University of Agriculture, Faisalabad, Pakistan 2Institute of
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Industrial Biotechnology, Govt. College University, Lahore 54000 Pakistan, 3Department of

Chemistry, University of Gujrat, Pakistan.
27. H. Singh, M. Hasan and L. J. Kang, Supercritical carbon dioxide extraction of Sarawak black
pepper oil, Department of Chemical Engineering, University of Malaya.
28. http://www.bellevuemassagetherapy.com/methods-of-extracting-essential-oils.html
29. Kumar K.satish, 2010 extraction of essential oil using steam distillation: National Institute of
Technology, Rourkela.
30. Kabuba Tshilenge john (2009) steam extraction of essential oils: investigation of process
parameters. 31. Extraction of essential oil using steam distillation, Department of Chemical
Engineering National Institute of Technology, Rourkela, 2010.
32. Solomon Hailemariam, Extraction and Characterization of Essential Oil from Rosemary,
Addis Ababa, Ethiopia October, 2016.
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APPENDIX
Laboratory equipment and sample photos
Collected orange peel Grinded the dried orange peels
Sieve analysis of orange peel Mixing orange peel powder and distilled water
Extraction of orange peel using steam distillationEssential oil
Iodine test of essential oil Titration of test solution
56 | P a g e

Extraction of Essential Oil from Orange Peel

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ADIGRAT UNIVERSITY

COLLEGE OF ENGINEERING DEPARTMENT OF

THESIS TITLE: EXTRACTION OF ESSENTIAL OIL FROM ORANGE PEEL USING

A Thesis Submitted to departments of Chemical Engineering in Partial Fulfilment of the Degree

1. Haftom Weldegebriel 0724/06

Instructor Tsegaluel k. (MSc)

Adigrat, Tigray, Ethiopia

………………… …………………. …………………

………………… …………………… …………………

2.2.2 Pharmaceutics .............................................................................................................................. 7

3.1 Materials ........................................................................................................................................... 20

5.3.2.1 Energy balance on drier .............................................................................................................. 35

List of acronym and abbreviations

AFNOR………………………………………………. AgenceFrançaise de Normalisation

1.2 Problem statement

1.4 Significance of study

2.1.1 Chemical constituents of Essential oils

2.1.8 Monoterpene [C10 H16]:

2.2 Advantages of essential oil

2.3 Expectorants and diuretics

2.3.1 Spasmolytic and sedative

2.3.3 Cosmetics and Perfumes

2.4 Major importing countries

Figure 1: Top five importers share of world essential oils exports.

2.5 Major exporting countries

Figure 2: Top 5 exporter’s shares of world essential oils exports

2.6 Availability of citrus peel waste around the world

Brazil 10,935,000 5,467,500

2.7 Orange peel waste composition and value

2.7.1 D-limonene and orange oil:

Figure 4: D – Limonene structure.

2.8 Methods of extraction

2.8.3 Cold Pressing

2.8.5 Super Critical CO2 Extraction

2.8.6 Steam Distillation Extraction

2.8.6.1 Extraction of Essential Oils Using Steam distillation Method

2.8.9 Advantages of using Steam Distillation

2.8.10 Methods for Distillation

B. Water and steam distillation

C. Direct steam distillation

B. Water and Steam Distillation

 Higher oil yield.

 If refluxing is controlled, then the loss of polar compounds is minimized.

C. Direct Steam Distillation

 Amount of steam can be readily controlled.

2.9 Parameters Affecting Yield and Quality of Essential Oils

2.9.2 Improper Design of Equipment

2.9.3 Material of Fabrication of Equipment

2.9.4 Condition of Raw Material

2.9.5 Time for Distillation

2.9.6 Loading of Raw Material and Steam Distribution

2.9.7 Operating Parameters

3.3 Raw Material preparation

Figure 5: process flow chart for preparation of orange peel

IV. Weighing the dried peel by using electronic balance

Figure 7: conformation test for limonene

3.5 Characterization of the extracted orange peel essential oil

3.5.1 Determination of physical properties

Moisture Content Determination

Size reduction and Sieve analysis of the peel

Percentage of orange peel essential oil extracted

PH value of essential oil

Q = mCp ΔT = 46.25 kg/hr3.9kj/Kg.K (60 -25) ◦k = 6,313.125kj/hr.

HB = mass of the sludge CpB∆T; But CpB = 3.671KJ/Kg.K

Then; HB = mass of the sludgeCpB∆T