DATE:
EXPERIMENT# 09
OBJECT:
Extraction of volatile oil from Eugenia caryophyllus by distillation
REQUIREMENTS:
• Round bottom flask
• Receiving flask
• Burner
• Measuring cylinder
• Funnel
• Thermometer
• Weighing balance
• Condenser tube
THEORY:
DISTILLATION:
Distillation is the process of separating the components of a liquid mixture through selective evaporation and
condensation.
1. WATER DISTILLATION: In this method, the material is completely immersed in water, which is
boiled by applying heat and then collecting the condensed vapor. The main characteristic of this process
is that there is direct contact between boiling water and plant material, it permits processing of finely
powdered material or plant parts that is dry substances, by contact with live steam, would otherwise form
lumps through which the steam cannot penetrate.
Example: dirty water can be distilled to produce pure water
Advantages:
1. This distillation process include its ability to separate water from virtually all dissolved and
suspended contaminants as well as the effect of high temperature to kill viruses, bacteria and
spores.
Disadvantage:
1. It does consume a huge amount of energy.
2. In some types of distillation it gives a slow output.
3. Higher operating costs.
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2. STEAM DISTILLATION: Steam distillation is a technique commonly used to extract volatile oils or
essential oils from plants. It is especially useful for extracting essential oils from plant materials that are
sensitive to – high temperatures because there is no-direct heat is applied to the sample, which can
potentially degrade the volatile compounds
Example: to extract eucalyptus oil from eucalyptus, citrus oils from lemon or orange peel, and to
extract oils used in perfumes from various plant materials
Advantages:
1. The method generates organic solvent-free products,
2. There is no need for subsequent separation steps,
3. Possesses large capacity for processing at the industrial scale
4. The equipment is inexpensive
5. Requires less fuel for the steam boiler for extraction of oils.
Disadvantages:
1. The liquid mixture with comparable boiling points cannot be separated since both evaporate at
the same temperature and are converted to vapor. So, we cannot collect them separately.
2. It needs high equipment and operating cost.
3. Special training is required to operate such an instrument.
3. .WATER & STEAM DISTILLATION In vacuum distillation, the distillation process is carried out
under reduced pressure (vacuum), which lowers the boiling point of the compounds involved. This
method is especially useful for substances that are heat-sensitive or have very high boiling points, which
would decompose or degrade at normal atmospheric pressure.The vacuum can be created using vacuum
pumps or aspirators, and the entire setup (boiling flask, condenser, and receiver) must be air-tight. This
method helps in controlling the thermal decomposition of compounds, as the distillation takes place at
much lower temperatures than usual.
Example: In this method, substances like glycerin, pharmaceutical solvents, fatty acids, and high-boiling
oil(e.g., vitamin E, essential oil concentrates) are distilled under vacuum on an industrial scale.
.
Advantages:
1. The reduced boiling point under vacuum prevents thermal decomposition of
temperature-sensitive compounds..
Disadvantages:
1. Compounds with very close boiling points under vacuum may still not be efficiently separated.
VOLATILE OIL:
Volatile oils are odorous volatile principles of plant and animal source, evaporate when exposed to air at
ordinary temperature, and hence known as essential or ethereal oils. Terpenes & Terpenoid are found in all
volatile oil. The term Terpene represents hydrocarbons (CSH8)n which is responsible for aroma. While
terpenoids include hydrocarbons, as well as their oxygenated derivatives. Terpenoids are chemically made of
isoprene units (C5H8). 2 Isoprene units (C5H8) combines to form monoterpenes (C10H16), 3 Isoprene units
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(C5H8) combines to form Sesquiterpenes, (C15H24) & 4 Isoprene units (C5H8) combines to form diterpenes
(C20H32). The density of volatile oil is as compared to water is low whereas the density of Clove oil is high as
compared to water.
OLEFINIE BOND:
Type of bond present in the unsaturated hydrocarbon. These are unsaturated bonds or pi bonds (double bonds)
present in the hydrocarbon. It is represented as >C=C<. The presence of an olefinic bond in the alkenes makes
the compound insusceptible for movement.
Musk: Musk is the only animal which is the source of volatile oil except plants. After photosynthesis when the
primary metabolites are formed, the biosynthesis occur in which the primary metabolites forms secondary
metabolites. Following are the 2 pathways by which biosynthesis of terpenes and other isoprenoids takes place:
ACETATE-MEVALONATE PATHWAY:
This pathway is concerned with biosynthesis of terpenes and also some other isoprenoids like sterols, through
conversion of the acetyl-CoA to mevalonic acid.
SHIKIMIC ACID PHENYLPROPANOID PATHWAY:
The shikimic acid phenylpropanoid pathway is biochemical pathway that occurs in, plants and microorganisms
and is responsible in the biosynthesis of phenylpropanoids, which is one of the classes of secondary metabolites.
GENERAL TECHNIQUES FOR EXTRACTION OF VOLATILE OIL
1. DISTILLAION: (EXPLAINED ABOVE)
2. ENFLEURAGE METHOD:
This method is used for extraction delicate volatile oil. Petals of the flower are spread on a layer
of fat present on glass sheets. The fat absorbs the volatile oil. After few days old petals are
removed & fresh petals are spread on the fat. This process is continued till fat becomes
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saturated with the volatile oil, the fat with the volatile oil is known as the pomade. The volatile
oil is extracted from the pomade.
3. EXPRESSION METHOD: Expression or cold pressing, as it is also known, is only used in the
production of citrus oils. The term expression refers to any physical process in which the
essential oil glands in the peel are crushed or broken to release the oil.
• Sponge method: The sponge is kept in water. Peel of lemon or orange is brought near
the sponge by hands and squeezed mechanically. The sponge is removed & pressed to
collect volatile oil & water. Further to eliminate the particles of peel the volatile oil is
separated from water by distillation.
• Scarification or Ecuelle method: In this method, there is round bowl to which a hollow
pipe is attached. Inside the bowl, there are pointed projections (spikes or spines like),
Peel of lemon or orange is kept in a bowl. Bowl is rotated with the machine. The
projections break oil glands of the peel. The volatile oil and liquid are collected from the
pipe. The volatile oil is separated from the liquid. e.g. Household juice extractors.
PROCEDURE:
1. Weight 25gm clove .
2. Mix 2clove with 25ml of water in distillation apparatus.
3. Heat to produce steam, which passes through sample and condenses in condenser.
4. Collect condensed liquid (oil and water) in receiver.
5. Separate oil from water using a separating funnel
6. Dry and filter oil to remove impurities.
CALCULATIONS:
• Volume of oil:
• Weight of oil:
• Density = mass/volume
• % yield= weight of oil / weight of clove x 100
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RESULT:
DISCUSSION:
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DATE:
EXPERIMENT NO: 10
OBJECT:
To determine the refractive index of volatile oil obtained by distillation process
REQUIREMENTS:
• Volatile oil sample
• Refractometer
THEORY:
VOLATILE OIL:
Volatile oil are odorous volatile principles of plant and animals source, evaporate when exposed to air at
ordinary temperature, and hence known as volatile or ethereal oils. These represents essence of active
constituents of the plant and hence also known as essential oils. Volatile oils exhibit an initial oil FVF in the
range of 1.5 to 3.0.
USES OF VOLATILE OIL:
• They may be used for their therapeutic action e.g. local stimulants, carminatives, diuretics, mild
antiseptics.
• They may be also used as spices and for flavouring of foods, confections, beverages, pharmaceuticals,
cosmetics and tobacco.
• They are most widely used in perfumery.
PROPERTIES OF VOLATILE OIL:
• Volatile oils are generally liquid and colorless at room temperature.
• They have a characteristic odor.
• They have a density less than unity, with the exception of a few cases.
• They have a refractive index and a very high optical activity.
REFRACTIVE INDEX:
It can also be defined as the ratio of the velocity of a light ray in an empty space to the velocity of light in a
substance. Refractive index is a vital parameter used to identify and characterize plant based drugs and essential
oils
n = c/v
REFRACTROMETER:
A refractometer is a tool that can determine the concentration of a particular substance in a liquid solution. It
uses the principle of refraction, which describes how light bends as it crosses the boundary between one medium
and another.
REMAINING THEORY SAME AS EXPERIMENT NO:06
PROCEDURE:
1. Clean prism and cover plate Place a small amount of liquid on the prism, and secure the cover plate. This
will evenly distribute the liquid on the prism.
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2. Turn on the light source.
3. Turn the refractometer scale knob to get the clear interface between the illuminated and dark regions.
4. When both regions are adjusted press the read button.
5. Note the refractive index shows on the screen
6. Compare the refractive index with standard range.
RESULT:
DISCUSSION:
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