ENVIRONMENTAL ANALYSIS LAB

ETM 521 - 2

PRACTICAL NO - 02
EXTRACTION TECHNIQUES ɪɪ

SOXHLET EXTRACTION AND SIMPLE

DISTILLATION

P. G.C.N.T.PILAPITIYA

UWU/PGU/MSC/ETM/22/019

MSc IN ENVIRONMENTAL TECHNOLOGY AND MANAGEMENT

1ST YEAR 2ND SEMESTER
Date - 01/22/23
Practical number - 02 (i)
Title - Soxhlet extraction and simple distillation

Introduction
Soxhlet extraction is a modern extraction techniques which use to circulate the
same solvent through the extractor several times. It is a type of continuous
extraction technique but we can call it a series of short maceration. Soxhlet extractor
needs the desired compound to be soluble in the solvent at a high temperature. One
cycle of the soxhlet extraction method involves extraction following the evaporation
of the solvent and theoretically the cycles can be perform as many time as want to
get maximum yield of the desired compound.

Soxhlet extraction makes the extraction process much efficient than that of the
traditional method. This extracts the compounds using the condensed vapors of the
solvent. The condensed vapor comes in contact with the sample powder and the
soluble part in the powder and the soluble part in the powder gets mixed with
solvent.

Materials
Clove, condenser, distillation flask, heat source

Methodology
(i) 2g of dried clove was weighted and placed in a thimble (W1) .
(ii) The thimble was covered with cotton wool and place in soxhlet.
(iii) A clean round bottom flask was weighted and labeled (W2).
(iv) 250ml of solvent was added to the round bottom flask and the soxhlet was sat
upped in heating mental.
(v) The water flow was connected and commenced the heating flask
(vi) The process was carried out for 2 hours.
(vii) After 2 hours, the flask was connected to a rotary evaporator.
(viii) The solvent was placed in a desiccator after evaporation.
(ix) Weight the round bottom flask (w3)
(x) The essential oil% was calculated,

Essential oil % = ( W3-W2)/W1 *100

Calculation

W1=1.45g
W2=159.19g
W3=160.07g

Essential oil % = ( W3-W2)/W1 *100 = (160.07-159.19)/1.45 *100 = 60.68%

Date - 01/22/2023
Practical no - 02 (ii)
Title - Extraction by simple distillation method.

Introduction
Distillation is a process for the purification or separation of the components in a
liquid mixture. The mixture is heated to evaporate the volatile liquid components
and the vapor is then condensed to a liquid distillation is not a chemical reaction but
it can be considered as a physical separation but it can be considered as a physical
separation process. There are several types of distillation,

(i) simple distillation (ii)Fractional distillation

(ii) steam distillation (iv)Vacuum distillation
(v)Air sensitive vacuum distillation (vi)Short path distillation
(vii)Zone distillation

The most popular method for separating miscible compounds with different boiling
points in by simple distillation.

Materials
(i) Cinnomen
(ii) Thermometer
(iii) Methanol mixture
(iv) Round bottom flask
(v) Conical flask
(vi) Condenser
(vii) Burner
Methodology - 01
(i) A known weight of (2g) of cinnomen was added to a round bottom flask with
distilled water
(ii) The steam distillation apperates was satuped.
(iii) A thermometer was fixed to the top of the flask.
(iv) The heating process was controlled for 1 hour.
(v) Condensed water was collected to a conical flask.
(vi) The following calculation was done after separation of cinnamon mixture.

Yield of essential oil = amount of material residual outcome (g)/amount of raw

material used (g)

Methodology -02
(i) The solvent mixture was added to the distillation flask (more than half of flask)
(ii) The distillation apparatus was placed carefully and placed the thermometer on
the top of the flask.
(iii)The water flow was fixed and the boiling temperature was controlled around 64.7
0
C (methanol boiling point)
(iv)The evaporated solvent was collected into a conical flask.

Calculation and results

Methodology 01

Resulted the solvent (g) = 0.53g

Weight of raw material (g) = 16.03g

Yield of essential = amount of essential oil (g) obtained/ amount of raw materials (g)
used
= 0.53g/16.03g

Methodology 02

Initial solvent color - Green

Resulted solvent color - Color less

Discussion
Clove (Syzygium aromaticum) is an aromatic spice used by several cultures around
the world. Ti is also known as cloved bud, it has been cultivated in europe since 16th
century for it’s culinary uses, mostly in curried dishes, spicy fruit cakes. Like other
species, clove bud can be used to create an essential oil that benefit to health.

Clove oil has a warm, strong, spicy small and clove oil is colorless to pale yellow with
a medium to watery viscosity. Clove oil can be extracted from plant leaves, stem and
buds and there are several methods to extracts these oils from their raw materials
such as water distillation and soxhlet extraction, supercritical CO2 extraction, hydro
and steam distillation. This experiment was used soxhlet extraction methods to
extract essential oil from their dried clove buds.
Soxhlet extraction is a common method for solid and liquid extraction. It is mainly
applied for the extraction and separation of solid samples. The soxhlet extraction
follows the principle of back-flow and siphon of the solvent and makes continuous
extraction of the needed components in the solid and liquid mixture. When the
liquid level of solvent which back-flows in the extraction shall surpass the siphon of
the soxhlet extraction, the solvent will flow back to round bottom flask, and then the
siphon happens.
As the temperature goes up the back-flow starts again. Before each time of siphon,
the solid matter can be extracted by the pure hot solvent, while in comparison with
other common solvent extraction methods, the soxhlet extraction minimizes
separation time and solvents needed and also improve the extraction efficiency.
However it can not applied to extract hot or labile elements.

There are several other plant materials that can extract using soxhlet extraction
method.

Plant name Part of the plant Solvent for extraction

Bauginville a glabra leaves methanol
Clitoriatema tea Linn leaves Petroleum, ether
Sida cardata Leaves, flowers. fruits ethanol
Hygrophilad ifformis Aerial parts Petroleum ether, benzene,
ethanol
Zanthoxylu mrhetsa stem Benzene, water, ethanol
Tecomosta nsand leaves Petroleum ether
Eclipta alba Aerial parts 50% ethanol
Cordiasubc ordota lam bark ethanol
Alternanthe rasessilis L. stems 50% methanol
Passiflorofo etida leaves methanol
Carissa spinarum leaves Petroleum ethanol
Merremiae marginate Whole plant ethanol
Cucumismelo Linn peels petroleum
Barieriapprio nites leaves methanol
Aeglemarm elas leaves ethanil

Distillation is the process of separating the compounds or substances from a liquid

mixture by selective evaporation and condensation. It is the most basic method use
for the purification of liquid mixtures. Distillation involves the heating of a liquid to
boiling and then collecting their vapors to condense them in liquid state. Distillation
is mainly apply applied in six different form according to the nature of the substance
to be purified or removed.

Simple distillation is a procedure by which two liquids with different boiling points
can be separated. Simple distillation can be used effectively to separate liquids that
have at-least 80 0C difference in boiling points. As liquid being distilled is heated, the
vapors that form will be richest in the component of the mixture that boils at lowest
temperature. Purified compounds will boil and thus turn into vapors over a relatively
small temperature range (2 or 3 0C) by carefully watching the temperature in the
distillation flask. As distillation progresses, the concentration of the lowest boiling
point component will steadily decrease. Eventually the temperature within the
apparatus will being to change, a pure compound is no longer being distilled. The
temperature will continue to increase until the boiling point of the next lowest
boiling compounds as approached. When the temperature again stabilized, another
pure fraction of the distillate can be collected. This process can be replaced until at
the fractions of the original mixture have been separated.

Essential oils also called volatile odoriferous are aromatic oily liquids extracted from
different plants as leaves, peels, barks, flowers, buds, seeps and so on. They can be
extracted from plant materials by several methods steam distillation, expression and
so on.

In steam distillation it use to separate temperature dependent substances. It is

separate the miscible liquid base according to its volatility. No chemical reaction is
take place. It is a physical process. At a very high sustained temperature level,few
organic compounds can be decompose. Often it is used to separate volatile essential
oil from the plant materials.

Part of the plant that use for distillation Plant extraction

Berries Anise, Joniper
Seeds Almand, Nutmeg, Cumin
Bark Cinnomen, Sassafran
Wood Cedar, Rose wood, Sandalwood
Rhizome Ginger
Leaves Basil, Bay, Sage, Eucalyptus, Oregone,
Pepermint, Pine, Rasemary , Tea tree,
Thyme, Lemon, Grass, Winter green
Resin Myrrh, Frankincense
Leaves Chammolie, Clovve, Geronium, Hops,
Jasmine, Lavender,Marjoram, Rose
Peels Orange, Lemon, Lime
Root Valerine

When a mixture of two immiscible liquids is heated and agitated, the surface of each
liquid exerts it’s own vapor pressure as through the other component of the mixture
is absent. An individual constituent on it’s own extracts vapor pressure
independently. Vapor pressure of the system increases consequently.

The two immiscible liquids start to boil when the vapor pressre of these liquids
outplace the atmospheric pressure. Many organic compounds are insoluble in water.
At an absolute temperature we can purify that is below the point where these
compound decompose.
As most complex organic compounds do not dissolve in water, instead they from a
mixture, which separates if allowed to settle as the water settles down and organic
compound float on top. In steam distillation, when the heating of a mixture of two or
more immiscible liquids takes place; the vapor pressure exerted by the steam
increases.

In extraction process, the steam passes through the organic matter that contains the
compounds for separation. The steam condensed and form a mixture of steam and
matter. This mixture gets heated further by passing more steam, which continues to
pass through matter, evaporating the mixture. Due to reduced vapor pressure, the
required organic compound evaporate as a part of the mixture.

Then the evaporated mixture of the steam and the organic compound passes
through a condenser that has cold water. It cool down the evaporator and settles the
separator. There are several advantages in the steam distillation such as; it’s
generate organic solvent-tree products, no need for subsequent separation steps,
can use in industrial scale, low fuel requirement, wide applications.

Steam distillation has the disadvantage of having a higher initial cost for investment
in the equipment needed to execute the process successfully and need some initial
training in order to operate the equipment. And it is a more time consuming due to
the low pressure of rising steam.

The efficiency of steam distillation can accelerate using microwave irradiation,

increase the boiling point of the solvent and reducing partial pressure of steam.
Simple distillation also contain some advantages such as low requirement of
materials, simple and fast process consume less energy than other distillation
methods and some disadvantages like poor separation compare to other separation
methods require pure compounds/raw materials for the separation, need to redo
process multiple time to obtain 99% pure component, requires a 50 0C difference in
boiling point for a good separation.

Efficiency of simple distillation can improve by using multiple phase column.

Nowadays there are several new technologies to extract essential oil as,

(I) Hydro distillation - use boiling water and plant or steam

(II) Physio-chemical process - Hydro diffusion, hydrolysis, decomposition by heat
treatment
(III) Water distillation
(IV) Ohmic-Heated water distillation
(V) Microwave assistant water distillation

Conclution
In soxhlet extraction, they use a liquid to dissolve a target molecule or group of
compound and to wash them out of the solid plant material and this method
complete extraction with minimum amount of solvent. Simple distillation
successfully separate solvent depend on their boiling point and it is an easy
experiment to handle but take a long time to give the result.

Reference
(i) Binous, H., abd Al-Harithi, M.A., (2014) ‘simple batch distillation of a binary
mixture’ BComputer applications in engineering education 22(4), pp 649-657

(ii) Luque de Costro, M.D., and Gorcia - Aussco,L.E., ‘soxhlet extraction of solid
materials:an outdated technique with a promising inovative future’ Analytical
chemica acta, 369(1-2) o1-10

(iii)Ramluckan, K., Moodley, K.G., and Bux, F., (2014) ‘An evalution of the efficiency
of using selected solvent for the extraction of lipids 116, pp 103-108.

(iv)Seroor Atalah Khaleefa Aki Khaleefa Ali and Qitan, M.A., (2021) ‘ simple
distillation)