Distillation

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SUBJECT:

PHARMACEUTICS-1B
ASSIGNMENT TITLE:
DISTILLATION
SECTION:
2-D
GROUP NO:
5
SUBMITTED BY:
MUSKAN GUL (70138487)
SAJID NAZIR (70137872)
HANAN ARSHAD (70137880)
MUDASSAR ALI (70136979)
NOREEN ASIF (70137797)
WAJIHA IJAZ (70137485)
ARFAH JAWED (70137926)
SUBMITTED TO:
Dr. NEERMAN
DEPARTMENT:
Faculty of Pharmacy

THE UNIVERISTY OF LAHORE


(Defence road campus, 1Km Defence Rd. Bhubtain chowk Rewind
road, Lahore, Pakistan)
DISTILLATION
DEFINITION:
Distillation is the process in which a liquid is vaporized, re-condensed (turned back into a liquid)
And collected in a container. It is a technique of separation of the constituents of a mixture
including a liquid by partial vaporization of the mixture and separate collection of the vapours.
TYPES OF DISTILLATION:
Some important types of distillation include:

• Simple distillation
• Fractional distillation
• Steam distillation
• Vacuum distillation
• Air-sensitive vacuum distillation
• Short path distillation
• Zone distillation

STEAM DISTILLATION

DEFINITION:
Steam Distillation is a method of separating temperature-dependent substances. It's a particular
type of distillation. Explaining in other terms, this is to separate the miscible liquid base
according to its volatilities. For example, aromatic compounds. It plays a vital role in certain
industrial regions. There is no chemical reaction taking place here. It's a physical process
PRINCIIPLE:

• When a mixture of two practically immiscible liquids is heated liquid exerts its own
vapour pressure as a function of temperature as if other constituent were not present.
• The vapour pressure of the whole system increases.
• Boiling begins when the sum of the vapour pressures of the two immiscible liquids just
exceeds the atmospheric pressure.
• In this way, many organic compounds insoluble in water can be purified at a temperature
well below the point at which decomposition occurs
• For example, the boiling point of bromobenzene is 156°C and the boiling point of water
is 100°C, but a mixture of the two boils at 95°C. Thus, bromobenzene can be easily
distilled at a temperature 61°C below its normal boiling point.
PROCEDURE:

• The impure compound and water are placed in a distillation flask kept at a slight slant
position and heated on a sand bath.
• Steam is then bubbled through this mixture.
• The vapours of the compound, along with steam, leave the flask from the outlet and get
condensed in the water condenser.
• The condensate collected in the receiver is transferred to a separating funnel.
• The liquid compound being immiscible with water forms a separate layer and can be
separated.

Applications of Steam Distillation:

Steam distillation is used in many industries for the purification or separation of compounds.
Some of these applications include:

1. The production of essential oils from plants.


2. The production of fragrances and flavours for the food and beverage industry.
3. The purification of natural products such as essential oils, terpenes, and cannabinoids.
4. The purification of petrochemicals.
5. The separation of compounds in the drug discovery process.
6. For extraction of volatile oils from their crude drugs_ clove oil, eucalyptus oil and anise
oil from clove, eucalyptus and anise.

VACCUM DISTILLATION
DEFINITION:
Vacuum distillation is a method of distillation whereby the pressure above the liquid
mixture to be distilled is reduced to less than its vapour pressure(usually less than its atmospheric
pressure) causing evaporation of the most volatile liquid(s) ( those with the lowest boiling
points).
PRINCIPLE:

1. Liquid boils when vapour pressure equal to the atmospheric pressure, i.e., pressure on its
surface. If the external pressure is reduced by applying vacuum, the boiling point of
liquid is lowered.
2. Therefore, the liquid boils at a lower temperature. This principle is illustrated using an
example of water. Water boils at a100 degree Celsius at an atmospheric pressure is
101.31 kPa (760mmHg). At 40 degree Celsius, the vapour pressure of water is
approximately 9.33kPa (70 mmHg). Hence, the external pressure is reduced to 9.33kPa
(70mmHg) where water boils at 40 degree Celsius. The net result is the increase in rate
of mass transfer into vapour.
PURPOSE:

The purpose of vacuum distillation is that it allows the purification of compounds not
readily distilled at ambient pressures or simply to save time or energy. This technique separates
compounds based on difference in boiling points. This technique is used when the boiling point
of the desired compound is difficult to achieve or will cause the compound to decompose. A
reduced pressure decreases the boiling point of compounds.
CONSTRUCTION AND DIAGRAM:

1. It consists of a double- neck Distillation flask knows as “Clasien flask”.


2. Thick walled glass apparatus with interchangeable standard glass joints are used for
vacuum distillation.
3. In one of the necks of the Claisen flask, a thermometer is fitted. The second neck
prevents splashing of the violently agitated liquid.
4. Bumping occurs readily during vacuum distillation. Placing a fine capillary tube in the
second neck of the flask can prevent bumping.
5. The capillary tube is dipped in the boiling liquid, so that a stream of air bubbles is drawn
out.
6. Water bath or oil bath is used for heating.
7. The Claisen flask is connected to a receiver through a condenser.
8. Vacuum pump is attached through an adapter to the receiver. A small pressure gauge
(manometer) should be inserted between the pump and the receiver.

WORKING:

1. Liquid to be distilled is filled ½ to 2/3 volume of flask.


2. Small piece of porcelain are added to avoid the process of bumping.
3. Then capillary tube and thermometer are placed in the flask.
4. Required vacuum is applied through vacuum pump.
5. The contents are heated and temperature of liquid raises and liquid get vaporized
rapidly due to vacuum.
6. Now these vapours pass through condenser and condensate is collected in
receiver.

ADVANTAGES AND DISADVANTAGES:

Advantages using vacuum is often preferable for following reasons:


1. Faster processing time.
2. Effective processing of higher boiling point solvents without igniting them or causing
thermal breakdown.
3. Vacuum distillation can improve a separation by increasing capacity, yield and purity.
Disadvantages of vacuum distillation are as follows:
1. In distillation, persistent foaming occurs. This may be overcome by adding capryl alcohol
to the liquid or by inserting a fine air capillary tube in the second neck of the Claisen
flask
2. The steam of air is drawn in and breaks the rising foam. The above method is not suitable
for the preparation of semisolid or solid extracts by distillation under vacuum.

APPLICATIONS:

The applications of vacuum distillation are as follows:


1. Preventing degradation of Active constituents like Enzymes, Vitamins, Glycosides,
Alkaloids.
2. Changing physical forms. Example: Cascara Sagrada Tablets at atmospheric
pressure form dense compact residue, but at reduced pressure form light porous mass.
3. This type of distillation is used in oil industry.
4. Separation of impurities.
5. Separation thermolabile (heat sensitive) substances. 6. Extracts or crude drugs are
prepared by this process.

DESTRUCTIVE DISTILLATION:
James Young discovered the process of destructive distillation.
Destructive distillation is a process involving the decomposition of a solid by heating it in
a closed container and collecting the resultant volatile components and is mainly used for
the distillation of coal.
PRINCIPLE:

It works on the principle of pyrolysis and large molecules are “cracked” during the process.

The most commonly produced substances from the process of destructive distillation are as
follows:

• Coke
• Coal tar
• Coal gas
• Ammonia
APPLICATION OF DESTRUCTIV PHARMACEUTICAL E DISTILLATION:
The most common applications of destructive distillation are as follows;

• Numerous substances, including tar, terpenes, turpentine, and methanol, as well as a solid
residue of charcoal, are produced during the destructive distillation of wood.
• It is an increasingly viable technique for recovering monomers produced from waste
polymers.
• The discovery of isoprene through the destructive distillation of natural rubber led to the
development of synthetic rubbers like neoprene.

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