Laboratory Manual of Pharmaceutical

KMCT COLLEGE OF PHARMACY

AFFILIATED TO KERALA UNIVERSITY OF HEALTH SCIENCES (KUHS)
PAZHUR, KUTTIPPURAM-679 571
(Affiliated to Kerala University of Health Sciences)
(Approved by AICTE, PCI and GOVT. of Kerala)

PHARMACEUTICAL ENGINEERING
PRACTICAL RECORD
Course: B pharmacy
Third semester
Prepared by: Ms. Jincy C P

Name: …………………………………………………………………...
Reg. No.…………………………………………………………………
Year: ……………………………………………………………………

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Laboratory Manual of Pharmaceutical
INDEX
SL EXPERIMENT EXPERIMENT VIVA VOCE REMARK
NO MARK
1 Factors affecting rate of Filtration
(Surface Area, Concentration ,
Viscosity
and Thickness)
2 Effect of Filter Aid on Rate of
Filtration

3 Factors affecting rate of

Evaporation (Surface Area,
Concentration and Thickness/
Viscosity)
4 Drying rate curve for Calcium
Carbonate
5 Drying rate curve for Starch
6 Determination of moisture content
and loss on drying
7 Determination of Humidity Of Air –
From Wet And Dry
BulbTemperatures (Use Of Dew
Point Method)
8 Determination of
humidity by
Psychrometric method
9 Particle size determination by
Sieving Method
10 Particle size determination by
beaker decantation method
11 Size reduction
12 Description of Construction,
Working And Application Of
Pharmaceutical Machinery Such As
Rotary Tablet
Machine, Fluidized Bed Coater,
Fluid Energy Mill, De –Humidifier
13 Demonstration Of Colloid Mill,
Planetary Mixer, FluidizedBed
Dryer,
Freeze Dryer

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Experiment No:1 Date:

EFFECT OF MATERIAL RELATED FACTORS ON

FILTRATION RATE

AIM
To study the effect of material related factors on the rate of filtration, using calcium
carbonate suspension.

REQUIREMENTS
Measuring cylinder (100ml), Mortar and pestle, Beakers (500ml), Buchner funnel, Buckner
flask(1000ml), Balance, Filter paper, calcium carbonate, Glycerin, Kieselguhr, talc, charcoal.

PRINCIPLE
Filtration may be defined as a process of separation of solids from a fluid by passing the
same through a porous medium that retains the solids, but allows the fluids to pass
through.
The following terms are used with respect to filtration. The suspension (solid in a liquid
medium) to be filtered is known as slurry. Here, slurry of calcium carbonate in water is
used. The porous medium is used to retain the solid is described as the filter medium.
The solids retained on the filter is referred to as filter cake, while the clear liquid that
passes through is known as filtrate. When solids are present in very low concentration.
i.e., not exceeding 1%w/v, the process of its separation from liquid is known as
clarification.
Surface filtration type is employed, i.e., pores and holes of the medium prevent the
passage of solids. Filterpaper is used as a filter medium. The mechanisms involve dare
straining and impingement. The effect of concentration of suspension, effect of
viscosity of the vehicle and the effect of filter aid are the material related factors that
are studied in this experiment.
Mechanism of filtration:

The mechanism whereby particles are retained by a filter is significant only in the initial
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stage of filtration. Some mechanisms are straining, impingement, entanglement and
attractive forces.

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Theory of filtration

The flows of fluid through a filter follow the basic rules that govern the flow of any liquid
passing through a medium, offering resistance. The rate of flow can be expressed as:
Rate of flow = Driving force
Resistance

The rate of filtration may be expressed as volume per unit time (ml/mt or L/hr).
Driving force is pressure difference between upstream and downstream of the filter.
The resistance increases with increase in deposition of solid on filter medium, so
filtration may not be uniform.
The factors affecting the rate of filtration were explained by Darcy’s equation. The
equation correlating the rate factors is known as Darcy’s law and may be expressed
as:

𝑉 = K A ΔP
ηL

Where,

V = rate of flow
K = permeability coefficient of cake, m2
A = surface area of porous bed (m2) filter

medium ΔP = pressure difference across

the filter medium η = viscosity of the

filtrate

L = thickness of the cake

Some of the factors affecting the rate of filtration are as follows
1. Surface area of the filter medium
The rate of the filtration can be increased by increasing the surface area of
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the filter medium. Hence rate can be increased by using large filter. The area
can also be increased by using a no. of small units in parallel.

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2. Pressure difference across the filter medium

Rate of filtration is directly proportional to overall pressure drop ie. across
both filter medium and filter cake. This can be achieved by

a) Gravity: a simple method of obtaining a difference in pressure is by

maintaining a bed of slurry above the filter medium. The pressure developed
will depend on density of the slurry.
b)Reduced pressure: the pressure below the filter medium may be reduced
below atmospheric pressure by connecting the filter receiver to a vacuum
pump and creating apressure difference across the filter.
c) Applying pressure: the common method is to obtain suitable pressure
difference by applying pressure to the surface of the slurry. The simplest
method is to pump the slurry into the filter medium under pressure.
3. Viscosity of the filtrate
Viscosity is inversely proportional to the rate of filtration. By rising the
temperature of the liquid, can increase the rate of filtration. When temperature
increases viscosity of the liquid decreases.

4. Thickness of filter cake

It is inversely proportional to the rate of filtration. In some slurries containing
high proportion of solids, it may be advantageous to reduce the rate at which
the cake

accumulates. This may be done by a primary decantation or straining which will

lower the solid content of the slurry.

Filtration is having different application in pharmaceutical industry such as

production of sterile products, production of bulk drugs, production of liquid oral
formulations and used in effluent and water treatment.

PROCEDURE:
I. Effect of Surface area:

1. Arrange the Buchner funnel of different size along with filter paper.
2. Pass 50ml of sugar syrup or 50ml of water through each of them and
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note the time taken for complete filtration.

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3. Calculate the area of filter paper and note the area in the table.
4. Plot the graph of rate of filtration Vs area of filter medium

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Effect of Concentration of slurry:

Preparation of calcium carbonate suspension

2 g of calcium carbonate was weighed and transferred to a mortar. 50 ml of water

is added and triturated to get a smooth paste. The contents are transferred into a
100 ml measuring cylinder. The mortar and pestle are washed with 10 ml water (2
or 3 times). The washings are transferred into the measuring cylinder. The volume is
made up to the mark by adding water. The suspension is shaken thoroughly.
The same procedure is repeated to prepare 4% and 6% suspensions using 4 g and
6g of calcium carbonaterespectively.

1. Prepare 100ml of 2%, 4%, and 6% W/V CaCO3 solution.

2. Arrange the filtration assembly with a single filter paper.
3. 100 ml of 2% calcium carbonate suspension was poured over the Buchner
funnel.
4. Time required to collect 50 ml of the filtrate was recorded in the table.
5. The experiment was repeated for same concentration of the suspension
for two more trials.
6. The experiment was repeated for other concentrations also.
7. The readings are recorded and the filtration rate was calculated from
the following equation:Rate of filtration = volume of filtrate passed
through the filter medium
Time required for the filtrate to pass through
8. A graph was plotted by taking concentration of
calcium carbonatesuspension on x-axis and rate of filtration
on y-axis.

II. Effect of Viscosity:

1. Arrange the Buchner funnel with filter paper.

2. 100 ml of 4% calcium carbonate suspension containing 2% glycerin
was poured over the Buchner funnel.
3. Time required to collect 50 ml of the filtrate was recorded in the table.
4. The experiment was repeated for same suspension for two more trials.
5. The experiment was repeated for
suspensions containing increased concentration of glycerin.
6. The readings are recorded and the filtration rate was calculated from the
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following
equation:

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Rate of filtration = volume of filtrate passed through the filter medium

Time required for the filtrate to pass through
7. A graph was plotted by taking concentration of glycerin in calcium
carbonate suspension on x-axis and rate of filtration on y-axis.

III. Effect of Thickness of filter beds (in terms of no. of filter paper):

1. The filter paper of appropriate size and known thickness (one filter
paper) was placed into the Buchner funnel.
2. 100 ml of 2% calcium carbonate suspension was poured over the Buchner funnel.
3. Time required to collect 50 ml of the filtrate was recorded in the table.
4. The experiment was repeated for same thickness for two more trials.
5. The experiment was repeated for two more filter media of same material
of different thickness(two and three filter papers can be used).
6. The readings are recorded and the filtration rate was calculated from
the following equation:
7. Rate of filtration = volume of filtrate passed through the filter medium

Time required for the filtrate to pass through

8. A graph was plotted by taking thickness of filter medium on x-axis
and rate of filtration on y-axis.

REPORT:

Effect of Surface area

As the surface area of filter medium increases, the rate of filtration
A graph was plotted by taking area of filter medium on x- axis and rate offiltration on y-
axis.

Effect of concentration of slurry

As the concentration of calcium carbonate increases, the rate of filtration

A graph was plotted by taking concentration of calcium carbonate suspension on

x- axis and rate offiltration on y-axis.

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Effect of viscosity of slurry

As the viscosity of calcium carbonate suspension increases, the rate of filtration
.

A graph was plotted by taking concentration of glycerin in calcium carbonate

suspension on x-axisand rate of filtration on y-axis.
Effect of thickness of filter medium
With the increase in thickness of filter medium, rate of filtration _.

A graph was plotted by taking thickness of filter medium on x-axis and rate of
filtration on y-axis.

REFERENCE
Laboratory manual of pharmaceutical engineering; C.V.S Subrahmanyam, [Link],
V. Kusumdevi, Sarasija Suresh; Page no.115-119.

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Experiment No:2 Date:

EFFECT OF FILTER AID ON RATE OF FILTRATION

AIM:
To study the effect of filter aid on the rate of filtration and to determine the
optimum concentration of filter aid.
REQUIREMENTS:
CaCO3, Bentonite, Funnel, Filter papers, Conical Flasks, balance measuring cylinder
PRINICIPLE:
Filtration may be defined as separation of solid from a liquid by means of porous
medium that retains the solid but allows the fluid to pass.
Usually the resistance to flow due to the filter medium itself is very low. But will
increase as the layer in the medium and forming the solids build up, blocking
pores of the medium and forming the solids impervious cake. The objective of
the filter aid is to prevent the medium from becoming block and to form open
porous cake, so reducing the resistance to flow the filterate. Thus the filter aid
must be a light porous inert solid. Filter can be used in either or both of two
ways.
1. By forming a precoat over the medium by filtering a suspension of
the filter aid sufficientto give a coating upto 0.5kg/m2.
2. A small portion of filter aid (0.1 to 5%) is added to the slurry, ensuring that
the filter cakehas a porous structure.
Examples of filter aid are bentonite, keiselghur, charcoal and kaolin.
PROCEDURE:

Weighed accurately 5 gm of CaCO3, transferred to graduated conical flask and

add water to dissolve calcium carbonate and make up the volume to 100ml.
Prepare solution like step I for five numbers in different conical flask. Then add
bentonite in the concentration of 0.0%, 0.1%, 0.2%, 0.3%, 0.4% and 0.5% to the
above solutions. Number the conical flask as 1, 2,
3, 4, 5 and
6. Now pass the first sample (0.0% bentonite in 5% calcium carbonate) marked
as number 1 through a selected filter paper and note the time taken for filtration.
Similarly repeat the entire environment for remaining solutions and determine
the time required for filtration and record them.
Determine the optimum concentration of filter aid.

For the optimum concentration of filter aid, draw a graph by taking

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concentration of aid on x- axis and rate of filtration on y-axis as the concentration of
filter aid is increased rate also increases. But point reaches where further addition of
filter aid decreases the rate of filtration. Concentration at

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this point is the optimum concentration of filter aid.

REPORT:

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Experiment No:3 Date:

FACTORS AFFECTING RATE OF EVAPORATION (SURFACE

AREA, CONCENTRATION, THICKNESS AND VISCOSITY)

AIM:
To study the effect of surface area, concentration, thickness and viscosity on rate of
evaporation.
REQUIREMENTS:
Funnel, Filter papers, Conical Flasks, balance, measuring cylinder.
PRINCIPLE:
Evaporation is a process of vaporizing large quantities of volatile liquid to get a
concentrated product. Evaporation is a surface phenomenon i.e., mass transfer
takes place from surface. The practical definition of evaporation is the removal
of solvent from solution by boiling the liquor ina suitable vessel and withdrawing
the vapours leaving concentrated liquid residue in the vessel.

M= KS (b-b’)
p
M= mass of vapour formed per unit time (rate),
m3/s S= surface area of the liquid exposed, m2
P= Atmospheric pressure, kPa
b= Maximum vapour pressure at the temperature of air, kPa
b’= pressure due to the vapour of the liquid, actually present in the
air, kPa K= constant, m/s
There are many factors which influence the rate of evaporation. They are as follows:

1. Temperature:-
As the temperature increases, the rate of evaporation also increases. This is
because when temperature increases, the kinetic energy of molecule
increases to vapour state. This is the situation below the boiling point of
liquid

2. Vapour pressure:-

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Rate of evaporation is directly proportional to the vapour pressure of the
liquid. Lower the external pressure, lower the boiling point of the liquid and
hence greater will be the

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rate of evaporation.

Surface area:-
As the surface area increases, the rate of evaporation also increases. For this
reason evaporation is conducted in evaporators with larger heating surface
area.
3. Time of exposure:-
If time of exposure is longer, greater will be the rate of evaporation provided
the constituents are thermo stable. Exposure of a drug to a relatively high
temperature for a short period of time may be less destructive of active
principles than a lower temperature with long exposureperiod.
4. Viscosity:
Viscosity is inversely proportional to the rate of evaporation. As the viscosity
increases, the rate of evaporation decreases.
5. Concentration:
As the concentration of the feed increases, the rate of evaporation decreases.

PROCEDURE:

Effect of surface area

 Beakers measuring 50 ml, 100 ml and 250 ml are cleaned.
 25ml quantity of water is taken in each beaker.
 Beakers containing water are weighed. The weights are recorded (initial weight, w1g.).
 All the beakers containing water are heated in a water bath at constant
temperature (70oC)for 30 minutes.
 After heating all the beakers are weighed again. The weights are
recorded(final weight ofbeaker, w2g).
 The difference between the weights are determined, w g. The difference
reflects the amountof water evaporated during 30 minutes.
 Radius of the beaker is noted. Using the radius, surface area is
calculated using the formulaSurface area of beaker=𝜋 r2
 Rate of evaporation is calculated using formula
Rate of evaporation = quantity of water evaporated (w) g
Time of heating in minutes min
 A graph is plotted by taking rate of evaporation on y-axis and surfacearea on y-axis.

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Effect of viscosity

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Different concentration of glycerine- water mixtures are weighed (w3 g).

Viscosities of these mixtures at room temperature are given in table.

Glycerin (ml) Water (ml) Concentration (%)
5 45 10
10 40 20
15 35 30
20 30 40

 The beaker containing glycerine -water mixture are weighed.

 All the beakers are heated in a water bath at constant temperature (70oC).
 All the beakers are weighed again (w4 g)
 The difference between the weights is determined.
 Rate of evaporation is calculated.
 A graph is plotted by taking rate of evaporation on y-axis and viscosity on x-axis.

Effect of concentration
 2,4,6 and 8%w/v solutions of sodium chloride are prepared by dissolving
1,2,3 and 4g of sodium chloride in 50ml water
 The initial weights are noted (w5g).
 All the beakers are heated in a constant temperature for 30 minutes.
 All the beakers are weighed again after heating (w6g).
 The difference between the weights is determined.
 Rate of evaporation is calculated.
 A graph is plotted by taking rate of evaporation on y-axis and
concentration on x-axis.

REPORT
Effect of surface area
With increase in surface area, rate of evaporation

A graph is plotted by taking surface area on x-axis and rate of evaporation on y-axis.
Effect of viscosity
With increase in viscosity of solution, rate of evaporation .
A graph is plotted by taking viscosity of solution on x-axis and rate ofevaporation
on y-axis.
Effect of concentration
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With increase in concentration of sodiumchloride solution, rate of evaporation

.
A graph is plotted by taking concentration of sodium chloride on x-axis and rateof
evaporation on y- axis.

REFERENCE
Laboratory manual of pharmaceutical engineering; C.V.S Subrahmanyam, [Link],
V. Kusumdevi, Sarasija Suresh; Page no.115-119.

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Experiment No:4 Date:

DRYING RATE CURVE OF CALCIUM CARBONATE

AIM:
To dry the given wet solid and construct a drying curve for calcium carbonate.
REQUIREMENTS:
Dryer, balance(triple beam), beaker.

PRINCIPLE:
Drying is defined as the removal of small amounts of water or other liquid from a
material by application of heat.
In this experiment the wet slab to be dried is placed in a tray whose bottoms and sides
are insulated. The air is blown over the solid under constant drying conditions. The
superficial water diffuses through the surrounding air film and is carried away rapidly
by the moving air stream. Then water diffuses from the interior of the solid to the
surface. This process continues until bound water gets evaporated. Then the
material attains equilibrium moisture content.
Rate of drying of this process can be determined by periodically weighing the
calcium carbonate slurry. The difference in the weights of two successive weighings
gives the loss of moisture content, i.e. amount dried. The following equation is used
to calculate rate of drying:
Rate of drying = weight of water removed
g/g.h.cm2 weight of dry powder×time of drying
×surface area exposed
A graph is plotted by taking FMC on x-axis and drying rate on y-axis. The curve
soobtained is called as drying rate curve. It represents different changes occurring
during drying, where “AB” is constant rate period, “BC” is first falling rate period, and
“CD” is second falling rate period. The FMC at the end of constant rate period is
known as critical moisture content (CMC).

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FMC Curve

The typical drying curve in the figure has four stages. They
are as follows:AB – Initial adjustment period
BC – Constant rate period during drying in which the rate of diffusion of moisture
from the interior of the solid to the diffusion layer formed on the surface of solid
will be equal to the rate of evaporation.
CD – First falling rate
period of dryingDE –
Second falling rate period
Moisture content at ‘E’ is equilibrium moisture content. Drying gets stopped when
moisture content reaches E.

PROCEDURE
1. The petridish was weighed and the weight was recorded as w1.
2. 5 g of calcium carbonate was transferred into a beaker. 10 ml of water was
added to prepare a
slurry
3. The starch slurry was transferred into the petridish.
4. Filling must be done in such a way that 3/4th of the volume of the petridish was
filled with slurry.
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5. The weight of petridish was taken and recorded as w2.

6. The petridish containing slurry was placed in dryer, whose temperature must
bemaintained at 60oC.

7. The time is noted soon after placing the petridish containing slurry in a dryer.
8. After 15 minutes, the weight of petridish with slurry was taken and the
weightwas recorded in thetable.
9. Again the petridish containing slurry was placed in the dryer. (Petridish should
be immediately placedback into the dryer, otherwise temperature decreases
enormously and result will be erroneous).

10. Steps 8 and 9 are repeated until constant weight was obtained.
11. The rate of drying was calculated.
12. A graph was plotted by taking free moisture content on x-axis and rate of drying on y-axis.

REPORT

Drying rate curve is plotted by taking FMC on x- axis and rate of drying on [Link]
moisture contentremoved from starch slurry was found to be ……g

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Experiment No:5 Date:

DRYING RATE CURVE OF STARCH

AIM:
To dry starch slurry and plot the rate of drying curve.

REQUIREMENTS:
Starch, dryer, balance, petridish, beaker.

PROCEDURE
1. The petridish was weighed and the weight was recorded as w1.
2. 5 g of starch was transferred into a beaker. 10 ml of water was added to prepare a slurry.

3. The starch slurry was transferred into the petridish.

4. Filling must be done in such a way that 3/4th of the volume of the petridish
wasf illed with slurry.
5. The weight of petridish was taken and recorded as w2.
6. The petridish containing slurry was placed in dryer, whose temperature must be
maintained at 60oC.

7. The time is noted soon after placing the petridish containing slurry in a dryer.
8. After 15 minutes, the weight of petridish with slurry was taken and the
weight was recorded in thetable.
9. Again the petridish containing slurry was placed in the dryer. (Petridish
should be immediately placedback into the dryer, otherwise temperature
decreases enormously and result will be erroneous).

10. Steps 8 and 9 are repeated until constant weight was obtained.
11. The rate of drying was calculated.
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12. A graph was plotted by taking free moisture content on x-axis and rate of drying on y-axis

REPORT
Drying rate curve is plotted by taking FMC on x- axis and rate of drying on y-axis. Total
moisture content removed from starch slurry was found to be ……g.

REFERENCE
Laboratory manual of pharmaceutical engineering; C.V.S Subrahmanyam, J. Thimma Setty, V.
Kusumdevi, Sarasija Suresh; Page no: 132-137.

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Experiment No:6 Date:

DETERMINATION OF MOISTURE CONTENT AND LOSS ON DRYING

AIM:
To determine the moisture content and loss on drying.
REQUIREMENTS
Petridish, Measuring cylinder, Pipette, Tray dryer, Calcium carbonate, Spatula, Weighing balance
PRINCIPLE:
The behavior of drying of solid is explained by drying curve. The time
required for drying a batch of weight of material in a dryer can be estimated
with the help of drying curve.
Drying curves are graphical representation obtained by drawing
percentage moisture content present during drying versus the drying wet
solid in a dryer and by determining the moisture content present at
particular intervals.
Weight of water
Percentage Moisture Content = Weight of dry solid x 100

Kg of moisture
Drying Rate =
Area of Petri dish x
time

PROCEDURE:
 Take clean dry petridish and weight it (x)
 Weigh 10g of calcium carbonate powder and transfer to petridish and weight it
 Add sufficient amount of water with the help of
pipette to the powder until slurryform.
 Again weigh the petridish and note down weight (y)
 Place the petridish in tray dryer and weigh it at every 5 min
 Allow it to dry until it’s constant weight the down the constant dry weight (z)
 Calculate the percentage loss on drying and percentage
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moisture content for the givensample.

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 Percentage moisture content (PMC) and rate of drying for

each time interval calculatedby following equation

𝑃 𝑀𝐶 = 𝑊 4 − 𝑊 2 X 100
W2-W1

REPORT:
 The moisture content and loss on drying was determined
 The percentage of moisture content is =
 The loss on drying is =

REFERENCE:
Laboratory manual of Pharmaceutical engineering C V S Subrahmanyan, J
Thimma setty first edition 2006 page no: 126-131

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Experiment No:7 Date:

DETERMINATION OF HUMIDITY OF AIR BY DEW POINT METHOD

AIM:
To determine the humidity of air by dew point method.

REQUIREMENTS:
Dew point is defined as the temperature to which a mixture of air water vapour must
be cooled (at constant humidity) to become saturated ( i.e. to be in equilibrium with
liquid)
Formation of mist and disappearance of mist are considered and dew point is
determined. Dew point temperature is noted on the temperature axis (x-axi-s) and
moved vertically on the psychrometric chart. The intersect point at saturated curve
(100%) is identified. The coordinates of the point (temperature, K , humidity) are
noted. The y-axis point is the humidity of air
The cooled and polished disk is placed in the vessel. The vessel is cooled gradually. At a
particular temperature, the mist begins to form and the temperature is noted. It is the
dew point. Alternatively, dew point can be determined using a round bottom flask
PROCEDURE
 A round bottom long neck flask (100 ml) was thoroughly cleaned and
dried the externalsurface.
 Water was filled into the flask upto 2/3rd volume.
 The above flask was kept on a glass tripod stand.
 A thermometer was dipped in the water.
 Crushed ice was slowly added to the water and stirred thoroughly with
the help of a glassrod.
 As the temperature of water was lowered, mist begins to form on the outer
bottom surfaceof the flask. At this point, the temperature was noted. This is
the dew point temperature.
 In psychrometric chart, from the temperature (x-axis) moved vertically up until
the saturation curve and identified the intersecting point. The coordinates of
the (temperature, humidity) intersecting point was noted. The y coordinate is
the humidity.

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REPORT
Humidity of the air was found to be lb water vapour/ lb dry air

REFERENCE
Laboratory of pharmaceutical engineering; C.V.S Subrahmanyam, J. Thimma Setty,
[Link], Sarasija Suresh; page no. 144-146.

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Experiment No:8 Date:

DETERMINATION OF HUMIDITY BY PSYCHROMETRIC

METHOD

AIM

To determine the humidity, humidity at adiabatic saturation, dewpoint, adiabatic

saturation temperature, humid heat, specific volume and percentage humidity of a
mixture of air.

PRINCIPLE

Humidity is defined as pounds of water vapour carried by one pound of dry air under
any given set of conditions.
Dry bulb temperature is the temperature of moist air when it is measured at rest. Wet
bulb temperatureis the dynamic equilibrium temperature attached by a water surface,
when exposed to air under adiabatic conditions.
In psychrometric method both dry and wet bulb temperatures are determined by
using a sling psychrometer. From the chart, the intersection point is identified atwhich
saturated curve crosses wet bulb temperature. From this point, horizontal line towards
y-axis is drawn and humidity values are noted. Percentage humidity was calculated
from equation
Percent humidity = humidity of air

Humidity of saturated air

PROCEDURE

Take two thermometers. Hang one thermometer at a place where air is free flowing.
The temperature recorded by this thermometer is the dry bulb temperature. Hang
other thermometer and cover the bulb with cotton and dip the other end of cotton in a
beaker containing water and the temperature reported by this thermometer is called
wet bulb temperature. The dry bulb temperature and wet bulb temperature are noted
for conditions inside the laboratory, outside the laboratory and in open air. From the
given wet bulb temperatures and dry bulb temperatures using psychrometric chart the
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humidity, dew point, adiabatic saturation temperature, humidity at adiabatic condition,
specific volume, humid heat and percentage humidity was determined for different
conditions.

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REPORT

The humidity, humidity at adiabatic saturation, dew point, adiabatic saturation

temperature, humid heat, specific volume and percentage humidity of a mixture of air
at different wet bulb and dry bulb temperature was determined from the
psychrometric chart.

REFERENCE

Laboratory manual of pharmaceutical engineering; C.V.S Subrahmanyam, [Link] Setty,

[Link], Sarasija Suresh; Page no.138-142.

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Experiment No:9 Date:

PARTICLE SIZE DISTRIBUTION OF POWDER BY SIEVING METHOD

AIM

To determine the particle size weight distribution of given sample (granules or

powder) by sievingmethod and to determine the average particle diameter of the
given sample, dsieve.

REQUIREMENTS

Standard sieves (no. 8,12,22,24,44,66,80 mesh sieves, bottom pan and lid), sieveshaker,
balance, granules.

PRINCIPLE

Pharmaceutical powders ideally should contain particles of one size, which is not
possible by any size reduction method. At least, the powder should contain narrow
particle size distribution. Therefore, these materials are controlled to meet official
specifications. For this evaluation sieving method is used. The basic principle involved
in this method is size separation using standard sieves or screens. Size separation is a
unit operation that involves the separation of various sizes of particles into two or more
portions by means of screening surfaces.
Sieving method directly gives weight distribution analysis. From the data, dsieve can
be calculated. Sieve diameter is defined as the diameter of a sphere that passes
through the sieve aperture as the asymmetric particle. Sieve diameter is applied to
those particles that pass through a sieve. It is useful for establishing size distribution
analysis. On the other hand, powder is expressed by average particle diameter.
The powder drug is separated according to its particle size using a number of sieves in
a nest. These are subjected to different types of agitation in sieve shaker, so that size
separation is rapid. Sieves are arranged in a nest with the coarsest at thetop. A
sample (100 g) of the powder or granules is placed on the top sieve. This sieve set is
fixed to the mechanical gyratory shaker and shaken for a period of time (5 minutes).
The powder retained on each sieve is weighed. Then normal weight distribution curve
is constructed.
KMCT College of
 Laboratory Manual of Pharmaceutical
The average particle diameter of a powder (daverage) is calculated using the following
equation.

KMCT College of
 Laboratory Manual of Pharmaceutical

daverage = Ʃ(n×d)
Ʃn

Where, n- frequency of particles in a particle size range, g or percent weight of

powder undersize, gd- average particle diameter of a particular sieve (sieve
diameter), µm.

PROCEDURE

 Standard sieves set are selected. This set consists of various sizes (8, 12,
22,24, 44, 66, 80 meshsieves)
 Arrange them in such a manner that the coarsest remains at the top and
finestat the bottom. Keep the pan below the sieve set.
 Weigh 100 g of the sample.
 Place the sample on the coarsest sieve and the lid was placed.
 Fix the above sieve set on a mechanical shaker and clamp it tightly.
 The mechanical shaker was switched on and set the time for 10 minutes.
 When the shaker stops, collect the sample retained on each sieve into
apaper.
 Weigh all the samples.
 Report the weights retained on each sieve in the table against the
corresponding sievenumber.
Analyze the data for normal, log normal, cumulative frequency and probability graphs.
REPORT

Normal and log normal distribution curve

was plotted. Average diameter of powder = .

REFERENCES

Laboratory manual of pharmaceutical engineering; C.V.S Subrahmanyam, J. Thimma

Setty, V. Kusumdevi, Sarasija Suresh; page no. 27-34.
Laboratory manual of physical pharmaceutics by C.V.S Subrahmanyam; page no.102-
KMCT College of
 Laboratory Manual of Pharmaceutical
107.

KMCT College of
 Laboratory Manual of Pharmaceutical

Experiment No:10 Date:

PARTICLE SIZE DETERMINATION BY BEAKER DECANTATION METHOD

AIM
To determine the particle size distribution of a material by sedimentation and decantation.

REQUIREMENTS

Magnesium carbonate, liquor ammonia, measuring cylinder, glass rod, filter paper
PRINCIPLE
Stoke’s derived a relationship for resistance offered to the motion of a sphere through a
fluid under various condition. The entire resistance is caused by the internal friction of
the fluid of definite height ‘h’, density ‘ρl’ and viscosity ‘η’
vt = h/t

therefore, t= h/ vt

This experiment is based on the theory that within a definite time, particle of size range
about 40µm diameter would have settled and after further time interval particle of size
range between 20µm and 40µm would settle. Those particle which have not settled are
assumed to be less than 20µm diameter. Thus, size distribution of a given sample of
powder can be determined.

PROCEDURE
1. Weigh about 10 g CaCo3 accurately and made to
slurry with water [Link] beaker as “A” and
made to height h=(12.5cm)
2. Added a drop of liquid ammonia
3. Stirred the slurry and allow to settle for exactly 96 sec (By this time all
solid

KMCT College of
 4. particles greater than 40 micron will settled)
5. Tapped the sides of beaker gently till 96 sec. so that settled
mass becomecompact and the particle of the side wall of the
beaker also settle down.
6. Transfer the supernatant liquid into second beaker named
“B”(liquid containparticle size less than 40 microns)
7. Then made up beaker A again to same height ‘h’(h=12.5 cm)
8. Stirred well and allow to settle the same for a period of 96s
9. Transfer the supernatant liquid from A to 3rd beaker C
10. Particle remaining in A will be of size greater than 40 microns
11. Filtered this, dried and find out the weight in %.
12. Made up the beaker B up to ‘h’ (h=12.5cm).stirred it and allowed to
settle for a period of 380s (which will help particle greater than
20micron to settle) Here inthis beaker ‘B’ contain particle size less
than 40 microns. Therefore in beaker ‘B’ particle between 20-40
micron.
13. Transfer supernatant liquid from beaker ‘B’ to beaker ‘D’(Beaker ‘D’
should be large)
14. Once again makeup beaker B to same height (h=12.5cm) and stir
well keep tosame period of 380sec and repeat this.
15. Adopt same procedure for beaker B and C now beaker B and
C contain particlesize between 20 and 40 microns.
16. Filter this and weigh after dried and expressed in %.
17. Beaker D contain particle of size less than 20 micron. Filter it
and find outweight of particle after drying express in %.

REPORT

Size (µm) Percentage weight of sample

> 40µm
20 -
40µm
<20µm

REFERENCE:
Tutorial pharmacy by Coopper and Gunn’s, page no: 260
30
Experiment No:11 Date:

SIZE REDUCTION
AIM:
To verify the laws of size reduction using ball mill and determining Kicks,
Rittinger’s,Bond’s coefficients, power requirement and critical speed of Ball Mill.
MATERIALS REQUIRED:

Ball mill, sieve set

PRINCIPLE:

Ball mill is one of the most important equipment used in the process of size
reduction. Ball mill works on the principle of impact between rapidly moving
balls and feed bath enclosed in a hollow cylinder. At low speed the balls roll
over each other and attrition will be predominant. So impact and attrition is
responsible for size reduction.
The ball mill consists of a hollow cylinder which is mounted on a metallic
frame which can be rotated on its longitudinal axis. The cylinder contains balls
that occupy 30- 50% of the mill volume. The weight of the ball is kept constant.
Larger balls give coarse product as compared to small balls. Generally
combinations of large and small balls are used. Balls used are made up of steel
or iron and its size depends upon the size of the feedand mill diameter. Smaller
balls are more preferable for effective size reduction. Size reduction of brittle,
hardened, obstructive materials can be carried out by using ball mill. Soft
fibrous and sticky materials cannot be ground by using ball mill. By using ball
mill we can obtain particle of 20-200 mesh size. The rotational frequency will
depend on the diameter of mill but usually of order 0.5 sec-1.
The drug to be ground is put into the cylinder of the mill in such a quantity that
it is filled to about 60% of the volume. A fixed number of balls are introduced
and cylinder is closed. The mill is allowed to rotate. The speed of rotation is
very important. At low speed, the balls roll over each other. The use of small
balls is recommended so thatsurface is greatest.

At correct speed (critical speed), the centrifugal force just occurs, as the
result the balls are packed up by the mill wall and carried out to the top where
they break contact with the wall end and fall to the bottom. The balls are rolled
by centrifugal and gravitational force. In this manner impact stress will also be
induced and the size reduction is made effective. At critical speed centrifugal
31
force equal to the gravitational force.
At higher speed, the balls are thrown out to be wall by centrifugal force. Hence
grinding will not occur. The compression by the ball against the wall will not
be sufficientfor effective

32
 comminution of the substance.
PROCEDURE:

1. Clean the sieve and ball mill.

2. Weigh about 1000g of substances to be required to be pass through sieve
no:44 and calculate the percentage of fine at zero time.
3. Introduce the feed into ball mill, operated the mill for 5 minute and
determine the percentage of fine.
4. Repeat the above step for 10, 15, 20 and 30 minute till the percentage
fine remains constant.
5. Tabulate the result and plot a graph by taking time of operation of ball mill
on Y-axis percentage of fine on X-axis.

REPORT: -

The size reduction ratio was found to

be

REFERENCE:
Laboratory manual of Pharmaceutical engineering C V S Subrahmanyan, J Thimma setty
firstedition 2006 page no:35-42.

33
EQUIPMENT

34
Experiment No:12 Date:

DESCRIPTION OF CONSTRUCTION, WORKING AND

APPLICATION OF PHARMACEUTICAL MACHINERY SUCH AS
ROTARY TABLET MACHINE, FLUIDIZED BED COATER, FLUID
ENERGY MILL, DE –HUMIDIFIER
AIM:
To Describe the Construction, Working and application of pharmaceutical machinery
such as Rotary Tablet Machine, Fluidized Bed Coater, Fluid Energy Mill, Dehumidifier.

1. ROTARY TABLET MACHINE:

It is also called multi station tablet press. It is called rotary machine rotary machine
because the head of the machine that holds the upper punches, dies and lower
punches in place rotates.
Steps involved in manufacturing of tablet:

 The material to fed through hopper

 The fill cam pulls the lower punches down to a fixed distance and
the dies are filled with material
 The quantity of the material filled is larger than the actual amount
required, remove excess amount with the help of spatula
 After that, upper punch is lowered and inserted into the dies
 The material is compressed and the tablet are formed
 After the compression, pulls the upper punches into their top
position and simultaneously lift the lower punches until the tablets
are ejected from the dies
 Then the tablet is passed through discharge chute
Applications:
 It is operated continuously
 Used for large scale production
 A single rotary press produce 1150 tablets in a minute while double
35
rotarypress can produce 10,000 tablets in a minute

36
 2. FLUIDIZED BED COATER:
Three types of air suspension coater are available, namely top spray coater, wurster
or bottom spray coater, and tangential spray coater. In top spray coater, there is a
counter current (opposite position) it movement of powder particles or pellets and
liquid spray. In wurster or bottom spray coater, there is a concurrent (same direction)
movement of powder particles or pellets and liquid spray. In tangential spray coater,
the powder particles or pellets move in a helical fashion due to spinning rotor disk
on the bottom of the equipment.

Steps involved in wurster or bottom spray coater:

 The drying inlet air is passed upwards through the bottom
perforated plate into the fluid bed chamber
 This air passes to wurster column, in which a spray gun
perpendicularto bottom plate and parallel to the wurster
column
 This air passes out from the exhaust filters situated at the
top of the equipment
 The material to be coated is located is loaded in the fluid bed
chamber and fluidized
37
 The inlet air cause fluidization of the material as well as its
drying during the coating operation

38
  The pellets are pass through the liquid spray of coating solution
from the spray gun positioned parallel to the column
 After coating the coated particle falls by gravity at the bottom of
wurster column and recycled to coating zone.
Application:

 It is used to coat pharmaceutical dosage form with polymeric

material to mark objectionable taste or odour and also to protect
an unstable ingredient and to improve appearance
 Fluidized bed coaters are used for coating of powders, granules,
tablets, pellets etc by column of air
 Fluidized bed coating equipment is popular for coating
multiparticulate systems such as beads and non parallel seeds

3. FLUID ENERGY MILL:

 A fluid usually air is injected at very high pressure through
nozzles at the bottom of the loop, as a result turbulence is
39
produced

40
  Solids are introduced into the steam through hopper
 Due to this turbulence occur and impacts and attrition
occurbetween the particles
 A classifier is fitted at the exist so that only finer size
particles are collected as products
 The larger size particles are again sent to the stream
of air for further size reduction
Application:
 The particle size of the product is smaller when compared to
othermethod of size reduction
 No chance of contamination of the product
 This material is suitable where fine powders are required
like micro ionization or griseofulvin

4. DE-HUMIDIFIER:

 Warm moist air is sucked in through one side of the machine

 An electric fan is used to draws the air inward

 The warm air passes through cold pipes through which a

coolant circulators, due to cooling of air, the moisture it
contains turns back into
41
 liquid water
 Then the air passes over a heating element and warms back
up to its original temperature
 Warm, dry air blows back into the room through another side of
machine
 The moisture that was in the air drips down into a collecting
tray at the bottom of the machine
 As the collecting tray fills up, a plastic float in the machine rises upward
 When the tray is fill, the float trips an electric switch that turns
off the fan and switches on an indicator light which indicates
that the machineneeds emptying
Applications:

 A dehumidifier is used to reduce the levels of humidity in the air

 Large dehumidifier are used in commercial buildings such as indoor ice rinksto
control the humidity level

42
Experiment No:12 Date:

DEMONSTRATION OF COLLOID MILL, PLANETARY MIXER, FLUIDIZED

BED DRYER, FREEZE DRYER

AIM:

To Demonstrate Colloid Mill, Planetary Mixer, Fluidized Bed Dryer, Freeze Dryer.

1. COLLOID MILL
Colloid mill consists of two steel discs having very small clearance between them.
One disc is rotating, while the other one is stationary. When the material is passed
through these discs, they get sheared.

Construction:

It consists of high speed rotor and stator with conical milling surface. The milling
surface may be smooth or rough. Rough surfaced mills are used for fibrous
materials because fibres tend to interlock and clog smooth surfaced mills. The
clearance between rotor and stator can be adjusted from 0.05-0.75mm.
Duringmilling the heat generated may rise the temperature upto 40ºC. Hence,
cold water circulation is provided to reduce the temperature. The discharge pipe
is also connected to hoper, so that discharge can be recycled.

Working:

The colloid mill used to reduce the size of the suspended droplets
The material is fed in through the inlet hopper and placed into the mill.
It is then moved through the narrow gap between the rotor and stator
toreduce the particlesize.
Then final product is removed through the outlet.

Applications:

It is used for preparing colloidal dispersions, suspensions,emulsions and

ointments. Particle size as small as 3µm can be obtained.
Fibrous material milled using rough surfaced rotor and stator.

43
REFERENCES

Pharmaceutical engineering, Unit operations – II by C.V.S Subrahmanyam, [Link]

Setty, [Link], Sarasija Suresh; Page no: 17-18.
Pharmaceutical engineering by Shalini Sharma; Page no: 224.

2. BALL MILL

Ball mill is also known as tumbling mill. Ball mill works on the principle of impact and
attrition. Impactoccurs between the rapidly moving balls and the powder material that
is enclosed in a hollow [Link] low speeds, balls roll over each other and attrition
will be the predominant mode of action. It is the speed of rotation that determines
the mode of action.

Construction:
It consists of a hollow cylinder, which is mounted on a metallic frame in such a way
that it can be rotated on its longitudinal axis. The length of the cylinder is slightly
greater than its diameter. It is madeof a metal and usually lined with chrome.
The cylinder occupies 30- 50 % of mill volume. The ball size depends on the size of
feed and the diameter of the mill. They are made of steel, iron or stoneware. These
act as the grinding medium. Working:
 The drug to be ground is placed in the cylinder such that it occupies only
60% of the volume.
 A fixed amount of balls is placed and the cylinder is closed.
 The mill is allowed to rotate in its optimal speed.
 The ground material is then collected.

Applications:
 Fine grinding is obtained for hard and abrasive materials.
 Stainless steel balls preferred in the production of ophthalmic and parenteral products.
 It can be also used for milling dyes, pigments and insecticides.

REFERENCES
44
Pharmaceutical engineering, Unit operations – II by C.V.S Subrahmanyam, J. Thimma Setty,
V.

45
Kusumdevi, Sarasija Suresh; Page no: 12-14.
3. PLANETARY MIXER

In a planetary mixer, the blade tears the mass apart and shear is applied between a
moving blade and a stationary wall. The mixing arm moves in two ways, around
itsown axis and around the central axis, so that it reaches every spot of the vessel.
The plates in the blade are sloped so that the powder makes an upward movement.
Therefore tumbling motion is also obtained.

Construction:
It consists of a vertical cylindrical shell, which can be removed either by loweringit
beneath the blade or raising the blade above the bowl. The mixing blade is mounted
from top of the bowl. The mixing shaft is driven by a planetary gear train. It rotates
around the ring gear, which further rotates around the mixer blade.

Working:
 The material to be mixed is loaded into mixing bowl or shell.
 The blades rotate on their own axis when they orbit the mixing
bowl on a common [Link], there is no dead spot in the
mixing and high shear is applied for mixing.
 After mixing, the material is discharged through a bottom valve, or by
manual scooping of thematerial from the bowl.

Applications:
 It produces precise blends in addition to breaking down of agglomeratesrapidly.
 Low speeds are used for dry blending.
 Faster speeds are used for the kneading action required in wet granulation.
 Steam jacketed bowls are used in the manufacture of sustained
releaseproducts and ointments.

REFERENCES

Pharmaceutical engineering, Unit operations – II by C.V.S Subrahmanyam, [Link] Setty,

V. Kusumdevi, Sarasija Suresh; Page no: 91-92.
Pharmaceutical engineering by Shalini Sharma; Page no: 224.

46
 4. FLUIDIZED BED DRYER

In fluidized bed dryer, hot air (gas) is passed at high pressure through a perforated
bottom of the containercontaining granules to be dried. The granules are lifted from
the bottom and suspended in the stream of air. This condition is called fluidized state.
The hot gas surrounds every granule to completely dry them.

Construction:

Two types of bed dryers are available, vertical fluid bed dryer and horizontal fluid bed dryer.

The construction of vertical fluidized bed dryer is shown in the figure. It is madeup
of stainless steel or plastic. A detachable bowl is placed at the bottom of the dryer,
which is used for charging and discharging. The bowl has a perforated bottom with a
wire mesh support for placing materials to be dried.A fan is mounted in the upper
part for circulating hot air. Fresh air inlet, prefilter and heat exchanger are
connected serially to heat the air to the required temperatures. Bag filters are
placed above the drying bowl for the recovery of fines.

Working:

 The wet granules to be dried are placed in a detachable bowl which is inserted in the
dryer.
 Fresh air can pass through a pre-filter, which is then heated when passing
through a heat exchanger.
 Hot air flows through the bottom of the bowl. At the same time, the fan
starts to rotate. The air speed increases gradually.
 After a specific time, a pressure point is reached in which the friction drag on
the particles is equal to the force of gravity. The granules rise in the container.
This condition is said to be fluidized state.
 The gas surrounds each granule to dry them completely. The air comes out
of the dryer passing through the filters in the bag.
 The entrained particles remain adhered to the interior surface
of the [Link], thebags are shaken to remove the
entrained particles.
 The materials are left in the dryer to reach roomtemperature.
 The bowl is removed for unloading. The final product is free flowing.

47
Applications:

48
  It is used for drying of granules in the production of tablets.
 It can be used for three operations – mixing, granulation and
drying. It can also bemodified for coating of granules.

REFERENCES

Pharmaceutical engineering, Unit operations – II by C.V.S Subrahmanyam, [Link]

Setty, V. Kusumdevi, Sarasija Suresh; Page no: 303-305.
Pharmaceutical engineering by Shalini Sharma; Page no: 22

5. FREEZE DRYER

In freeze drying, water is removed from the frozen state by sublimation, i.e. direct
change of water from solid into vapour without conversion into a liquid phase. Solid-
liquid-vapour equilibrium phase diagram of water is useful to decide the experimental
conditions. The drying is achieved by subjecting the materialto temperature and
pressures below the triple point. Under these conditions, any heat transferred is used
as latent heat and ice sublimes directly into vapour state. The water vapour is removed
from the system by condensation in a cold trap maintained at a temperature lower than
the frozen material.

Construction:

It consists of :

 Drying chamber in which trays are loaded.

 Heat supply in the form of radiation source, heating coils.
 Vapour condensing or adsorption system
 Vacuum pump or steam ejector or both.

Working:

 The material is pretreated before freezing. Pretreatment methods include

freezing concentration, solution phase concentration, formulation to
preservethe appearance of the product, formulation to stabilize reactive
products, formulation to increase the surface area and decreasing high vapor
49
 pressure solvent.
 The product should be frozen at a temperature low enough to solidify completely.
The

50
 products are frozen in two ways, most of the products that are lyophilized
consist mainly of water. It is very important in lyophilization to pre-freeze the
product below the eutectic temperature before beginningthe lyophilization
process.
 After prefreezing the product, conditions must be established in which the ice
can be removed from the frozen product through sublimation, resultingin a dry,
structurally intact product.
 After primary freeze drying is complete, and all ice has sublimed, bound
moisture is still present in the product. The product appears dry, but the
residual moisture content may be as high as 7- 8%. Continued drying is
necessary at warmer temperature to reduce the residual moisture content to
optimum values. This process is called isothermal desorption. Secondary
drying is usually carried out for approximately 1/3 or ½ the time required
forprimary drying.
 After vacuum is replaced by inert gas, bottle and vials are closed.

Applications:
 It is used in the production of dosage forms such as injections, solutions
andsuspensions.
 It is also used for drying a number of products :
 Blood plasma and its fractionated products.
 Bacterial and viral cultures.
 Human tissue.
 Antibiotics and plant extracts.
 Steroids, vitamins and enzymes.

REFERENCES

Pharmaceutical engineering, Unit operations – I by C.V.S Subrahmanyam, [Link] Setty,

V. Kusumdevi, Sarasija Suresh; Page no: 307-310.
Pharmaceutical engineering by Shalini Sharma; Page no: 225-226.

51
52
 Laboratory manual of Pharmaceutical Engineering

KMCT College of