[Mahajan, 4(6): June 2017] ISSN 2348 – 8034

DOI- 10.5281/zenodo.804823 Impact Factor- 4.022

GLOBAL JOURNAL OF ENGINEERING SCIENCE AND RESEARCHES
EXTRACTION OF D- LIMONENE FROM ORANGE PEELS
Prasad R. Mahajan*1, Pratika D. Wankhede2 & Omkumar S. Gulhane3
*1,2&3
Student, Chemical Department, Jawaharlal Darda Institute OfEngg and Tech, Yavatmal

ABSTRACT
The orange peel which is considered as a waste can be used for the extraction of limonene (D-Limonene ) which has
many applications ranging from food flavouring agent to cosmetics. Limonene can be extracted by various
conventional methods like steam distillation cold press, solvent extraction, novel methods like super critical CO2
extraction, it means varied typical ways like steam distillation cold press, solvent extraction, novel ways like super
essential greenhouse emission extraction. The conventional method though simple are robust and the yield
percentage is less whereas the novel methods are not cost effective as well as easy the yield share is a smaller
amount whereas the novel ways aren't price effective.This experiment demonstrates the extraction of plant oils. The
peel of oranges is boiled in water and the oil produced {limonene} distilled in steam at a temperature just below
100 ̊C, well below its normal boiling point. This experiment demonstrates the extraction of plant oils. The depart
oranges is cooked in water and therefore the oil created distilled in steam at a temperature slightly below a
hundred ̊C, well below its traditional boiling purpose. The incompatible oil will then be separated. Direct extraction
by heating would lead to decomposition whereas steam distillation doesn't destroy the attractive force.Limonene is
an unsaturated hydrocarbon which can be tested for using bromine water or potassium magnate which may be tested
for victimization element water or potassium business leader.

Keywords: Orange peels, D-limonene, steam distillation.

I. INTRODUCTION

Low molecular weight water immiscible compound can be separated by natural gas product by steam distillation. In
this case steam distillation is use to isolate essential oil limonene from orange peels. Limonene is concentrated in the
peel of oranges. The orange peels have two distinct layers, the skin and the pith .Limonene is not distributed evenly
between these two layers. Experimentation has shown that only minimum quantities of limonene can be extracted
from white pith. The outer skin accounts for the 2/3 of the mass of the peel. The best yield of limonene can be
obtained from outer skin.[2]

D-Limonene is obtained as a by-product of the citrus juice industry. It is the major component of the oil extracted
from the rinds of citrus fruits. There are two main grades of d-Limonene which are called food grade and technical
grade. Once citrus fruits square measure juiced, the oil is extracted out of the rind. The juice is separated from the oil
and the oil is distilled to recover certain flavour and fragrance compounds. This is called food grade d-limonene
which is 96% to 97% pure and has a mild orange aroma. After the juicing process, the peels are taken to a steam
extractor. More oil is extracted from the peel. When the steam is condensed, a layer of oil floats on the surface of the
condensed water. This is called technical grade d-Limonene which is 95% pure and has a strong orange aroma. Both
products are called orange turpenes.

Pure D-Limonene is lighter than water, and is usually colourless industrial products. D-Limonene can be used as a
straight solvent or as a water dilutable product.

In this process steam distillation was used to extract oil from orange peels research has confirm- centuries of
practical use of limonene and we know that fragrant pharmacy contains compound with an extremely broad range of
bio chemical effect with extremely broad range of biochemical effect. The recovery of essential oil from orange
peels as a starting material is very important. Analysis of essential oil was done using gas chromatography-mass

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(C)Global Journal Of Engineering Science And Researches
[Mahajan, 4(6): June 2017] ISSN 2348 – 8034
DOI- 10.5281/zenodo.804823 Impact Factor- 4.022
spectroscopy apparatus, which gives qualitative volume of oil obtained, was changing with respect to the time and
quantity of orange peels.[1]

A. Motivation And Objectives

Idea behind this is increasing demand of citrus fruits juice by people increases the production of juice in the citrus
fruit juice industries, at the same time, waste peels from industries are used to extract the D-limonene for the several
applications.

 Fruit peels like orange and lemon are discarded after consumption.
 Combustable, thus can be used as a potential renewable biofuel.
 Important medicinal properties: sedative, anti-stress, anti-carcinogenic, relieves heartburn and
gastrointestinal reflux.
 Useful in chemical synthesis: a precursor to carvone.
 Solvent for cleaning product
 Used in cosmetic products, food flavourings and as a fragrance in the perfume industry.

B. Methods Of Extraction
 Cold pressing.
 Solvent extraction.
 Steam distillation.

By using Steam Distillation Extraction we conduct this process

Steam distillation could be a special kind of distillation or a separation method for temperature sensitive materials
like oils, resins, hydrocarbons, etc. that square measure insoluble in water and will decompose at their
boiling purpose.The elemental nature of steam distillation is that it permits a compound or mixture of compounds to
be distilled at a temperature well below that of the boiling point(s) of the individual constitute(s).
Essential fifteen oils contain substance with boiling stress to 200̊C or higher temperature. within the presence of
steam or boiling water, however, these substance square measure gasified at a temperature 10̊C terribly near gas
pressure.

Variety of things determined the ultimate quality of a steam distilled volatile oil. excluding the material, most vital
square measure time, temperature and pressure, and quality of the distillation instrumentality. Essential oils are very
complex products. Each is made up of many, sometimes hundreds, of distinct molecules which come together to
from the oil’s aroma and therapeutic properties. Some of these molecules are fairly delicate structure which can be
altered or destroyed by adverse environmental conditions. So, much like a fine is more flavourful when made with
patience, most oils benefit from a long, slow ‘cooking’ process.

It is possible that longer distillation times may give more complete oil. It is also possible however, that longer
distillation time may lead to the accumulation of more art facts than normal. This may have a curious effect of
appearing to improved the odor, as sometimes as sometimes when materials that have a large number of components
are sniffed, the perception is often of slightly increased sophistication, added fullness and character, and possibly,
and extra pleasantness.[3]

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(C)Global Journal Of Engineering Science And Researches
[Mahajan, 4(6): June 2017] ISSN 2348 – 8034
DOI- 10.5281/zenodo.804823 Impact Factor- 4.022
C. Chemical structure of limonene

Fig- 1 Molecular Structure Of Limonene

D. Properties Of Limonene
 Molecular formula : C10H16
 IUPAC NAME: 4-ISOPROPENE-1-METHYLE-CYCLOHEXANE
 Molar mass : 136.24 g/mole
 Density : 841kg/m3
 Melting point : 74.35°C
 Boiling point : 176°C
 Specific gravity : 0.838 at 680F
 Physical State : Colourless or pale yellow
 Limonene is an alkene, meaning its functional group is C=C, its suffix is-ene and its formulaic CnH2The
Molecular formula is C10H16.
 Its full name is 1-methyl-4-prop-1-en-2-yl-cyclo hexane.
 Limonene melts at -95.2 °C and it boils at 176 °C, therefore Limonene is liquid at room temperature.
 It is lighter than water and insoluble in water, unless a surfactant is added.
 D-limonene is considered a combustible liquid. Limonene is a cyclic terrene[5].

E. Applications Of D-Limonene

1. Cleaner for concrete

D-limonene will usually clean graffiti (including effectively replacing xylene in graffiti removers) off concrete
because of its ability to remove paint. Strong enamels and epoxy paints will not usually be removed.

2. Release Agent
D-limonene can be used at various levels for a release agent that is sprayed on the beds of asphalt trucks before
picking up their loads to facilitate easy unloading. Since d-limonene will not readily freeze (-142º F freezing point),
the product lends itself to underground storage through cold winters.

3. Straight Solvent Replacement

D-limonene is a great solvent to directly replace the toxic solvent components in existing solvent blends. One
example is the 1:1 substitution of d-limonene in the place of xylene or 111 tri-chlor in blends with other inexpensive
solvents to make up the balance (mineral spirits, isopropyl alcohol).

4. Digestive problems
D-limonene has amazing curative properties for healing various stomach problems, for example; indigestion and
bloating. Add a mixture of equal parts essential oils for example lavender or rose wood to orange oil and rub
carefully on the skin over the stomach area.

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(C)Global Journal Of Engineering Science And Researches
[Mahajan, 4(6): June 2017] ISSN 2348 – 8034
DOI- 10.5281/zenodo.804823 Impact Factor- 4.022
5. Hand cleaner
D-limonene is very effective removing almost any soil including: ink, paint, grease and tar .solvent based hand
cleaners usually contain approx. 30% solvent. At 10%, D-limonene will out-perform most other solvent hand
cleaners.

6. Penetrating oil
D-limonene can be used as the spray on product to loosen bolts and nuts, much like WD-40TM. D-limonene has the
ability to wick into tight joints and dissolve hardened greases and oils to assist in the removal of bound nuts and
bolts.

7. Adhesive removal
D-limonene is very good solvent for removal of adhesives from various substrates. Most contact adhesives will
dissolve very quickly; however, D-limonene has almost no effect on epoxies which have already cured [4]

II. MATERIAL AND METHOD

A. Apparatus

 Two necked round bottom flask

 Burette stand
 Condenser
 Measuring cylinder of 2.5ml
 Heater

B. Raw Material
 Orange peels =15 grams
 Distilled water =50 ml

C. Procedure

1. Grate the outer orange colored rindof 2 oranges andboost100 ml distilled. Water within the 250 cc
spherical round-bottom flask.
2. Found out the distillation equipment as shown within the equipment section.
3. Heat the flak in order that distillation issue at a gentle rate more or less onedrop per second of liquid.
4. Collect more or less fifty cc of liquid within the activity cylinder. The oilLayer are on the surface.
5. Employing a dropping measuring system fastidiously take away the oil layer into a tube.

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(C)Global Journal Of Engineering Science And Researches
[Mahajan, 4(6): June 2017] ISSN 2348 – 8034
DOI- 10.5281/zenodo.804823 Impact Factor- 4.022

Fig-2: Layer of D-limonene

obtained

III. METHOD OF ANALYSIS

The qualitative and quantities analysis was done to identify the constituents in the oil and the percentage of
component present in the oil respectively.

A. IODINE TEST
This test is performed to check the presence of unsaturated bonds in a molecule. Few drops of the orange oil were
taken in a test tube. A few crystal of iodine were added and shaken well.[7]

B. pH TEST
The pH of any liquid sample is generally measured using pH meter. A few ml of the orange oil was taken for pH
analysis. [7]

Fig-3: Iodine test

IV. RESULT AND DISCUSSION

A. Extraction of D-limonene
The orange peels were cut into small size and were pre heated below 100 degree Celsius at constant temperature at
30, 60,90 and 120 minutes respectively for 4 readings. It has been observed that yield of the D-limonene increases
with increasing time. Steam distillation is the promising method for the extraction of D-limonene. The increase in
orange oil d-limonene yield (%) by steam distillation is more due to reasons that the orange peels were pre heated
which softened the cell walls of the orange peels which are made up of cellulose, hemicelluloses and pectin and the
orange peels were pre heated that softened the cell walls of the orange peels that square
measure created of polysaccharide, hemicelluloses and cellulose. once the pre heated peels were additional subjected

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(C)Global Journal Of Engineering Science And Researches
[Mahajan, 4(6): June 2017] ISSN 2348 – 8034
DOI- 10.5281/zenodo.804823 Impact Factor- 4.022
to traditional steam distillation procedure, it additional softened and open the cell walls of the orange peels to
liberate all the parts gift in it within the variety of orange oil.

1. Iodine test
Iodine take a look at was the characterization take a look at for the presence of any unsaturated compound in an
exceedingly take a look at sample. On addition of iodine, the colourless oranges oil sample extracted by steam
distillation become brown colour. The presence of d-limonene and alternative aromatic compounds within
the sample was confirmed. The brown colour is thanks to the reaction of iodine with d-limonene
and alternative unsaturated compounds like essential oil, Miocene, α-pinene,β-pinene.[7]

2. pH Test
The oil samples after distillation of the pre-heated peels were collected and subjected for pH analysis using a pH
meter. The pH value of sample found to be 4.98, which is very much acidic in nature.[7]

Formulae for finding yield%after extraction process:

 %Yield=(final mass of orange oil/ initial mass of orange peel)*100 (1)
 % yield = (0.4/50)*100=0.8(2)
 % yield = (0.8/50)*100=1.6 (3)
 % yield = (1.1/50)*100=2.2(4)
 % yield = (1.5/50)*100=3(5)

B. Observation table

Table no 1: Volume of oil collected (ml) per 50 gram of orange peels

Sr. no. Weight of orange peel Volume of oil collected Time (min)
(gm) (ml)

1 50 0.4 30
2 50 0.8 60
3 50 1.1 90
4 50 1.5 120

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[Mahajan, 4(6): June 2017] ISSN 2348 – 8034
DOI- 10.5281/zenodo.804823 Impact Factor- 4.022
C. Graph

Time(Min)

1.6
1.4
1.2
1
0.8 Volume(ml)
0.6
0.4
0.2
0
0 50 100 150

Fig-4 Graph- Time Vs Volume

V. CONCLUSION

 Finally we conclude the following deductions from the above experimental and analysis part.
 Steam distillation method was found to be one of the promising technique for extraction of orange peel oil
D-limonene.
 Volume of orange peel oil D-limonene increase with increase in time by keeping temperature as constant.
 As the time increases percentage recovery of orange oil also increases.

VI. ACKNOWLEDGEMENT

The authors are thankful to Jawaharlal Dada Institute of Engineering and Technology, Yavatmal, for their valuable
support and providing facilities to carry out this research work.

REFERENCES
1. www.biochemcorp.com/dilimonene2.htm
2. http://en.wikipedia.org/wiki/steam distillation
3. A sahoo,Satish Kumar (2010) extraction of essential oil and fulfilment for degree of bachelor of technology
national institute ,Rourkela.
4. D-limonene- uses. Pdf
5. http://en.wikipedia.org/wiki/limonene
6. www.einsten.net.pdf.5150253503
7. http://www.researchgate.net/publication/27494799.extractionof-orange-oil-by-improved-steam-distillation-
and-its-characterization-studies

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