BP308P

M. S. Ramaiah University of Applied Sciences

Private University Established in Karnataka State by Act No. 15 of 2013

Laboratory Manual

Faculty Faculty of Pharmacy (FPH)

Programme B.Pharm
Course Bachelor of Pharmacy
Year/Semester 3rd Semester
Name of the Laboratory Pharmaceutical Engineering
Laboratory Code BP 308

Name: Ms/Mr/

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LIST OF EXPERIMENTS

Sl.No. Experiments
1 Factors affecting Rate of Evaporation
(Surface area, Concentration and Thickness/ viscosity)
2 Factors affecting Rate of Filtration
(Surface area, Concentration and Thickness/ viscosity)
3 Determination of radiation constant of brass, iron, unpainted and
painted glass.
4 To determine the overall heat transfer coefficient by heat exchanger
5 Size reduction: 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.
6 Size analysis by sieving – To evaluate size distribution of tablet
granulations – Construction of various size frequency curves
including arithmetic and logarithmic probability plots
7 Construction of drying curves (for calcium carbonate and starch).
8 Determination of moisture content and loss on drying.
9 Determination of humidity of air – i) From wet and dry bulb
temperatures – use of Dew point method
10 Description of Construction working and application of Pharmaceutical
Machinery such as rotary tablet machine, fluidized bed coater, fluid
energy mill, de humidifier
11 Demonstration of colloid mill, planetary mixer, fluidized bed dryer,
freeze dryer and such other major equipment

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REGULAR PRACTICAL ASSESSMENT SCHEME

Sl. no. Parameters Marks allotted

01 Maintenance of practical manual book 01

02 Record book neatness and timely 02

submission
03 Product evaluation 01

04 Product presentation (Container and 02

Label)
05 Viva voce 02

06 Attendance, discipline and involvement 02

Total 10

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INDEX

Date Date /
Sl.No Name of the Experiment Grade/
& Teacher’s
Marks
Pg. No Signature
Evaporation
Factors affecting Rate of Evaporation
1
(Surface area, Concentration and
Thickness/ viscosity)
Filtration
Factors affecting Rate of Filtration
2
(Surface area, Concentration and
Thickness/ viscosity)
Heat transfer
Determination of radiation constant of
3
brass, iron, unpainted and painted glass
Determination of overall heat transfer
4
coefficient by heat exchanger
Size reduction
Size reduction: To verify the laws of size
5
reduction using ball mill and
determining Kicks, Rittinger‘s, Bond‘s
coefficients, power requirement and
critical speed of Ball Mill.
Size Separation
Size analysis by sieving – To evaluate size
6
distribution of tablet granulations –
Construction of various size frequency
curves including arithmetic and
logarithmic probability plots
Drying
Construction of drying curves
7
(for calcium carbonate and starch)

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Date Date /
Sl.No Name of the Experiment Grade/
& Teacher’s
Marks
Pg. No Signature
Determination of moisture content and
8
loss on drying

Humidity
Determination of humidity of air –
9
i) From wet and dry bulb temperatures –
use of Dew point method
Engineering equipments
Description of Construction working and
10
application of Pharmaceutical
Machinery such as rotary tablet
machine, fluidized bed coater, fluid
energy mill, de humidifier
Demonstration of colloid mill, planetary
11
mixer, fluidized bed dryer, freeze dryer
and such other major equipment

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RECORD WRITING

The details to be written in the left The details to be written in the right
hand side of the record hand side of the record

1) Observations 1) Name of the Preparation

2) Calculations 2) Aim
3) Tables 3) Principle
4) Graphs 6) Procedure
7) Report

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REQUIREMENTS FOR PRACTICALS

1 Practical Manual
2 Clean Apron
3 White Mask and Cap
4 Record
5 Ball pens- Red, Blue, Black and Green pens
6 Scissors
7 Glue
8 Butter paper
9 Spatula
10 Rubber sheet
11 Wiping cloth
12 Calculator

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Experiment No: 1 Date: / /2018

Title: Factors affecting Rate of Evaporation

1. Aim and Objectives

• To study the factors affecting the rate of evaporation

• The student will be able to observe, record and report the influence of factors on rate of
evaporation

2. Introduction to the Experiment

Evaporation Theory, Applications, Principle

3. Requirements

Beakers, weight box, water bath, specific gravity bottle, viscometer, dryer.

4. Procedure:
A. Effect of surface area on the rate of evaporation

1) Determine the surface area of three different beakers

2) 25ml of purified water was taken into the beaker and weighed (W1 g). The beaker was
then placed over a constant heat source for 10 mins to enable evaporation.
3) The beaker was then taken out, cooled and weighed (W2 g). The differences between the
initial and final weight was noted.
4) The rate of evaporation was calculated using the following formula:

Quantity of water evaporated (g)

Rate of evaporation =
Time of heating (min)

5) A graph was plotted with surface area on the x axis and rate of evaporation on the y axis.

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B. Effect of viscosity on the rate of evaporation

1) Different concentrations of Glycerin–water mixtures (5 %, 10 % & 20 % w/v) were

prepared and their viscosities were determined using Ostwald’s viscometer.
2) 25ml of the sample solution was taken into a 100ml beaker and weighed (W1 g). The
beaker was then placed over a constant heat source for 10 mins to enable evaporation.
3) The beaker was then taken out, cooled and weighed (W2 g). The differences between the
initial and final weight was noted.
4) The rate of evaporation was calculated. A graph was plotted with viscosity on the X axis
and rate of evaporation on the Y axis.

C. Effect of concentration of solute in solution on the rate of evaporation

1) Different concentrations of Sodium chloride solutions (5 %, 10 % & 20 % w/v) were

prepared.
2) 25ml of the sample solution was taken into a 100 ml beaker and weighed (W1 g). The
beaker was then placed over a constant heat source for 10 mins to enable evaporation.
3) The beaker was then taken out, cooled and weighed (W2 g). The differences between the
initial and final weight was noted.
4) The rate of evaporation was calculated. A graph was plotted with concentration of
solute on the X axis and rate of evaporation on the Y axis.

5. Presentation of Results
Tables and graph

6. Report

The effect of three factors were on rate of evaporation was determined and found to be :

a. With an increase in surface area the rate of evaporation ---------------

b. With an increase in viscosity the rate of evaporation ---------------

c. With an increase in solute concentration the rate of evaporation ---------------

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Observations

Effect of surface area on the rate of evaporation

Sample Diameter Radius Surface Initial Final Weight Time of ROE

& (cm) D/2 area weight weight loss heating W/t
Beaker cm (πr2) of of (t) in (g/min)
capacity beaker beaker W= W1-W2 min
+ + (g)
water water
(W1 g) (W2 g)
Distilled
water
(50 ml)
Distilled
Water 10
(100 ml)
Distilled
water
(250 ml)

Effect of concentration of solute on the rate of evaporation

Initial Final
Sample weight of weight of Weight loss Time of heating ROE
beaker beaker (t) W/t
( NaCl + + W= W1-W2 in min (g/min)
solution ) water water (g)
(W1 g) (W2 g)

Distilled
water
(50 ml)

Distilled
Water
10
(100 ml)

Distilled
water
(250 ml)

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Effect of viscosity on the rate of evaporation

Sample Viscosity Initial Final Weight loss Time of ROE

of the weight of weight of heating W/t
( glycerine : sample beaker beaker W= W1-W2 (t) (g/min)
water ) (cps) + + (g) in min
water water
(W1) g (W2) g
10 % 1.2823

1.484 10
15 %
1.8765
20 %

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Experiment No: 2 Date: / /2018

TITLE: Determine the factors affecting the rate of filtration

1. Aim and Objectives

• To determine the factors affecting the rate of filtration

• The student will be able to record and represent the various factors affecting the rate of
filtration

2. Introduction to the Experiment

Filtration theory, Factors affecting filtration, applications

3. Requirements

Beakers, funnels, stop clock, filter paper, tripod stand

4. Procedure

A. Effect of surface area on the rate of filtration

1. Determine the surface area of three funnels.

2. 50 ml of the sample solution was passed through the funnel with filter paper as the filter
medium.

3. The time taken for the volume 10, 20, 30, 40, 50 ml to get collected was noted.
4. The rate of filtration was calculated and represented graphically by plotting surface area
(X axis) versus rate of filtration (Y axis).

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B. Effect of viscosity on the rate of filtration

1. The viscosity of sample solution was determined using Ostwald’s viscometer.

2. The given sample solutions were passed individually through the filter medium.
3. The time taken for 50 ml of the filtrate to be filtered was noted. The rate of filtration was
calculated and represented graphically by plotting viscosity (X axis) versus rate of filtration
(Y axis).
C. Effect of pressure difference across the filter medium.

1. Filter paper of accurate size was placed over a Buchner funnel and the area calculated.
2. 50ml of the sample solution was passed through the filter medium and the time taken for
filtration at normal atmospheric pressure was calculated.
3. The same step was repeated by connecting the Buchner funnel to a vacuum pump and
applying negative pressure.

D. Effect of thickness of filter medium:

1. Filter paper of accurate size in different numbers were placed over a Buchner funnel
2. 50 ml of the sample solution was passed through the filter medium and the time taken for
filtration at normal atmospheric pressure was calculated.
3. The time taken for 50 ml of the filtrate to be filtered was noted
4. The rate of filtration was calculated and represented graphically by plotting thickness of
filter medium (X axis) versus rate of filtration (Y axis).

5. Report

1. With an increase in surface area, rate of filtration _______________.

2. With an increase in viscosity, rate of filtration __________________.
3. With an increase in the pressure difference across the filter medium, rate of filtration
_____________.

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Observations

Effect of surface area on the rate of filtration:

Area of the filter medium Time taken (Sec) Rate of
filtration
Diameter(D) Radius S.A of 10ml 20ml 30ml 40ml 50ml (ml/Sec)
in cm Funnel
Sample funnels (=D/2) in
(πr2)in cm
cm

1. (Small)

2. (Medium)

3. (Big)

Effect of viscosity on the rate of filtration:

Sample (Glycerine Viscosity of sample Time taken for Rate of filtration Permeability co-
in water mixture) (mill poise) filtration(Sec) (ml/Sec) efficient (K)

1. 5% 0.688

2. 10% 1.283

3. 15% 1.432

Effect of thickness of filter medium:

Thickness of the filter Volume of the sample Time taken for filtration Rate of filtration
medium in Sec (ml/Sec)

One Filter paper

Two Filter paper
Three Filter paper
Four Filter paper

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Effect of pressure difference across the filter medium:

Sample Volume of Normal atmospheric pressure Negative pressure

sample
Time taken fir Rate of Time taken for Rate of
filtration (Sec) filtration filtration filtration
(ml/Sec)
(ml/Sec) (Sec)

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Experiment No: 3 Date: / /2018

Title: Determination of radiation constant of brass, iron, unpainted and painted

glass

Aim: To determine the radiation constant of the given metal (iron, copper, brass, or aluminum) cylinder at
80°C and 240°C.

Discussion: 1. Heat transfer with modes of heat transfer

2. Thermal Radiation

3. Stefan Boltzmann Law with equations

Procedure
1. A metal (iron) cylinder is cleaned and weighed (w g) thrice. The average weight is noted in the
table 1-1.
2. The diameter and height of the cylinder are measured thrice. The average values are calculated.
The radius of the cylinder is calculated. The surface area of the cylinder is calculated and recorded
in table 1-1.
3. The metal cylinder is heated using a Bunsen burner.
4. After reaching a constant maximum temperature, the hot body (metal cylinder) is transferred to
the glass tripod stand using long tongs.
5. The thermometer (360°C) is placed in the central hole of the cylinder and fixed to a stand using a
thread.
6. Slowly the temperature of the hot body decreases. The decrease in temperature is noted every 5
minute interval. The data are recorded in table 1-2.
7. A graph is plotted taking time (mins) on X- axis and temperature (°C) on Y-axis. Normally, a curve is
observed.
8. Depending on the temperature at which the radiation constant is to determined, a tangent is
drawn at that temperature. The slope of the tangent is calculated, which represents the rate of
loss of heat (dq/dt) by the hot body.
9. Radiation constant (α) is determined at that temperature.

The same procedure is repeated with cylinders made by different metals.

Precautions:
1. The metal cylinder should not be touched with hands.
2. Care should be taken while transferring the hot metal cylinder from the metal tripod to the glass
tripod.

Observation and Calculations

At room temperature: Wet bulb temperature= ----------°C---------K

Dry bulb temperature=------------°C---------K
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Parameters of the Metal Cylinder

SL.No. Parameter of Trial Average in Average in
the metal cgs system SI system
1 2 3
cylinder

1 Weight, w g

2 Diameter, d cm

3 Radius, r cm -------- --------- ---------

4 Height, h cm

5 Surface area, A -------- -------- --------

Heat loss by convection, β= 0

Specific heat of metals
Iron, s =106 J/Kg.K
Copper, s= 385J/Kg.K
Brass, s =370 J/Kg.K
Aluminum, s = 913 J/Kg.K
Radiation Constant of a Metal ----Time vs. Temperature plot Data

Time(min) Temp(°C) Time(min) Temp(°C) Time(min) Temp(°C) Time(min) Temp(°C)

Report
Radiation constant of metal. α =
(iron / copper/ brass/ aluminum)

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Experiment No: 4 Date: / /2018

Title: Determination of overall heat transfer coefficient of a heat exchanger

Aim: To determine the overall heat transfer coefficient of a heat exchanger (glass cylinder/
insulated glass cylinder).
Discussion: Heat transfer by convection, Applications, Principle

Procedure
1. The length and diameter of the plain water condenser is determined and reported in the
observations. Based on these values, surface area of the condenser is estimated.

2. Using the plain water condenser, the distillation apparatus is assembled

3. The inlet of water condenser is connected to the tap. The outlet of the condenser is placed in the
beaker (2 liter beaker).

4. The temperature of the water at the inlet of the condenser is noted. This will be same as the
temperature of the tap water. The temperature is reported in table 3-1

5. The steam generator is heated so that steam will be generated. After some time, the
thermometer shows constant temperature. The temperature id noted (Table 3-1) and experiment
is started from the point. The steam passes through the water condenser and gets condensed in
the condenser due to circulation of water in the jacket.

6. The condensate gets collected in to the beaker(50 ml)

7. Allow the experiment for 2 minutes (after attaining constant temperature of the steam)

8. The quantity of condensate water is collected and its temperature is noted.

9. The quantity of circulated water is collected at the outlet of the condenser and its temperature is
noted.

Precautions:

1. The rate of flow of water through the jacket of the water condenser must be maintained
constant.
2. The joints in the assembly of apparatus must be as short as possible, so as to prevent the heat
loss at these points.
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Observations and Calculations

Observation with plain water condenser

Diameter of the condenser, d=---------cm=---------------------m

Radius of the condenser, r=-------------cm=--------------m

Length of the condenser, l=-------------cm=---------------m

Area of the condenser, A= 2πrl

Parameters for counter current flow

Water condenser circulating water On steam side of the condenser

Tap water Water outlet Steam Condensate

Temperature, °C

Temperature, K

Difference in Δt1 Δt2

temperatures

Average Δt1+Δt1/2
temperature, Δ tav

Volume of water ---- M2 ------ M1

in 2 minutes

Mass of water in 2
minutes, Kg

Mass of water per

second, Kg/s

Report: Overall heat transfer coefficient of plain glass tube (water condenser) =

Overall heat transfer coefficient of insulated glass tube=

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Experiment No: 5 Date: / /2018

TITLE: Size reduction: 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.

Aim: To achieve size reduction of the given granular material using a ball mill.
To calculate Kick’s constant, Rittinger’s constant, and Bond’s work index for the above size reduction
process.

Discussion: Size reduction, Principle, Kick’s law, Rittinger’s law, Bond’s work Index

3. Requirements

Sieves (# 8 and 12), crystal salt, energy meter, metal balls m, sieve shaker, digital
balance

4. Procedure

1. The ball mill was cleaned and loaded with sufficient number of steel balls.

2. The ball mill was operated at an optimum speed without the load for 10 minutes and the
revolutions in the energy meter (N1) was noted.

3. The sample (500 g of crystal salt) whose feed size is -8 to +12 was loaded into the ball mill
and operated at the same speed for 10 minutes and number of revolutions were noted
(N2).

4. The product was unloaded from the equipment and subjected to sieve analysis.

5. The Kick’s law and Rittinger’s law coefficients were calculated.

5. Presentation of Results
Tables and graph

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6. Report

Size reduction was carried out using ball mill for the given sample.

The feed particle size was found to be (D1) = mm

Particle size of the product was found to be (D2) = mm

Kick’s law coefficient = KJ/Kg

Rittinger’s law coefficient = KJ/Kg

Observations
Wt. of the sample taken = g
No. of revolutions without load (N1) =
No. of revolutions with load (N2) =

Calculation of energy meter constant (EC)

For 150 revolutions, the energy consumed = 3600 KJ
There four for 1 revolution, the energy consumed = 24 KJ
Energy consumed by ball mill without load E1 = N1 × EC =
Energy consumed by ball mill with load E2 = N2 × EC =
Net energy consumed per unit mass = E= E2-E1/W =
Determination of size (D1) = nominal aperture size of sieve no.8 + Nominal aperture size of
Sieve no.12

= 2 + 1.4 = 1.7
2

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Determination of particle size after size reduction (D2)

Sieve no. Nominal Sieve no Mean Wt. of powder Wt. size
aperture size range aperture size retained on each
(n × d)
(mm) sieve (n)

(d)

€n= € nd =

Average particle size = € nd = = mm

€n

Kick’s law coefficient (E)

E = Kk log (D1 / D2) = KJ/kg

Kk = E / log (D1 / D2) = KJ/kg

Therefore

Ritingers constant

E = KR [ 1 /D2 – 1 / Da) = KJ/kg

Bond’s Work Index

E = 2KB [ 1 /√ D2 – 1 / √ D1] = KJ/kg

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Experiment No: 6 Date: / /2018

TITLE: Size analysis by sieving – To evaluate size distribution of tablet
granulations – Construction of various size frequency curves including
arithmetic and logarithmic probability plots

Aim:To determine the particle size weight distribution of a given sample (powder or granules) by
sieving method.
To determine average particle diameter of a powder, d sieve-
Discussion : Size Separation, Sieving, Applications, Principle
Procedure:
1. Standard sieves set is selected. This set consists of various sizes (10, 22, 44, 60, 85, 100, and 120
mesh sieves)
2. Sieves are arranged in such a manner that coarsest remains at the top and finest at the bottom.
The pan is kept below the sieves
3. Hundred grams of given sample (granules or powder) is weighed.
4. The sample is placed on the coarsest sieve. The lid is placed.
5. The above sieves set is fixed on mechanical shaker and clamped tightly.
6. The timer is adjusted on the dial for 05 minutes and the mechanical shaker is switched on. (Each
sieve shaker must be standardized for the time of shaking)
7. When the shaker automatically stops, the sample retained on each sieve is collected on in to a
paper.
8. All samples are weighed.
9. The weights retained on each sieve are recorded in the table 5-2 against the corresponding sieve
number.
10. The data is analyzed for normal weight distribution pattern. A plot is drawn by taking mean size of
opening on the X axis and percent weight retained on smaller sieve on Y-axis
11. The average particle size is calculated.

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Observations and Calculations

Weight distribution of sample (Powder or Granules)-Undersize

Sive Nominal Aperture Mean size of Weight Percent weight Weight size
number mesh size(Passed/retai opening, d, of retained on
aperture ned), µm µm powder smaller sieve nxd
size µm undersiz
e, n, g

(1) (2) (3) (4) (5) (6) (7)

pan -------- --------- ------ ** -------- -------

- -

120 125 125/pan 125.0

100 150 150/125 137.5

85 180 180/150 165.0

60 250 250/180 215.0

44 355 355/250 302.5

22 840 840/355 597.5

10 1700 1700/840 1270.0 ***

Report:

Normal weight distribution curve is drawn.

Average particle diameter of the powder =-------------------µm

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Observations

Determination of particle size after size reduction (D2)

Sieve no. Nominal Sieve no Mean Wt. of Wt. size % of Cumulative Cumulative
aperture range aperture powder weight % of
(n×d) % of
size size (mm) retained powder weight
weight
on each retained powder
(d) powder
sieve retained
retained
(n) (oversize)
(undersize)

€n= € nd =

Average particle size = € nd = = mm

€n

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Experiment No: 7 Date: / /2018

TITLE : Construction of drying curves (for calcium carbonate and starch)

Aim: To dry calcium carbonate slurry and plot the rate of drying curve.
Discussion: Drying and its applications, EMC and FMC,Principle
Procedure:
1. The stainless steel plate is weighed and the weight is recorded as w1.
2. 15.0 g of calcium carbonate is transferred in to a beaker. Water (about 30 ml ) is added slowly to
prepare a slurry.
3. The calcium carbonate slurry is transferred into the stainless steel plate.
4. Filing must be done in such a way that 3/4thof the volume of the stainless steel plate is filled with
slurry.
5. The weight of steel plate plus slurry is taken and recorded as w2.
6. The plate containing slurry is placed in hot air oven, whose temperature must be maintained at
600C.
7. The time is noted soon after placing plate containing slurry in hot air oven.
8. After 15 minutes, the weight of plate with slurry is taken. The weight is recorded in column 3 of
the Table 21-1.
9. Again the steel plate containing slurry is placed back into the dryer. ( Steel plate should be
immediately placed back into the dryer, otherwise temperature decreases enormously and results
will be erroneous ).
10. Steps 8 and 9 are repeated until constant weight is obtained.
11. The rate of drying is calculated.
12. A graph is plotted by taking free moisture content ( weight of water, column 5 ) on x-axis and rate
of drying ( column 9 ) on y-axis.

Observations and Calculations

1. Weight of empty stainless steel plate, w1=__________________g
2. Weight of stainless steel plate + sample slurry, w2 =__________________g
3. Weight of sample slurry, w3 = w2 -w1_________________g
4. 45 g of sample slurry contains 15 g of calcium carbonate w3 g of sample slurry contains ? g of
calcium carbonate
15 x w3= w4 g of calcium carbonate
45
5. Weight of total water content ( TWC ), w5 =( w3 - w4 ) =___________________g
6. Diameter of stainless steel plate, d =______________cm
7. Radius of stainless steel plate, r= (d/2)=_____________cm
8. Area of stainless steel plate, A = πr2=____________cm2
9. Moisture content removed from the sample = w2 - last weight of steel plate taken with sample +
water ( if any)

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TABLE 21-1
Drying Rate of Calcium Carbonate
SI. Drying Weight of Weight of Free Weight of Drying in Rate of Rate of
No. time, steel calcium moisture water the time drying drying
minute plate + carbonat content, remained interval, per per hour
wt. of e + wt. of g (present)/g g/g.min hour, per
calcium water, g ram of dry g/g.h surface
carbonat powder, area
e + wt. of g/g exposed
water, g ,
g/g.h.c
m2

(3) –w1 (4) –w4 (5)/w4 6(n-1)-6(n) (7) x 60 (8)/A

(2)n-(2)n-1

(1) (2) (3) (4) (5) (6) (7) (8) (9)

1. 0

2. 15

3. 30

4. 45

5. 60

6. 75

7. 90

8. 105

9. 120

Report
1. Drying rate curve is plotted by taking FMC on x-axis and rate of drying on y-axis.
2. Total moisture content removed from calcium carbonate slurry ( 30 – 3n ) =___________g

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Experiment No: 8 Date: / /2018

TITLE : Determination of moisture content and loss on drying

Aim: To determine equilibrium moisture content of starch and bentonite at different humidities and at
room temperature.

Discussion: Theory (EMC and its applications),Factors affecting EMC, Principle

Procedure:
Bentonite and starch should be dried at 1000C for one hour ( or until constant weights are obtained before
using them for EMC studies.

1. Six desicators( either glass or plastic ) are taken and labelled.

2. Thirty ml saturated solutions ( with littlke excess crystals ) of potassium acetate, sodium chloride,
and potassium nitrate are prepared in beakers.
3. Saturated solutions are transferred separately into the `well’ of desicators.
4. Weight of each empty bottle (W1 g) is recorded in Table 20-2 and further the data is processed in
the same Table20-2
5. One gram quantities of bentonite are transferred into each of 18 vials.
6. Weights of empty bottle and bentonite is noted (W2 g).
7. Three vials of bentonite are placed in each desicators.
8. Desiactors are closed with lids firmly using wax.
9. Desicators are allowed at room temperature (250C) undisturbed for one week. (Equilibrium
establishes and bentonite absorbs the possible amount of moisture.)
10. After one week, weight of empty bottle and bentonite is noted (W4 g).
11. The data are processed as per the Table 20-2.
12. With the data obtained, a graph is plotted by taking relative humidity ( Column 1 of Table 20-2)
on x-axis and per cent EMC ( Column 8 of Table 20-2) on x-axis.
13. Similarly using starch, steps 5 to 12 are repeated.

Observations and Calculations

(a) Weight of empty bottle =W1 g
(b) Weight of empty bottle + bentonite =W2 g
(c) Weight of bentonite =W3 g
(d) Weight of empty bottle + bentonite after one week of storage =W4 g
(e) Weight of bentoniteafter one week of storage =W5 g
(f) Weight of moisture content absorbed during storage = EMC = (W5-W3)= W6 g
(g) Per cent moisture absorbed = 100 x W6
W3

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Data for the EMC
Humidity, W1 W2 W3 W4 W5 W6 Per cent
% RH EMC

100X W6

W3

23

Average =

33

Average =

52

Average =

64

Average =

75

Average =

93

Average =

Report

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Experiment No: 9 Date: / /2018

TITLE : Determination of humidity of air –
i) From wet and dry bulb temperatures –use of Dew point method

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

Discussion: Theory of humidity, Dew point
Procedure:
1. A round bottom long neck flask (100 ml) is thoroughly cleaned and dried the external surface.
2. Water is filled into the flask upto 2/3rdvolume.
3. The above flask is kept on a glass tripod stand.
4. A thermometer (1100C) is dipped in the water.
5. Crushed ice is slowly added to the water (in the flask) and stirred thoroughly with the help of a
glass rod.
6. As the temperature of water (in the flask) is lowered, mist begins to form on the bottom surface of
the flask. At this point, the temperature is noted. This is the dew point (temperature).
7. 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 are noted. The y coordinate is the humidity.

Observations and Calculations

Trails Dew point, 0C Humidity

Mist appearance Average value

From humidity chart, humidityof standard air dew point =______________kg water/kg dry air

Percent relative humidity = humidity of air x 100

Humidity of saturated air

Report
Humidity of the air =

Per cent relative humidity of air=

Department of Pharmaceutics 30
 BP308P

Experiment No: 10 Date: / /2018

TITLE: Description of Construction working and application of
Pharmaceutical achinery such as rotary tablet machine, fluidized bed
coater, fluid energy mill, de humidifier

Experiment No: 11 Date: / /2018

TITLE:Demonstration of colloid mill, planetary mixer, fluidized bed dryer,
freeze dryer and such other major equipment

Department of Pharmaceutics 31
 BP308P

1. Aim and Objectives

• To determine the mixing index of a mixer for a solid mixture

• The student will be able to fractionate the sample into size ranges and draw the frequency
distribution curve
2. Introduction to the Experiment

Principle: Mixing is the most widely encountered unit operation. It is defined as complete
intermingling of two or more dissimilar portions of materials, so that the final product attains
a level of uniformity. In a completely mixed system, each particles of any one ingredient is as
close as possible to the other ingredient.

When a mixing operation is done, it is important to note when the uniformity of mixing is
obtained. This depends on the type of equipment used for mixing, size of mixer, ratio of the
amount of material to the capacity of the mixer, speed of rotation and the nature of materials
to be mixed.

The precision of determination of end point of the mixing operation depends upon the
method of sampling, the number and location of the sample taken, the precision of the
method used to examine the sample and desire properties of the mixture.

Whether or not particular batch is mixed never an absolute one but is always a relative and it
is determined by degree of uniformity that is desired or that can be determined.

Qualitative terms, such as mixing indices are used to describe the goodness of mixing in a
powder mixture. Criterion for uniformity of mixing can be expressed as a value in term of
variance. Variance is the sum of squares of deviation divided by the number of observations.
This can be expresses as

S2=1/n ∑(X- X )2

S2 = Variance(criterion for uniformity of mixing)

X= Actual composition of component A in a mixture

X=Average composition of compound A in the mixture

N=Number of samples

Department of Pharmaceutics 32
 Mixing index can be used to determine the approximate end point required for a good
mixing to occur in mixing process. Therefore unnecessary mixing for excess time can be
avoided. BP308P
Consider a powder of two components is completely segregated. Then in such a mixture,
variance is maximum. SO2 = p q, where SO2 is variance of completely segregated mixture, p, q
are the proportions of the two components. This is maximum variance.

For a completely randomised mixture of same powder mixture containing ‘N’ number
of particles, the variance is given as

SR2=pq /N = SO2/N

It is the maximum variance that can be obtained for a mixture. SR2 is the
completely randomise mixture.

Once the limiting variances,SO2 and SR2 are calculated, Lacey mixing index (ML), which is
defined as ratio of how much mixing has occurred to how much mixing could have occurred,
can be calculated.

Lacey Mixing index

(ML) = SO2-S2/ SO2- SR2

Where, S2 is the variance in the sample powder mixture. But Lacey Mixing Index is
little insensitive to mixture quality, as for bad mixtures also the index value is high. It ranges
from 0.75 to 1.0.

Pool, Taylor and wall have proposed alternative formula for mixing index, where variance of
segregated mixture is omitted. It is calculated as

Pool Tylor and wall mixing index (M’) = S2/SR2

3. Requirements

Department of Pharmaceutics 33
4. Procedure

1. Prepare 50 ml of 0.1N sodium hydroxide solution and standardise it against 0.1N oxalic acid
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solution using phenolphthalein indicator.

2. Take 5 wide mouthed containers of similar size. Number them 1 to 5. Take 5g of Oxalic acid
and 5g of an inert substance (lactose or dextrose) in each container. (Both the component
should be dry and have approximately same density and particle size.)

3. Tumble the containers 1- 4 for 0, 1, 2 and 3 minutes respectively with a uniform rate of
tumbling. Mix the container-5 vigorously for 10 minutes or more (or triturate in a mortar) such
that completely randomized mixture is obtained.

4. Take at least 3 sample (5-6 samples are preferred) from each container form different loations.
Weigh accurately 1g of material from each sample and dissolve it in water in a volumetric flask
to produce 100ml of solution. (Sample are to be taken from different location where the
mixing is expected to be poor.)

5. Take 10ml of solution from each sample solution and titrate with standardised 0.1N NaOH
solution using phenolphthalein indicator. Note the volume of NaOH consumed.

6. Repeat the same for all samples.

7. Calculate the amount of oxalic acid present in each sample (1g)

(1ml of 0.1 N NaOH =6.3 mg of oxalic acid.)

Amount of oxalic acid present in 1 g of sample =

8. Calculate the variance (S2) for the data collection for each container.

S2 =1/n∑ (X-X)2

Where n= number of observations, X= calculate amount of oxalic acid present and

X= Arithmetic mean of the observed values.

1. Calculate the Lacey’s Mixing Index (ML) and pool Talor and Wall Mixing Index (M’) for
different mixing times.

10. Plot a graph with time of mixing Vs Mixing Index.

Department of Pharmaceutics 34
Procedure :
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A. Preparation of 0.1N NaOH solution:
40g NaOH + 1000ml Dist.Water= 1N NaOH
2g NaOH +500ml Dist.Water =0.1N NaOH

B. Preparation of 0.1 N Oxalic Acid

0.43g Oxalic Acid + 1000ml Dist.Water= 1N Oxalic Acid
0.63g Oxalic Acid +100ml Dist.Water= 0.1N Oxalic Acid

STANDARDIZATION OF 0.1N NaOH

BURETTE: CONICAL FLASK:

INDICATOR: END POINT:

SL.No Initial burette reading Final burette reading Vol.of NaOH

(ml) consumed (ml)
(ml)
1

N1V1=N2V2
N NaOH =

Table: Data for calculation for mixing index

Department of Pharmaceutics 35
Container Sample Time of Vol. of Amount of
mixing NaOH oxalic acid BP308P
no. No. (X-X )2
(min) consumed in 1g of
(ml) sample. S2=1/n ∑(X-X)2
(mg) ‘X’
1

n=3
2 A

n=3
3

Department of Pharmaceutics 36
 C

n=3
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4

n=3
5

n=3

Lacey Mixing index (ML) = So2 - S2 /So2- SR2

Department of Pharmaceutics 37
Lacey Mixing Index for

Container 2 (1 minute mixing )=

Container 3 (2 minute mixing) = BP308P

Container 4 (3 minute mixing) =

(For a completely randomized mixture (M’) = should be close to 1.0(always 1 or less than 1)

Pool, Taylor and Wall Mixing Index for

Container 2 (1 minute mixing) =

Container 3 (2 minute mixing) =

Container 4 (3 minute mixing) =

(For a completely randomized mixture (M’) = should be close to 1.0(always 1 or more than 1)

Experiment No: 6 Date: / /2017

TITLE: Determination of mixing efficiency of a propeller when operated at
Department of different positions (solid –liquid mixing)
Pharmaceutics 38
 BP308P
1. Aim and Objectives

• To determine the mixing efficiency of a propeller at different positions in solid liquid

mixing

• The student will be able to observe the efficiency of mixing of solid and liquid with stirrers at
different positions

2. Introduction to the Experiment

Definition: Mixing is probably the most widely performed unit operation in pharmaceutical
manufacturing mixing involves random distribution of two or more ingredients. The process
of mixing may be involves the mixing the solid, liquids or gases above or in combination.

Mixing can be defined as an operation in which two or more components in a separate or

roughly mixing condition are treated so that every particle of one ingredient lies as near as
possible to the particles of the other ingredient to form a uniform mixture.

Factors affecting mixing:

1. Volume
2. Duration mixing
3. Blending of mixtures
4. Speed
5. Nature of substance
i. Particles size/shape
ii. Particle charge
iii. Nature of surface
iv. Density
6. Proportion of material
7. Proper selection of a mixer

Difference between Turbines and Propellers.

Department of Pharmaceutics 39
SL.No TURBINES PROPELLERS

1. A turbine consists of a circular disc to A propeller normally contains a number of

which a number of short blades are blades. A three bladed design is the most
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attached. common for liquids.

2. The blades may be straight, curved, The marine type propeller is similar to the
pitched or vertical. blade fan or a ceiling fan.

3. The diameter of the turbine ranges from For large tanks the maximum size of 0.5 meters
30-50 percent of the diameter of the propeller is used.
vessel.

4. It rotates at a lower speed 50 to 200 It rotates at a speed of 8000 revolutions per

revolutions per minutes. minutes

5. A flat bladed turbine produced radial and The propeller produces axial (longitudinal)
tangential flow, but as speed increases, movements of liquid.
radial flow dominates. A pitched blade
turbine produced axial flow.

6. Turbines are effective for high viscous Propellers are used when high mixing capacity
solutions with a very wide range of needed. These are effective in handling liquids
viscosity upto 7000 pascal. Seconds. having maximum viscosity of about 2.0 pascals.
Second.
Eg: Syrup, liquid, paraffin, glycerine etc.,
are manufactured using turbines Eg: Multi vitamins elixir, disinfectant solutions
are manufacture using propellers.

3. Requirements

Mixing vessel, propeller, stop clock, digital balance

1. Procedure

1. Sodium chloride crystals were passed through sieve no. 12 and 50 g of the collected
crystals were weighed (or) Sugar was weighed.
2. The weighed sample was then transferred into a mixing vessel containing water.
3. The propeller was placed at the centre with constant speed adjustment.
4. The time taken for complete dissolution of solid was noted.
5. The same process was repeated by introducing the propeller at different positions like
offset, angle and centre with baffles and the time taken for complete dissolution was
noted.

6. The best position is one which takes least time for dissolution.

Department of Pharmaceutics 40
 BP308P

6. Report

The mixing efficiency of propeller was found to be maximum when it was placed in the

position of

Observations

Sl. No Propeller Position Time taken for complete

dissolution
(Sec)

1. Centre

2. Off Set

3. Angle

4. Centre with baffles

Department of Pharmaceutics 41
 BP308P

Department of Pharmaceutics 42
 BP308P

Experiment No: 8 Date: / /2017

TITLE: Determine the effect of concentration of a filter aids on the rate of
filtration of a given sample

1. Aim and Objectives

• To determine the effect of concentration of filter aids on the rate of filtration

• The student will be able to record and represent the various factors affecting the rate of
filtration

2. Introduction to the Experiment

Definition of filtration: filtration may be defined as a process of separation of solids form a

fluid by passing the same through a porous medium that retains the solids, but allows the fluid to
pass through.

Filter aids: are the substance which increases the rate of filtration by reducing the resistance
developed by the filter cake during the process. The object of the filter aid is to prevent the
medium from becoming a blocked and to form an open porous cake, hence, reducing the
resistance to the flow of filtrate.

Examples of filtration aids are: Keiselghur, Talc, Char coal, Paper pulp, Bendonite, Ferrers earth.

Ideal characteristics of filter aids:

1. It should be chemically inert to the liquid being filtered

Department of Pharmaceutics 43
 2. It should have low specific gravity and low density so that filter aid remains suspended in
liquid
3. It should be light, porous and non-compressible so that pours can be formed BP308P
4. It should be free from impurities
5. It should the effective in low concentration
6.

3. Requirements

Beakers, measuring cylinder, funnel, filter paper, different filter aids

4. Procedure

1. The sample solution of 50 ml was mixed with different filter aids of given concentration
separately. (0.1 % W/V or 0.2% W/V or 0.3% W/V or 0.4% W/V or 0.5% W/V).
2. The solution was passed through a funnel containing filter paper as the filter medium.
3. The time taken for the volume 10ml, 20ml, 30ml, 40ml & 50ml of solution to be
filtered was noted and the rate of filtration was determined.
4. The clarity of the final solution was compared with the sample and the results were
represented graphically.

Filter Aids used were:

Talc
Bentonite
Charcoal
Kieselguhr
Kaolin

Department of Pharmaceutics 44
 BP308P

Determination of efficiency of different filter aid on the rate of filtration:

Normal filter paper

Sample Volume of Time taken for filtration

filtration
(ml) A B C D

10

20

30
Iodine solution
40

50

Rate of filtration ml/Sec

Clarity

Report

The rate of filtration & clarity of the given sample solution was compared using
_________ of filter aids like Talc, Bentonite, Charcoal, Kieselguhr & Kaolin. Among all
these filter aids, _____________ was found to be the best.

Department of Pharmaceutics 45
 BP308P

Experiment No: 9 Date: / /2017

TITLE: Determine the efficiency of various filter aids on the rate of
filtration of a given sample

1. Aim and Objectives

• To determine the efficiency of various filter aids on the rate of filtration

• The student will be able to perform and report the influence of various filter aids on the rate
of filtration

2. Introduction to the Experiment

Filter aids: are the substance which increases the rate of filtration by reducing the resistance
developed by the filter cake during the process. The object of the filter aid is to prevent the
medium from becoming a blocked and to form an open porous cake, hence, reducing the
resistance to the flow of filtrate.

Examples of filtration aids are: Keiselghur, Talc, Char coal, Paper pulp, Bendonite, Ferrers earth.

Ideal characteristics of filter aids:

1. It should be chemically inert to the liquid being filtered

2. It should have low specific gravity and low density so that filter aid remains suspended in
liquid

Department of Pharmaceutics 46
 3. It should be light, porous and non-compressible so that pours can be formed
4. It should be free from impurities
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It should the effective in low concentration (0.1 - 0.5 % w/v)

3. Requirements

Beakers, measuring cylinder, funnel, filter paper, different filter aids

5. Procedure

1. The sample solution of 50 ml was mixed with different concentrations of the given filter
aid, separately. (0.25% W/V, 0.50% W/V, 0.75% W/V, 1% W/V).
2. The solution was passed through a funnel containing filter paper as the filter medium.
3. The time taken for the volume 10ml, 20ml, 30ml, 40ml & 50ml of solution to be filtered
was noted and the rate of filtration was determined.
The clarity of the final solution was compared with the sample and the results were
represented graphically
Filter Aids used were:

Talc
Bentonite
Charcoal
Kieselguhr
Kaolin

6. Report
The rate of filtration & clarity of the given sample solution was using _____________as
filter aid at concentrations ________________________________________________
were compared.

___________ was found to be the best concentration as it increased the rate of filtration.

Department of Pharmaceutics 47
 BP308P

Observations

Filter aid used:

Concentration: 0.25, 0.5, 0.75 and 1 % w/v

Sample Volume of Time taken for filtration (Sec)

filtrate (ml)
0.25 % W/V 0.50 % W/V 0.75 % W/V 1 % W/V

10

20

30

Iodine solution 40

50

Rate of filter

Clarity

Department of Pharmaceutics 48
 BP308P

Experiment No: 10 Date: / /2017

TITLE: Measurement of humidity of the sample air using wet bulb - dry
bulb
thermometer

1. Aim and Objectives

• To determine the efficiency of various filter aids on the rate of filtration

• The student will be able to perform and report the influence of various filter aids on the rate
of filtration

2. Introduction to the Experiment

The humidity of air is an important environment’s property in many industrial processes and
a technology as well as it affects a men’s health. There is always some moisture in the air.
Absolute humidity of air (ϕ) refers to water vapour in 1m3 volume of air.

Absolute humidity of air (ϕ) = mp / V……………………………………..1

Where, mp is the mass of water that is contained in the air of volume V. As it follows from
equation (1), the SI unit of absolute humidity is kg/m3. Amount of water vapour contained in the
air is delimited by the point of vapour saturation at each temperature. The humidity reaches its
maximal value ϕmax at this point. Maximal value of humidity as well as vapour pressure that
corresponds to vapour saturation point increases with the temperature. When the temperature of air

Department of Pharmaceutics 49
with maximal value of humidity decreases, excess amount of water vapour condenses (transform
its phase) into liquid water such that air humidity is equal to its maximal value.
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Relative humidity of air (RH) is the ratio of absolute humidity ϕ to its maximal value ϕmax.

RH = ϕmax/ϕ………………………………2

Relative humidity is typically expressed in percent as

% RH = × 100……………………………………….3

Minimal value of relative humidity (0 %) corresponds to the dry air and maximal value
(100%) corresponds to vapour saturated air. Relative humidity of that falls between 50 and 70%
represents most pleasant environment for men.

3. Requirements

Procedure

1. Read the temperature t1 of the dry thermometer.

2. Wet the fabric that covers the bulb of wet thermometer by placing the test-tube with
distilled water into the opening underneath the thermometer for 10 seconds.
3. Spin the string of fan in top part of psychrometer such that it will rotate during the entire
measurement.
4. Record the continuous decrease of temperature of the thermometer and write down the
value t2 after it becomes steady.
5. Wait until fan stops moving and temperature of wet thermometer increase again.
6. Repeat the measurement two more times and record all the values into the table.
7. Read the atmospheric pressure b of the barometer.
8. Calculate relative humidity (RH) accordingly and express it in percent (%RH).
9. Calculate absolute humidity ϕ using the equation (1) and values from the table 2
determine average values of % RH and ϕ using all three measurements.

Department of Pharmaceutics 50
 Table 1: Determination of relative humidity
1. Temperature of dry thermometer = t1.
2. Temperature of wet thermometer = t2. BP308P
3. Partial pressure of water vapour at temperature t1 = p1.
4. Partial pressure at temperature t2 = p2.
5. Relative humidity = RH.
6. Maximal humidity = ϕmax.
7. Absolute humidity ϕ of air at the laboratory temperature = t1.
8. Difference in wet bulb and dry bulb temperature = Z.

ϕmax ϕ
Measurement t1 [oC] t2 [oC] p1 [pa] p2 [pa] RH
[kg/m3] [kg/m3]

1.
2.
3.
Mean

Table 2: Temperature dependence of the partial pressure of water vapour (pa) and maximal
humidity of air (ϕmax)
Z (oC) Partial pressure [Pa] ϕmax [kg/m3]
11. 1307 10.0 × 10-3
12. 1400 10.7 × 10-3
13. 1493 11.4 × 10-3
14. 1600 12.1 × 10-3
15. 1707 12.8 × 10-3
16. 1813 13.6 × 10-3
17. 1933 14.5 × 10-3
18. 2066 15.4 × 10-3
19. 2173 16.3 × 10-3
20. 2333 17.3× 10-3
21. 2493 18.3 × 10-3
22. 2640 19.4 × 10-3
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 23. 2813 20.6 × 10-3
24. 2986 21.8 × 10-3
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25. 3173 23.0 × 10-3

Department of Pharmaceutics 52