SISP

SUBJECT NAME:Pharmaceutical Unit Operations - II

Name of the Department: pharmaceutical technology

Page 1

SISP

SUBJECT NAME:Pharmaceutical Unit Operations - II

EXPERIMENT NO: 04

NO.4 Evaluation of Stability by Centrifugation

Aim:
To study the influence of centrifugal effect in separating the oil phase of freshly prepared
turpentine liniment emulsion I.P.
Requirements:
Turpentine, liniment emulsion, centrifuge with graduated tubes, beakers, stirrer,
measuring cylinder and balance.
Principle:
Centrifugal force is used to provide the driving force for the separation. Centrifugation is
particularly useful when separation by ordinary filtration is difficult. For example separating
highly viscous mixtures and colloidal dispersions in which difference in the densities is less.
Centrifugation provides a convenient method of separating either 2 immiscible liquids or solids
from a liquid. In this experiment turpentine liniment is subjected to centrifugal force into a
centrifuge operated at a speed of 4000 rpm for 80 minutes. Percent oil separated is calculated
for every 5 minutes in both the cases, with the data obtained graphs are plotted by taking
centrifugation time versus percent volume of turpentine oil separated.
Theory:
Centrifugation is a unit process employed for separating the constituents present in
dispersion with the aid of centrifugal force. The equipment in which centrifugal force is implied
on dispersion is called centrifuge.
r
m

Separating power of a centrifuge is expressed as centrifugal force effect. It is a ratio of

centrifugal force to gravitational force. Centrifugal effect can be calculated by using the
following equation.
Centrifugal effect = 2.013 dm2
Diagram:
Name of the Department: pharmaceutical technology

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SISP

SUBJECT NAME:Pharmaceutical Unit Operations - II

Procedure:
Preparation of turpentine liniment:
1. Soft soap was transferred into a motor and add few ml of water and resulting mixture was
triturated.
2. In another beaker required quantity of camphor was dissolved in turpentine oil.
3. This solution was transferred into motor with continuous trituration until a soft cream is
formed then it was transferred to a measuring cylinder and made up to a level with
required number of water.
Step 2:
1. The calculated centrifuge tubes are cleaned labeled and filled with turpentine liniment up
to the 10 ml mark.
2. The tubes are placed in the basket, the centrifuge is switched on.
3. The centrifuge is allowed to exert centrifugal effect on the emulsion for 5 minutes.
4. After 5 minutes the speed controlled knobs is turned anti clock wise for 4 position to 0
position, when a setar has came to the centrifuge and the centrifuge tubes are taken out.
5. The volume of turpentine oil separated which is present as a lower tube is noted as
regarded.
6. Without disturbing the tubes are placed back into the basket.
7. This is repeated for 30 minutes with 5 minutes time interval and all the readings were
tabulated.
8. A graph is plotted by taking centrifugation time on x- axis and percent volume of
turpentine oil separated on y- axis.
Applications:
Name of the Department: pharmaceutical technology

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SISP

SUBJECT NAME:Pharmaceutical Unit Operations - II

1. Evaluation of suspensions and emulsions.

2. Determination of molecular weight of colloids.
3. Production of biological products.
4. Production of bulk drug.
5. Biopharmaceutical analysis of drugs.
Graph:
Graph is plotted by taking centrifugation time on x- axis and percent volume of turpentine oil
separated on y- axis
Report:
The volume of turpentine oil separated _____________ with _____________in centrifugation
time.
Table
S no.
Ingredients
Quantity for 100 ml
Purpose
Potassium hydroxide
5.25 gm
1
Emulsifying agent
Arachis oil
20 ml
Oleic acid
5 ml
2
Camphor
5 gm
Anti microbial
3
Turpentine oil
65 ml
Counter irritant
4
Purified water
Up to 100 ml
Vehicle

Separation of Oil from Emulsion with 4000 Rpm

Time of
Volume of turpentine oil separated (ml)
S
centrifugatio
no.
n
Name of the Department: pharmaceutical technology

Averag
e
volume

% oil separated=
x100/
total volume of
Page 4

SISP

SUBJECT NAME:Pharmaceutical Unit Operations - II

(min)

(x)
Centrifuge
tube (A)

1.2 ml

1.4 ml

1.5 ml

1.9 ml

Centrifuge
tube (B)

Centrifuge
tube (C)

emulsion

Centrifuge
tube (D)

Question & Answers for Viva Voice

Name of the Department: pharmaceutical technology

Page 5

SISP

SUBJECT NAME:Pharmaceutical Unit Operations - II

EXPERIMENT NO: 05

NO.5 Construction of Drying Rate Curve of CaCO3 Using Tray Dryer

Aim:
To construct the drying rate curve of CaCO3 using tray dryer.
Requirements:
Dryer, stainless steel plate, beaker, balance and CaCO3.
Theory:
Drying is defined as removal of small amount of water or other liquid from a material by
the application of heat. Drying involves both heat and mass transfer operations. Heat must be
transferred to the material to be dried in order to supply the latent heat required for vaporization
of moisture. Mass transfer involves the depletion of water through the material to the
evaporating surface and subsequent evaporation of water from the surface.
Water content- equilibrium relationship
In wet solid mass water will be present as bound and unbound water. Bound water is the
minimum water held by the material that exerts on equilibrium vapor pressure less than the pure
water at the same temperature.
Unbound water is the amount of water held by the material that exerts an equilibrium
vapor pressure equal to that of the pure water at the same temperature.
Equilibrium relationships:
Air of constant temperature and humidity is passed over the wet solid. After a long
exposure equilibrium of the process will be attained. Further exposure will not alter moisture
content in the solid. At this stage vapor pressure of wet solid is equal to that of the surrounding
atmosphere. Hence there is no drying or mass transfer. Based on the moisture content present in
the sample several terms are expressed. Equilibrium moisture content is the amount of water
present in the solid that exerts vapor pressure equal to that of vapor pressure of atmosphere
surrounding it.
Free moisture content is the amount of water i.e. free to evaporate from the solid surface.
FMC= total water content EMC.

Name of the Department: pharmaceutical technology

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SISP

SUBJECT NAME:Pharmaceutical Unit Operations - II

Principle:
Rate relationship can be studied considering simple model, which we mimic the
conditions of a dryer. In this model the wet slab of material of sufficiently high moisture content
is placed in the tray whose sides and bottoms are insulated the air is blown over the solid under
constant drying conditions. The superficial water diffuses through the surrounding stationary air
film and is carried away rapidly by the moving air stream, then water diffuses from interior of
the solid to the surface. This process continues until pond water gets evaporated. Then the
material attains equilibrium moisture content.
The rate of drying can be determined by periodically weighing CaCO 3 slurry. The
difference in the weights of two successive weights gives the loss of moisture content i.e.
amount dried. The following equation is used to calculate the rate of drying.
Procedure:
Preparation of turpentine liniment:
4. Soft soap was transferred into a motor and add few ml of water and resulting mixture was
triturated.
5. In another beaker required quantity of camphor was dissolved in turpentine oil.
6. This solution was transferred into motor with continuous trituration until a soft cream is
formed then it was transferred to a measuring cylinder and made up to a level with
required number of water.
Step 2:
9. The calculated centrifuge tubes are cleaned labeled and filled with turpentine liniment up
to the 10 ml mark.
10.The tubes are placed in the basket, the centrifuge is switched on.
11.The centrifuge is allowed to exert centrifugal effect on the emulsion for 5 minutes.
12.After 5 minutes the speed controlled knobs is turned anti clock wise for 4 position to 0
position, when a setar has came to the centrifuge and the centrifuge tubes are taken out.
13.The volume of turpentine oil separated which is present as a lower tube is noted as
regarded.
14.Without disturbing the tubes are placed back into the basket.
15.This is repeated for 30 minutes with 5 minutes time interval and all the readings were
tabulated.
16.A graph is plotted by taking centrifugation time on x- axis and percent volume of
turpentine oil separated on y- axis.
Applications:
6. Evaluation of suspensions and emulsions.
Name of the Department: pharmaceutical technology

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SISP

SUBJECT NAME:Pharmaceutical Unit Operations - II

7. Determination of molecular weight of colloids.

8. Production of biological products.
9. Production of bulk drug.
10.Biopharmaceutical analysis of drugs.
Report:
The volume of turpentine oil separated _____________ with _____________in centrifugation
time.

S no.

Ingredients
Potassium hydroxide

Table
Quantity for 100 ml
5.25 gm

Arachis oil
Oleic acid
Camphor
Turpentine oil
Purified water

20 ml
5 ml
5 gm
65 ml
Up to 100 ml

2
3
4

Purpose
Emulsifying agent
Anti microbial
Counter irritant
Vehicle

Separation of Oil from Emulsion with 4000 Rpm

S
no.

Time of
centrifugatio
n
(min)

Volume of turpentine oil separated (ml)

Centrifuge
tube (A)

1.2 ml

1.4 ml

1.5 ml

1.9 ml

Centrifuge
tube (B)

Centrifuge
tube (C)

Averag
e
volume
(x)

% oil separated=
x100/
total volume of
emulsion

Centrifuge
tube (D)

Question & Answers for Viva Voice

Name of the Department: pharmaceutical technology

Page 8

SISP

SUBJECT NAME:Pharmaceutical Unit Operations - II

Name of the Department: pharmaceutical technology

Page 9