Pharmacutical Engineering, Practical, Lab Mannual..kT

1.
To evaluate size distribution of tablet granules by sieving method and construct

size frequency curves including arithmetic and logarithmic probability plots.
2. To verify the laws of size reduction using Ball mill and calculate Kick's constant,
Rittinger's constant, and Bond's work index of ball mill.
3. To calculate uniformity index for given sample by using double cone blender.
4. To dry calcium carbonate slurry and plot the drying curve.

5. To determine Moisture Content and Loss on Drying from given solid sample
6. To determine Relative humidity (%RH) and dew point temperature using Sling
thermometer
7. To study effect of surface area on the rate of filtration.
8. To study the effect of viscosity on rate of filtration.
9. To study the effect of concentration on rate of filtration.
10. To evaluate factors affecting rate of evaporation.
11. To study the effect of time on rate of crystallization
12. Steam distillation:- To calculate the efficiency of steam distillation
13. To determine Overall Heat Transfer Coefficient of water by heat exchanger.
14. To determine the radiation constant of Iron.

15. To determine the radiation constant of Brass
16. Determination of radiation constant of glass (unpainted and painted)
17. Description of construction, working and application of pharmaceutical

machineries
18. Demonstration of Colloidal Mill, Planetary mixer, Fluidized bed dryer and
Freeze dryer
Experiment No – 1
Aim: To evaluate size distribution of tablet granules by sieving method and construct size frequency curves
including arithmetic and logarithmic probability plots.
ReferENCES:
1. Introduction to Chemical Engineering by Badger and Banchero; Mc Graw Hill publication, New York.
2. Laboratory Manual of Pharmaceutical Engineering by Subrahmanyam CVS, Setty JT, Suresh S.,
Vallabh Publications, New Delhi.
RequiremenTS: Sample of granules
ApparaTUS/ INStrumenTS: Standard sieves set (Sieve No 10, 22, 36, 44, 60, 85) Sieve shaker, weighing
balance, butter paper, etc.
Principle:
There are a number of methods used to monitor particle size distribution. The most popular methods
include sieve analysis, direct imaging and laser diffraction. Sieve analysis presents particle size information
in the form of an S – curve of cumulative mass retained on each sieve versus the sieve mesh size. The most
commonly used metrics when describing particle size distributions are D-Values (D10, D50 & D90) which
are the intercepts for 10%, 50% and 90% of the cumulative mass.
D-values can be thought of as the diameter of the sphere which divides the sample's mass into a specified
percentage when the particles are arranged on an ascending mass basis. For example, the D10 is the
diameter at which 10% of the sample's mass is comprised of particles with a diameter less than this value.
The D50 is the diameter of the particle that 50% of a sample's mass is smaller than and 50% of a sample's
mass is larger than.
In the sieve analysis granules are placed on the upper sieve and sieve set is shaked using electric motor. The
smaller granules will pass through sieve and larger granules will be retained on the upper sieve. Sieve
analysis consists of determination of particle size distribution of solid material by determining the amount
of powder retained on series of sieves with different sized apertures. The weight of the sample of each
sieve is divided by the total weight to give a percentage retained on each sieve. The size of the average
particle on each sieve is then analyzed to get cut off point or specific size range. To find the percent of
aggregate passing through each sieve , first find the percent retained on each sieve by following equation.
Where,
W sieve = weight of granules retained on sieve
W Total = Total weight of granules
1 Pharmaceutical Engineering (SEM III)

DESIGNAtion and DIMENSIONS of IP and USP Specification SievES
Procedure:
1. A standard sieve set is selected. This set consists of various sizes (10, 22, 44, 60, 85, 100 and 120
mesh sieves).
2. Sieves are arranged in descending order of size (Sieve no 10 at top followed by 22, 44, 60, 85 etc).
3. 50 gm of granules is weighed and placed on the top of the sieve set.
4. Loaded sieves are placed on sieve shaker and lid is placed.
5. The timer is adjusted for 5 min and mechanical shaker is switched on.

6. When the shaker automatically stops the sample retained on each sieve is collected on the butter
paper and weighed separately.
7. Weight retained on each sieve is recorded in the observation table against corresponding sieve
number.
8. The data is analysed for normal weight distribution pattern. A graph is drawn by taking mean
particle size of opening on x axis and percentage retained on smaller sieve (undersize) on y axis.
9. The log of granules size is plotted against the cumulative percentage frequency on the
probability scale. It showed linear relationship. The slope of the line and reference point can be
determined.
10. The geometric mean weight diameter Dg can be obtained from straight line.
11. The average particle size can be calculated.
Mechanical Sieve SHAKer

ObSERvaTIONS
 Total Weight of granules----------------g
 Time of shaking-------------min
Note: When all the sieves have been weighed including the bottom pan, the total weight MUST CHECK
WITH THE ORIGINAL WEIGHT WITHIN ± 0.3%. If not the entire sample shall be weighed again and
procedure shall be repeated.
Calculations:
1. For percent weight retained on SIEve:
Where,
W sieve = weight of granules retained on sieve

W Total= Total weight of granules

2. For average diameter (d average):
daverage = ∑nd/∑n =.........µm
ObSERvation Table:

RESULT & DISCUSSION: The average diameter of the sample granules is ..........µm
Practical QUESTIONS (ASSIGNMENt/WorkSHEEt):

1. Define sieve and classify it
2. What are the disadvantages of sieve analysis method of particle size analysis
3. What are the different methods of particle size analysis?
4. What is the significance of particle size analysis?
5. Enlist the different types of sieve shaker.

Experiment No – 2
Aim: To verify the laws of size reduction using Ball mill and calculate Kick's constant, Rittinger's constant, and
Bond's work index of ball mill.
ReferENCES:
1. Theory and practice of industrial pharmacy by Leon Lachman,
2. Cooper and Gunn’s Tutorial Pharmacy by S. J. Cartel
RequiremenTS:
ChemicALS: Powder sample
ApparaTUS/ INStrumenTS: Ball mill, Gyratory Sieve shaker, Sieve set, Balance, Energy Meter
Size Reduction:
Size reduction is the process of reducing the particle size of a substance to a finer state of subdivision to
smaller pieces to coarse particles or to powder. Size reduction process is also referred to as comminution
and grinding. When the particle size of solids is reduced by mechanical means it is known as milling.
MECHANISM of Size Reduction
CuGng – here the material is cut by means of a sharp blade or blades. Eg: Cutter mill
ComprESSION – in this method, the material is crushed between the rollers by application of pressure. Eg:
Roller mill
Impact – impact occurs when the material is more or less stationary and is hit by an object moving at high
speed or when the moving particle strikes a stationary surface. In either case, the material shatters to
smaller pieces.
Usually both will take place, since the substance is hit by a moving hammer and the particles formed are
then thrown against the casing of the machine. Eg: hammer mill
Impact & A†rition – In attrition, the material is subjected to pressure as in compression, along with impact.
Ball mill
Energy of Size Reduction
• Supplied energy is used to Increase the new surface area
• Initiate the flaws or cracks in the particle.
The rESt of energy USED for following
• Elastic deformation
• Transport
• Friction in b/w mill &particle
• Heat

• Vibration& noise
Principle:
A ball mill consisting hallow cylinder mounted on a metallic frame such that it can be rotated along its
longitudinal axis with balls of different diameter which occupy 30-50%of the volume and its size depends on
the feed and mill size. The large balls tend to break down the coarse feed material and smaller balls tend to
form fine product by reducing void spaces between the balls. Ball mills grind material by impact and
attrition.
The degree of milling in a ball is influenced by:
 Residence time of the material in the mill chamber.
 The size, density and number of the balls.
 The nature of the balls(hardness of the grinding material)
 Feed rate and feed level in the vessel.
 Rotation speed of the cylinder.
Several types of ball mill exist. They differ to an extent in their operating principles. They also differ in their
maximum capacity of the milling vessel, ranging from0.010 litres for planetary ball mill, mixer mill or
vibration ball mill to several 100 litres for horizontal rolling ball mills.
Grinding bodies in cascade (a), mixed (b) and waterfall (c) mill operation modes
In multilayer filling mill by grinding media depending on the rotational speed, there is possible line of the
following modes the grinding media motion:
A) CASCade mode trANSPORT: Speed mode with a rolling of grinding balls, but without they flight.
b) Mixed mode motion: Speed mode with a portal rolling and a portal flight of grinding balls.
c) Waterfall mode motion: Speed mode with flying of grinding balls.
Theory:
Size reduction or communication is the process of reducing substance to smaller particles.
ObjectivES:
1. Size reduction leads to increase surface area.
2. Shows around five time's better absorption.

3. Size reduction produces particles in narrow size range. Mixing of powders with narrow size range is
easier.
4. Pharmaceutical capsule, insufficient (i.e. powder inhaled directly into lungs), Suppositories and
ointments require particles size to be below 60mm size.
USES of Size reduction meTHODS
Degree of SIZe reduction Typical meTHODS ExAMPLES
Large pieces Cutter or compression mills Rhubarb
Coarse powders Impact mills Liquorice, cascara
Fine powders Combined impact and attrition mills Rhubarb, belladonna
Very fine powders Fluid energy mills Vitamins and antibiotic
LawS governing energy and power requiremenTS of MILLS:

During size reduction energy is supplied to the equipment (mill).Very small amount of energy(less than
2%).actually produce size reduction. Rest of the energy is dissipated (wasted) in
1. Elastic deformation of particles.
2. Transport of material within the milling chamber.
3. Friction between the particles.
4. Friction between the particles and mill.
5. Generation of heat.
6. Vibration and noise.
7. Insufficiency of transmission n doter.
THEORIES of milling:
A number of theories have been proposed to establish a relationship between energy input and degree of
size reduction produced. A general equation giving the power required for size reduction is
And from this can be derived the following laws:

KickS law (KickS Theory):
It states that the energy required for the size reduction is proportional to the logarithmic of the
ration between the initial and final size. It assumed that the energy required to reduce a material in
size was directly proportional to the size reduction ratio dL/L.
This leads to n=-1.Then,

Where,
Kk =Kicks constant
E = Amount of energy required to produce a change in unit mass, kW.h
d1=Initial particle size of sample (Before size reduction), µm
dn=Final particle size of sample ( AGer size reduction),µm
For crushing (Compression) of large particles, kick's equation is more useful.
RiGngER'S law (RiGngER'S Theory)
It states that the energy consumed in the size reduction of solid is directly proportional
the new surface created. It assumed that the energy required for size reduction is directly proportional, not
to the change in length dimensions, but to the change in surface area.
This leads to n -2 and K= K fc Then,
Where,
E= Amount of energy required to produce a change in unit mass kW.h
3
KR= Rttinger's constant, energy per unit area, KW.h/µm
It is mostly applicable to brittle materials undergoing fine milling. It ignores particle deformation
before fracture.
BOND'S work index (BOND'S Theory)
It states that the energy used for deforming a set of particles of equivalent shape is proportional to the
change in particle dimensions Means, energy used in crack proportional to the change length produced.
According to bond's theory, the equation can be written as,
Where,
E=Energy required for size reduction
KB=Bond's work index, energy per unit mass, kW.h.
di=Initial diameter of particl
dn=Final diameter of particles.
The bond's useful work index is a useful way for comparing the efficiency of milling operation.
This is useful for rough mill size.
AdvantagES:
Ø Ball mill is capable of grinding a wide variety of materials of differing character and of different
degrees of hardness.

Ø It can be used in a completely enclosed form, which makes it especially suitable for use with toxic
materials.
Ø It can produce very fine powders.
Ø It can be used for continuous operation, and a classifier can be used in conjunction with the mill, so
that particles of suitable size are removed while oversize particles are returned.
Ø It is equally suitable for wet or dry grinding processes.
DISADVantagES
Ø Wear occurs, principally from the balls, but partially from the casing and this may result in the
product being contaminated, with abrasive materials this may exceed 0.1 percent, but even
ordinary substances may be contaminated with 0.03 percent metal aGer grinding.
Ø In some cases, this may not be significant, but in others it may be of great importance.
Ø SoG or sticky materials may cause problems by caking on the sides of the mill or by holding the
balls in aggregates.
Ø The ball mill is very noisy machine, particularly if the casing is of metal, but much less so if rubber is
used.
Ø Relatively long time of operation
Critical Speed of Ball Mill
In a ball mill balls rotating at a low speed, the balls rolls and cascade over one another, providing an attrition
action. As the speed is increased, the balls are carried up the sides of the mill and fall freely on to the
material with impact action which is most responsible for size reduction. The speed at which ball falls on the
material known as cascading effect is called as critical speed of ball mill
Example
In a ball mill of diameter 2000 mm, 100 mm dia steel balls are being used for grinding. Presently, for the
material being ground, the mill is run at 15 rpm. At what speed will the mill have to be run if the 100 mm
balls are replaced by 50 mm balls, all the other conditions remaining the same?

The critical speed of ball mill is given by,
1 g
nc = 2 R-r
where
R = radius of ball mill;
r = radius of ball.
For R = 1000 mm and r = 50 mm,
nc = 30.7 rpm
But the mill is operated at a speed of 15 rpm. Therefore, the mill is operated at 100 x 15/30.7 = 48.86 % of
critical speed.
If 100 mm dia balls are replaced by 50 mm dia balls, and the other conditions are remaining the same,
0.5
Speed of ball mill = [0.4886/(2p)] x [9.812/(1 - 0.025)]
= 14.8 rpm
PROCEDURE:
1. The initial dial reading of energy meter is noted as N1
2. The cleaned metal chamber (of ball mill) is taken with sufficient number of balls.
3. The ball mill is operated without load for 30 min.
4. The reading (revolutions) in energy meter is noted down, N2.
(The difference, i.e., N3= N2 – N1 gives the energy required for running the ball mill without feed).
5. Hundred grams of sample is weighed and subjected to sieve analysis. The average particle size of
the sample is calculated.
6. Hundred grams of feed, which was subjected to sieve analysis is transferred into the ball mill.
7. The ball mill is operated for 30 minutes
8. The reading (revolutions) is noted down as N4. (The difference, i.e., N5 = N4– N2 gives the energy
required for running the ball mill and size reduction of material).
9. The difference, i.e., N6 = N5 – N3, gives the energy actually consumed for the size reduction material.
10. The product is unloaded on to a tray and subjected for sieve analysis.
11. The average particle size of the product aGer size reduction is determined.
12. The data is substituted in respective equation for obtaining Kick's constant, Rittinger's constant, and
Bond's work index, respectively.

Sieve Analysis of Sample Prior to and After Size Reduction
Sieve Nominal Aperture Mean size Before size After size

number mesh size of opening reduction reduction
aperture (passed/ d. µm
Weight of Weight of
size, µm retained)
powder powder
,
retained on retained on
µm
smaller sieve, smaller sieve,
undersize n, g undersize n, g
(1) (2) (3) (4) (5) (6)
- -
Weight DIStribution AnalySIS of Sample – Before Size Reduction
Mean Weight of powder Per cent weight Wt. Size in (n *

size of retained on smaller retained on d) (1) * (3)
opening, sieve, undersize, g smaller sieve, n
µm d
(1) (2) (3) (4)
Σn= 100 Σnd =
Mean diameter of the powder SAMPLE (before SIZe reduction), di = Σnd / Σn

Weight DIStribution AnalySIS of Sample – After Size Reduction
Mean Weight of powder Per cent weight Wt. Size in (n * d)
size of retained on smaller retained on (1) * (3)
opening, sieve, undersize, g smaller sieve, n
µm d
(1) (2) (3) (4)
Σn= 100 Σnd =
Mean diameter of the powder sample (before size reduction), dn = Σnd / Σn
OBSERVATION AND CALCULATIONS

Initial reading of energy meter, N1 =
Energy meter reading aGer the use of ball mill without feed, N2
= Energy consumed by the ball mill, N3 = (N2- N1) =
Energy meter reading aGer the use of ball mill with feed, N4 =
Energy consumed for size reduction plus the ball mill, N5 = N4=
Energy consumed for size reduction, N6 = (N5 – N3) =
Weight of the sample taken, W= (100gm) 0.1kg
Calculation of energy meter constant E (on the energy meter, the relationship between the revolutions and
energy given. Use that relationship for calculations)
750 units reading (revolutions) the energy = 3600 kW.s (1 kW.h)
1 unit reading = ?
1 unit = 3600 / 750 = 4.8 kJ (E)
Energy on no load, E1=N3 * E = .........kJ
Energy on load , E2 = N5 * E = ..........kJ
Net Energy required per unit mass = { ( E2 – E1 )/w} =. ......kJ
Average particle diameter of feed, di =..........µm

Average particle diameter of product, dn = µm
The energy required to reduce the size of particles can be calculated by Rittinger's equation and Bond's
equation. The principle involved is the determination of mean particle size of material before and aGer size
reduction. These changes are related to the energy consumed for size reduction.
EQUATIONS
KICK'S LAW :
Where,
Kk =Kicks constant
E = Amount of energy required to produce a change in unit mass, kW.h
di=Initial particle size of sample (Before size reduction), µm
dn=Final particle size of sample ( After size reduction),µm
RITTINGER's LAW:
Where,
E= Amount of energy required to produce a change in unit mass kW.h
KR= Rttinger's constant, energy per unit area, KW.h/µm
BOND'S WORK INDEX:
Where,
E=Energy required for size reduction
KB=Bond's work index, energy per unit mass, kW.h.
di=Initial diameter of particle

dn =Final diameter of particles.
RESULT & DISCUSSION:

Rittinger's Constant:
Kick's Constant:
Bonds Work Index:

1. Give objectives of size reduction process
2. Write the principle of ball mill.
3. What is Kick's law?
4. What is Rittinger's law
5. Define Bond work index.

Experiment No – 3
Aim: To calculate uniformity index for given sample by using double cone blender.
ReferENCES:
rd
1. Lieberman, Herbert A, Lachman, Leon (2009), Industrial pharmacy: 3 edition
2. Cooper and Gunn's Tutorial pharmacy by S. J. Carter.
RequiremenTS:
ChemicALS: 01 N Hydrochloric acid solution, 0.1 N Sodium hydroxide solution, Phenolphthalein
indicator, Calcium carbonate, Talk and Oxalic acid
ApparaTUS/ INStrumenTS: Double cone blender, conical flasks (250 ml), Pipette (10 ml), Burette (50
ml), Voumetric flask (100 ml, 500 ml), Weighing balance and Stop watch.
Principle
Mixing of calcium carbonate and talc is studied using double cone blender. Blender allowed rotating on its
own axis. During this process, the particles move freely to ever of the equipment. Time of mixing should be
long enough to obtain an acceptable randomization. Samples of the mixed materials are collected at
different intervals ran from the different locations. The components are analyzed by the method of acid
titration. Amount of calcium carbonate is determined by treating the sample with excess of hydrochloric
acid. Unreacted hydrochloric acid solution can be determined by titrating against sodium hydroxide
solution using phenolphthalein as indicator. Drug uniformity achieved during mixing is calculated by a
statistical procedure.
Uniformity index is determined using the following formula
∑
√
2
( y− y¿)
Us = ¿
n(1− y) y
Where,
Us=Uniformity index
n =Number of
samples
y¯ = True average composition of component A in the
mixture y = Actual composition of component A in a single
sample.
Us values are calculated at different time intervals. Based on results, optimum time required for actual
mixing is estimated. A graph can be plotted by taking time of mixing and uniformity index on y-axis.
Theory:
Mixing is the process of thoroughly combining different materials to process thoroughly combing different
materials to produce a homogenous product. The mixture is generally a combination of dissimilar materials;
eg.

Coal ash and cement are blended in a specified ratio to produce Pozzocrete cement. In other cases, a
chemically homogenous material may be mixed to produce a uniform lot of a desired weight/volume with
consistent particle size distribution, colour, texture and other required attributes, e.g. metal powders
produced in 1 ton batch size are blended to a homogeneous lot size of 4 tons. The term mixing and
blending are oGen used interchangeably, but technically they are slightly different. Blending is process of
combining materials, but blending is a relatively gentle process Compared to mixing. In terms of the phase
of material blending is the process of solid-solid mixing or mixing of bulk solids with small quantity of liquid
The terminology mixing is more closely associated with liquid-liquid gas-liquid and viscous materials. Mixing
and Blending are the most demanding unit operations in the chemical process industries.
MECHANISM of mixing of SOLIDS
1 Convective mixing/Macro mixing: Inversion of the powder bed using blades or paddles or Screw element
in which large mass of material moves from one place to another.
2 Shear mixing: In this type, forces of attraction are broken down so that each particle moves on its own
between regions of different components and parallel to their surface.
3. DIFFUSION mixing/Micro mixing: Involves the random motion of particle within the powder bed, thereby
particles change their position relative to one another.
Double Cone Blender:
The Double Cone Blender is a conventional mixer suitable for dry powder mixing. These mixer is suitable for
mixing a number of powders in varied proportions to obtain uniform output.
Double cone blender
FeaturES:
1. The conical shape at both ends enables uniform mixing and easy discharge.
2. The cone is statically balanced which protects the gear box and motor from any excessive load.
3. Powder is loaded into the cone through a wide opening and discharged through a excessive
load butterfly or a Slide valve.
4. Depending upon the characteristic of the product, paddle type baffles can be provided on the
shaG for better.

5. Contact parts are made of S304 or SS 316.
6. Flame proof electrical can be provided as optional.'
7. Slant' design (off centre) CLIN CONE BLENDER
8. Dust free bin charging system ensures minimum material handling
9. Mixing, uniform blending and de-agglomeration
Preparation and Standardization of SOLUTIONS:
 Preparation of Oxalic acid SOLUTION IP:
About 0.63 g of oxalic acid (molecular mass is 63 g/mol) is weighed and transferred into a 100 ml volumetric
flask. Water is slowly added and shaken to dissolve the substance. Sufficient water is added to make 100 ml.
Exact normality is calculated.
Weight of oxalic acid added, w =.................g
Normality of oxalic acid solution, N1 =
 Preparation of SODIUM hydroxide (0.1 N) SOLUTION IP

Solution of any normality, xN, may be prepared by dissolving 40x g of sodium hydroxide in water and
diluting to 1,000ml. About 0.4g of sodium hydroxide is weighed and transferred into 100 ml of volumetric
flask. Water is slowly added with continuous stirring while cooling the flask under running tap water.
Sufficient water is added to make 100 ml. The solution is allowed to stand overnight and decanted the clear
liquid in to a bottle. This clear liquid is used.
 Standardization of SODIUM hydroxide (0.1N) SOLUTION IP
10 ml of standardized oxalic acid solution is pipette into conical flask. A drop of phenolphthalein indicator
solution is added. The solution is titrated against sodium hydroxide solution placed in burette. Then, exact
normality is calculated.
Burette =Sodium hydroxide solution
Conical flask =10 ml oxalic acid solution
Indicator =Phenolphthalein indicator solution
End point= Colourless to pink
Burette readings I II III
Initial reading, ml
Final reading, ml
Volume used, ml

Average volume, V2=… ...........ml
Normality of oxalic acid solution, N1=……............
Volume of oxalic acid solution taken, V1 =10ml
Volume of sodium hydroxide solution consumed,V2=…..............
Normality of sodium hydroxide solution,
Preparation of hydrochloric acid (0.1N) SOLUTION IP:

Solution of any normality, xN, may be prepared by diluting 85x ml of hydrochloric acid to 1,000ml with
water. 250ml of distilled water is taken into a 500ml volumetric flask. 4.25ml of concentrated hydrochloric
acid is slowly added with continuous shaking. The flask is Cooled under tap water. Distilled water is added
to make the volume (500ml) up to the mark.
Standardization of hydrochloric acid (0.1N) SOLUTION IP:

10 ml of hydrochloric acid solution is pipette in to a conical flask. A drop of phenolphthalein indicator
solution is added. The solution is titrated against standardized sodium hydroxide solution placed in burette.
Then exact normality is calculated.
Burette= Standardized sodium hydroxide
solution Conical flask =10 ml hydrochloric acid
solution Indicator =Phenolphthalein indicator
solution End point=Colourless to pink
Burette readings I II III
Initial reading, ml
Final reading, ml
Volume used, ml
Average volume, V3=…….

Normality of sodium hydroxide solution, N2 =… .......N
Volume of hydrochloric acid solution taken, V4 = 10 ml
Volume of sodium hydroxide solution consumed.
V3=10ml
Normality of hydrochloric acid solution,

Determination of converSION factor:
Accurately weighed 100mg of calcium carbonate is placed in a conical flask (250ml). 30 ml of hydrochloric
acid solution (N3 =…….) is added. The contents are thoroughly shaken to ensure complete reaction. The
unreacted hydrochloric acid is titrated against standard sodium hydroxide solution. (N2 =……) Conversion
factor is calculated.
It IS Calculated with rESPECT to calcium carbonate only, SINCE talc IS an inert material.
Burette= Standardized Sodium hydroxide solution
Conical flask = 100mg calcium carbonate + 30 ml standardized hydrochloric acid
solution Indicator Phenolphthalein indicator solution
End point Colourless to pink
Burette rEADINGS I II III
Initial reading, ml
Final reading, ml
Volume used, ml
Average volume, x=…............ml

The volume of sodium hydroxide solution consumed, x=…............ml
A mixture of 100mg of CaCO3 and 30 ml of (N3 ==….....N) HCI consumes x ml of (N2=… N) NaOH solution.
Unreacted HCL (N3 ==…N) in the mixture reacted with x ml of sodium hydroxide
solution. Normality of sodium hydroxide solution, N2 =… N
Normality of hydrochloric acid solution taken, N3=… ....N
Volume of sodium hydroxide solution = x =…........ml
Equivalent volume of hydrochloric acid solution
unreacted, (30 e)ml of HCI (N3= N) reacts with 100
CaCO3
1 ml of HCl =
Procedure:
1. 5.0g of calcium carbonate and 5.0 g of talc are weighed.
2. These two powders are placed in a cylindrical blender.
3. The blender is allowed to rotate for 10 minutes at 25 revolutions per minute.
4. The samples ( 500 mg) are drawn from three different places of the blender and
placed in three different conical flasks. Labelled them as 1A, 1B and 1C.
5. The blender is again allowed to rotate for another 10 minutes.
6. Again three samples are drawn in a similar way as menti oned in step 4. They are
transferred into three different conical flasks and labelled them as 2A 2B and 2C.
7. Repeat the steps 5 and 6 for another 10 minutes. The samples are labelled as 3A 3B
and 3C.
8. 30ml of standard HCl solution (N3 = --------) is placed in each conical flask.
9. The contents of flasks are shaken thoroughly to complete the reaction between HCl
and calcium carbonate.
10. Unreacted HCI is determined by titrating against standard NaOH solution. (N2 =-----)
11. The content of calcium carbonate present in each sample is calculated and reported
in table.
12. The data is substituted in equation of the uniformity index and further uniformity index is
calculated for the desired intervals.
13. A graph is plotted by taking time on x-axis and uniformity index on y-axis.
ObSERvation and Calculation:
Titration data for EStimation of calcium carbonate in the blended SAMPLE:
Sampling Sample Volume of NaOH Volume of Volume of HCl Weight (y‐y)2
time number CONSUMED NaOH reacted with of
CONSUMED CaCO3, CaCO3
(3)‐(4),ml ml 30‐(5) (6) x d,
equivalent of y.
HCl
Initial Final
volume, volume,
ml ml
1 2 3 4 5 6 7
At 10 1A
minutes
1B
1C
Average y=S(y -y)2=
At 20 2A
Minutes
2B
2C
Average y=S(y -y)2=
At 30 3A
Minutes
3B
3C
Average y=S(y -y)2=

Weight of sample taken=500mg
Volume of HCl (N3=… .....) added =30ml
Conversion factor(d)=….......
Calculation of Uniformity Index
Us = ∑
√( y− y¿)2
n(1− y) y
¿
Where,
Us=Uniformity index
n =Number of samples
y¯ = True average composition of component A in the mixture
y = Actual composition of component A in a single sample.
RESULT:
The uniformity index of mixing using double cone blender was for given sample was found to
be , Uniformity index aGer 10minutes,U10=…..
Uniformity index aGer 20minutes,U20=…..
Uniformity index aGer 30minutes,U30=…..

1. Enlist powder mixing mechanisms?
2. Give examples of different types of blenders.
3. Enlist factors affecting rate of mixing.

Experiment No – 4
Aim: To dry calcium carbonate slurry and plot the drying curve.
ReferENCES:
2. Perry's Chemical Engineers' Handbook, by Don W. Green, Robert H. Perry, Mc Graw Hill publication,
New York.
nd
4. Geankoplis, Christie, J (1983). Transport Processes and Unit Operations, 2 ed. Massachusetts,
Allyn and Bacon. Inc., pg 508-552.
RequiremenTS:
ChemicALS: Distilled water, calcium carbonate.
ApparaTUS/ INStrumenTS: Beaker, Stirrer, Porcelain dish, hot air oven, weighing balance.
Principle:
Drying is defined as removal of small amount of water or other liquid from a material by application of heat. Drying
involves both heat and mass transfer operations. Heat must be transferred to the material to be dried in
order to supply the latent heat required for vaporization of the moisture. Mass transfer involves the
diffusion of water through the material to the evaporating surface and subsequent evaporation of water
from the surface.
Rate relationship can be studied considering a simple model, which mimics the conditions of a dryer. In this model,
the wet slab to be dried is placed in a tray whose bottom and sides are insulated. The air is blown over the
solid under the constant drying conditions (air velocity, temperature, humidity and pressure). The
superficial water diffuses through the surrounding air film and is carried away rapidly by the moving stream.
Then water diffuses from the interior of the solid to the surface. This process continues until bound water
gets evaporated. Then the materials attain equilibrium moisture content.
ApplicaTIONS:
 In the manufacturing of bulk drugs.
 Drying is necessary in order to avoid deterioration.
 Granules are dried to improve the fluidity and compression characteristics.
 Drying of viscous and sticky material modifies the flow characteristics.
 Removal of moisture makes the material light in weight and reduces the bulk.
Procedure:
1. The stainless steel plate / petridish is weighed and the weight is recorded W1gm.

2
2. Area of The stainless steel plate/ petridish is determined (2rh + r ).
3. 10 g of calcium carbonate is transferred into a steel plate/ petridish. Let the weight of stainless steel
plate / petridish and powder be W2 gm.
4. Water (around 30 ml) is added slowly to prepare slurry into the stainless steel plate / petridish.
th
Filling must be done in such a way that 3/4 of the volume of the stainless steel plate / petridish is
filled with slurry.
5. The weight of steel plate / petridish plus slurry is taken and recorded as W3 gm.
0
6. The plate containing slurry is placed in hot air oven, whose temperature must be maintained at 60 C.
7. The time is noted soon after placing plate containing slurry in hot air oven. Drying is continued and
weight of the sample is recorded every 15 minutes until constant weight is obtained.
8. % Moisture content and drying rate for each time interval is determined using following equation
% moisture content W3 - W2
= W3 - W1 x 100
Drying rate = W3 - W2
area of petridish
x Time (in min)
'A'
9. The rate of drying is calculated. A graph is plotted by taking % moisture content on x-axis and rate of
drying on y-axis.
10. Another graph is plotted by taking drying time on x axis and % moisture content on y-axis
Drying time curve

Rate of drying curve

ObSERvaTIONS
 Weight of dry calcium carbonate: g
 Weight of the empty porcelain dish, W1 g
 Weight of the porcelain dish + Sample, W2 g
 Weight of the porcelain dish + slurry, W3 g
 Weight of the porcelain dish + slurry, (After drying at different time intervals), W4
MC1 = moisture content at '0' time = W3 - W2

W2 - W1
W4 - W2
MC2 = = moisture content after 15 mins. =
W2 - W1
Average moisture content = MC1 + MC

22
ObSERvation Table:
Sr. Time(min) W4 Moisture content Average moisture Rate of drying

No. content
(MC2)
MC1 + MC2
2

CalculaTIONS:
RESULTS & DISCUSSION:

1. Define Drying, FMC, EMC
2. What is drying rate?
3. What are applications of drying?
4. Describe and differentiate drying of porous and non- porous solids along with their drying curves.

Experiment No – 5
Aim: To determine Moisture Content and Loss on Drying from given solid sample
ReferENCES:
New York.
RequiremenTS:
ChemicALS: Sample (Calcium carbonate)
ApparaTUS/ INStrumenTS:
Hot air oven, analytical balance, glass crucibles, Petri dish, tongs.
Principle:
Loss on drying is a widely used test method to determine the moisture content of a sample, although
occasionally it may refer to the loss of any volatile matter from the sample. Loss in drying does not usually
refer to molecularly bound water or water of crystallisation. The temperature at which you should expose
the substance to be tested is always specified and must not be exceeded it or you get the wrong results.
Every substance has its specific heat level. Loss on drying testing in pharmaceuticals is a technique of
removing water and other volatile impurities from a sample of well-mixed substance. The amount of heat
applied on the substance is dependent on time and temperature. Total moisture content of pharmaceutical
products can contain both bound and free water. Where there are impurities present then loss on drying
level will be higher as compared to water content.
The rate of drying is determined moisture content and the temperature of the compound and the
temperature, the humidity (relative) and the velocity of the air in contact with the compound. Equilibrium
moisture content (EMC) is the amount of water present in solid, which exerts vapour pressure equal to the
vapour pressure of the atmosphere surrounding it. When air is continuously passed over the solid
containing moisture more than EMC, then solid adsorbs water continuously till EMC is reached. This
phenomenon is known as sorption. From these observations, it is clear that material can be dried up to
EMC, but not below it.
There are two basic mechanism involved in the drying process viz. the migration of moisture from the
interior of an individual compound to the surface, and the evaporation of moisture from surface to
surrounding air the value of EMC depends on the material and relative humidity and temperature of the air
with which it is in contact. The speed with which it is approached depends on the properties of the
material, the surface-area-to- volume ratio of its shape, and speed with which humidity is carried away or
towards the material (e.g. diffusion in stagnant air or convection in moving air)

Important factor affecting the rate of drying are :
Ø Initial moisture content of the raw
material. Ø Composition of raw material.
Ø Initial load of the feed kept in drier.
Ø Size, shape and arrangement of stacking of the raw material.
Ø Temperature, relative humidity and velocity of air used for
drying. Ø Rate of heat transfer on the surface of the food.
Ø Pre-treatment of the raw material prior to drying (peeling, blanching, etc)
Ø During drying process, the control air temperature and its circulation in the system is important.
Procedure:
A] Determination of MOISture content
1) 5 gm of sample (chalk powder/ starch/ talc) is accurately weighed.
2) Sample is transferred into empty crucible and weight is recorded.
3) Crucible containing sample is placed into hot air oven at 60ºC and its weight is recorded aGer each
10 minutes interval for a period of 1 hour.
4) Moisture content and % moisture content is calculated.
B] Determination of LOSS on Drying
1) 5 gm of sample (chalk powder/ starch/ talc) is accurately weighed.
2) Sample is transferred into previously weighed empty crucible and its weight is recorded along with
sample.
3) Crucible containing sample is placed into hot air oven at 100ºC for a period of 1 hour.
4) AGer one hour of heating again the weight of crucible is recorded.
5) Loss in weight of sample is calculated aGer 60 minutes of heating.
6) % LOD is calculated.
ObSERvaTIONS:
A] Determination of MOISture content
Weight of sample powder =W=
Weight of empty crucible =W1=
Weight of crucible with sample =W2=
Temperature of oven =

ObSERvation table:
Time (min) Weight of crucible MOISture content % MOISture content

with powder a†er w2- w3 w2-w3
= = x 100
drying W3 (gm) w2- w1 w2-w1
0
10
20
30
40
50
60
B] Determination of LOSS on
Drying Weight of sample powder
=W1= Weight of empty crucible
=W2=
Weight of crucible with sample before drying=W3=
Weight of crucible with sample aGer drying of 60 minutes =W4=
Weight of sample aGer drying of 60 minutes =W5= W4 –W2
Temperature of oven =
ObSERvation table:
Sr. No. Sample Weight of powder a†er 1 hour of drying

CalculaTIONS:

1. % Moisture content of sample was found to be
2. % Loss on drying of sample was found to be

1. What are applications of LOD
2. Does LOD determine free water / total water content of sample?
3. What is significance of LOD and % moisture content?

Experiment No – 6
Aim: To determine Relative humidity (%RH) and dew point temperature using Sling thermometer
ReferENCES:
2. Basic Refrigeration and Air Conditioning Paperback by Anantha Narayanan
RequiremenTS:
ChemicALS: Distilled water
ApparaTUS/ INStrumenTS: Cotton wick, Sling's thermometer (Psycrometer)
Principle:
Sling Psychrometer is used to measure both the dry bulb and wet bulb temperatures at time. These
temperatures are a measure of humidity content in air. This instrument works on the principle of
evaporation of water. When water on a surface evaporates, it extracts a significant amount of heat from it,
cooling the surface down. This is how sweat is able to cool down our body and skin when it gets hot.
However, air can only hold a limited amount of water, aGer which it becomes saturated. This can be
observed in beaches and coastal regions, where, since the air is humid, the sweat from our bodies doesn't
evaporate easily. The psychrometer is designed to make use of both these facts, to help us measure the
humidity of air.
Sling PSychrometer
DESCRIPTION of Sling
PSychrometer
Ø The instrument frame carrying the thermometer is covered by a glass casing.
Ø A swivel handle is attached to frame-glass casing – thermometer arrangement to ensure that the air
at the wet bulb always in immediate contact with the wet wick.
Ø When a thermometer bulb is directly exposed to an air-water vapour mixture, the temperature
indicated by the thermometer is the dry-bulb temperature.

Ø When a thermometer bulb is covered by a constantly wet wick and if the bulb covered by the wet
wick is exposed to air water vapour mixture, the temperature indicated by the thermometer is the
wet bulb temperature.
Ø The instrument frame which holds the thermometers. One mercury in glass thermometer whose
sensing bulb is bare to directly contact the air and to measure the temperature which is called as
the dry‐bulb temperature.
Ø One mercury in glass thermometer whose sensing bulb is covered with a cotton or muslin wick
made wet with pure water. This sensing bulb covered with the cotton wick moistened is made to
contact the air and the temperature indicated by this thermometer is called as the wet bulb‐
thermometer.
The parameterS on a pSychrometric chart are:

 Dry bulb temperature (DBT): DBT of an air sample, as determined by an ordinary thermometer. It is
typically plotted as the abscissa (horizontal axis) of the graph.
 Wet bulb temperature (WBT): WBT is that of an air sample, aGer it has pass through a constant
pressure, ideal, adiabatic saturation process. That is, aGer the air has passed over a large surface of
liquid water in an insulated channel. This temperature is indicated by diagonal lines on the chart.
 Humidity ratio: It is the proportion of mass of water vapour per unit mass of dry air at the given
conditions. It also known as moisture content or mixing ratio. It is typically plotted as the ordinate
(vertical axis) of the graph.
 Specific volume: It is the volume of mixture (dry air plus the water vapour) containing one unit of
mass of “dry air”
 Dew point temperature: DPT is the temperature at which a moist air sample at the same pressure
would reach water vapour “saturation”. At this point further removal of heat would result in water
vapour condensing into liquid water fog. This temperature is shown as horizontal lines on chart.
 Enthalpy: It is the sum of the internal (heat) energy of the moist air in question, including the heat
of the air and water vapour within. Enthalpy is indicated by diagonal lines on chart.
 Relative humidity: RH is the ratio of the mole fraction of water vapour to the moles fraction of
saturated moist air at the same temperature and pressure. RH is dimensionless and is usually
expressed as a percentage. Lines of contrast RH reflect the physics of air and water; they are
determined via experimental measurement. Lines of constant relative humidity are shown as
exponential lines on the pshychrometric chart. The line at 100% is referred to as the saturation line.
 MOISture content: This is also known as humidity ratio and is usually designated as W. It is the
proportion of the mass of water vapour per unit mass of dry air. Humidity ratio is dimensionless,
but in the US it is usually expressed as pounds of moisture per pound of dry air, elsewhere it may be
expressed as pounds per kilogram of dry air or as a percentage. The moisture content is the vertical
axis of the chart.

Wet and Dry bulb temperaturES or PSychrometer
Application of Sling PSychrometer / thermometer

 It is used for checking humidity level in air-conditioned rooms and installations.
 It is used to set and check hair hygrometer.
 It is used in the measurement range of 0 to 100% RH.
 It is used for measuring wet bulb temperature between 0'C to 180ºC.
Procedure:
 In order to measure the dry bulb and wet bulb temperature, the Psychrometer frame – glass
covering – thermometer arrangement is rotated at 5 m/s to 10 m/s to get the necessary air motion.
 Note: An important condition is that correct/accurate measurement of wet bulb temperature is
obtained only if air moves with velocity around the wet wick. In order to get this air velocity, the
Psychrometer is being rotated.
 The thermometer, whose bulb is bare, contacts the air and indicates the dry bulb temperature.
 At the same time, the thermometer whose bulb is covered with the wet wick comes in contact with
the air and when this passes on the wet wick present on the bulb of the thermometer, the moisture
present in the wick starts evaporating and a cooling effect is produced at bulb. Now the
temperature indicated by the thermometer is the wet bulb thermometer which will naturally be
lesser than the dry bulb temperature.
 Note: If the Psychrometer is rotated for a short period, then the wet bulb temperature recorded will
not be proper.
 Note: If the Psychrometer is rotated for a longer period, the wick will get dried soon and the wet
bulb temperature will not be at its minimum value.

Step1: Pre‐preparation
Before using the psychrometer, it is advisable to perform an initial pre-preparation step, to ensure that you
get accurate readings out of it. Basically you have to ensure that both, the thermometers on the device are
displaying the same initial reading, so that the measurement commences from the same starting point. A
good way to do this is to shake the psychrometer rapidly for about a minute.
Step2: Prepare the Wick
The device uses a wet bulb thermometer in addition to a normal (dry) one. You need to completely soak the
wick/sock of the wet bulb thermometer in water to prepare it for use.
Step3: Whirl the PSychrometer
Once you have readied your instrument by following the steps given above, you can start using it. You have
to swing it around in circles for approximately a minute to allow the water from the wick to get evaporated
into the surrounding air, and thus cool the wet-bulb thermometer.
Step 4: Take the READINGS
AGer swinging it for a minute, note down the readings from both the thermometers, starting first with the
wet one.
Step 5: Calculate the Humidity
To calculate humidity, simply take the difference between the temperature values obtained in the previous
step, and then refer to a psychrometric chart to know the humidity value.
Step 6: The horizontal line that paases though point of intersection of wet bulb temp and dry bulb
temperature on leG hand side of the chart ( on 100%RH line) reads dew point temperature.
ObSERvaTIONS
0
 Dry bulb temperature : C
0
 Wet bulb temperature : C
ObSERvation Table:
Dry bulb temperature Wet bulb temperature % Relative humidity Dew point temp.
0 0
C C
CalculaTIONS:
Using Psychometric chart extrapolate the obtained dry and wet bulb temperature to read the % Relative
humidity

Relation between dry and wet bulb temperature and the % Relative humidity is obtained

1. What are applications of psychrometric?
2. Relation between dry and wet bulb temperature and the % Relative humidity
3. Study of psychrometric charts and how to plot them.
4. What is dew point temperature? Why does it lie on 100 % RH line always?

Experiment No – 7
Aim: To study effect of surface area on the rate of filtration.

ReferENCES:
New York.
RequiremenTS:
ChemicALS: Calcium carbonate, water.
ApparaTUS / INStrumenTS: Beakers, Buchner funnel of various sizes, glass rod, measuring cylinder, stop
watch.
Principle:
 In the process of filtration the liquid passes through the filter medium, which offers resistance to its
passage. The pressure differential across the filter is the driving force for the operation. The rate of filtration
is given by :
 Rate of filtration = driving force / resistance
 The resistance for filtration is offered by filter medium and filter cake. Resistance of filter cake is
nothing but specific resistance of cake i.e. resistance per unit cake thickness multiplied by thickness of cake.
The resistance is also proportional to the viscosity of the fluid.
 The other factor affecting the rate of filtration are said to be surface area, pressure drop, viscosity,
etc.
 The total volume of filtrate flowing from the filter will be proportional to the area of the filter. The
rate of filtration increased by increasing surface area of filter medium.
Procedure:
(Effect of SURFace area on rate of filtration)
1. Buchner funnels with filter paper is arranged properly.
2. Three different sizes of Buchner funnel are used in this study.
3. Area of each funnel is calculated.
4. 2 g of calcium carbonate is weighed and dissolved in 100 ml of water, the prepared slurry is passed
through filtration assembly (small size funnel)
5. Time required to collect 50 ml of filtrate is recorded.
6. Rate of filtration is calculated.
7. The same process is repeated for different sizes of filter assembly and the rate of filtration is
calculated for each size.

Formula:
ObSERvaTIONS and calculaTIONS:

ObSERvation table: for effect of SURFace area on rate of filtration
TRIALS Volume Small diameter funnel Medium diameter funnel Large diameter funnel
of Area = Area = Area =
filtrate Time (min) Rate of Time (min) Rate of Time (min) Rate of
( ml) filtration filtration filtration
ml/min ml/min ml/min
I 50 ml
II 50 ml
III 50 ml
Average 50 ml
RESULT :

1. What is rate of filtration?
2. What are the factors affecting the rate of filtration
3. Enlist name of filter aids.
4. What are filter aids?
5. What will be effect of change in viscosity, surface area on rate of filtration?

Experiment No – 8
Aim: To study the effect of viscosity on rate of filtration.

Reference:
New York.
RequiremenTS: ChemicALS: Calcium carbonate and Glycerin
INStrumenTS/ apparaTUS: Beakers, Buchner funnel of various sizes, glass rod, measuring cylinder, stop watch.
Principle:
 An increase in viscosity of the liquid will decrease the flow rate. The increase in viscosity of filtrate
will increase the resistance to flow so that the rate of filtration is inversely proportional to viscosity of flow.
 This problem can be overcome by increasing the temperature of liquid or by reducing the
concentration of solids in the liquid.
 The vehicles containing different concentrations of glycerine – water mixtures are used. Viscosity
increases with increase in the concentrations of glycerine in the mixture.
Procedure:
(Effect of VISCOSITY on rate of filtration):
2. Three different solutions, viz. water, 5% glycerine in water and 20 % glycerine in water is taken for
the experiments.
3. The prepared solutions are passed through filtration assembly separately.
5. Rate of filtration is calculated using following equation.
ObSERvation and calculaTIONS:

ObSERvation table:
Sr. Sample name VISCOSITY of SAMPLE Filtration time Rate of filtration
no required for 50 ml (ml /min)
of filtrate (min)
1 Water Low
2 5% glycerine in water Medium
3 10 % glycerine in High
water
RESULT:

1. Give principle of filtration process.
2. Distinguish between filtration and clarification?
3. How viscosity affects rate of filtration?
4. Discuss applications of filtration.
5. What is the effect of viscosity on rate of filtration?

Experiment No – 9
Aim: To study the effect of concentration on rate of filtration.

Reference:
New York.
RequiremenTS:
ChemicALS: Calcium carbonates and Water
INStrumenTS/ apparaTUS: Beakers, Buchner funnel of various sizes, glass rod, measuring cylinder, Stop watch.
Principle:
The rate of filtration depends on the concentration of solids. As the concentration of solids in the
suspension increases the thickness of the filter cake increases. As a result the rate of filtration decreases.
This can be estimated by collecting definite quantity of filtrate in give interval for given set of conditions.
Procedure:
(Effect of concentration on rate of filtration):
2. Different concentrations of 100 ml of calcium carbonate slurry (5%, 10% and 15% w/v) is prepared
in water
3. The prepared slurries are passed through filtration assembly separately.
5. Rate of filtration is calculated using following equation.
ObSERvation and calculaTIONS:

ObSERvation table:
Sr. Sample name Concentration of Filtration time Rate of filtration
no SOLUTION required for 50 ml (ml /min)
of filtrate (min)
1 5 % w/v calcium 5%
carbonate slurry
2 10 % w/v calcium 10 %
carbonate slurry
3 15 % w/v calcium 15 %
carbonate slurry
RESULT:

1. What is the effect of concentration of slurry on rate of filtration?
2. Write the action of filter aid on filtration?
3. What is the effect of filter aid concentration on filtration rate?

Experiment No – 10
Aim: To evaluate factors affecting rate of evaporation.

ReferENCES:
New York.
RequiremenTS:
ChemicALS: Water, Sodium Chloride, glycerin.
INStrumenTS/ apparaTUS: Water bath, thermometer, weighing balance, beakers (50, 100, 250 and 500 ml),
stirrer, measuring cylinder.
Principle:
 Evaporation is the process of vaporizing the large quantities of volatile liquid to get a concentrated
product. The rate of evaporation depends on several factors temperature, viscosity, and concentration of
slurry, vapour pressure, surface area, and time of evaporation, films and deposits.
 Higher the temperature greater will be rate of evaporation. Greater the surface area of liquid ,
greater will be rate of evaporation.
 Films and deposits formed during evaporation reduce the rate of evaporation. Higher the viscosity
of the slurry lowers the rate of evaporation and same is for the higher concentration of the solid.
Procedure:
Effect of SURFace area on rate of evaporation
1. Four beakers of different sizes (50, 100, 250 and 500 ml) are taken.
2. All beakers are thoroughly cleaned and weighed individually (Weight of individual beaker is denoted
W1).
3. Four different heating mantles are arranged and the temperature is set to 80°C.
4. 30 ml of water is placed in all the beakers.
5. All the beakers with water weighed individually and the values are recorded as W2.(beaker + water)
6. The beakers are placed on heating mantles and heated for 30 minutes.
7. AGer 10 min all the beakers are cooled carefully.
8. AGer cooling again all the beakers are weighed individually and the weights are recorded as W3.
9. Difference in initial and final weight is determined and the weight of water evaporated is noted.

10. Radius, Surface area of beakers and the rate of evaporation is calculated by using respective
formulae.
11. A graph is plotted by taking surface area of the beakers on X axis and rate of evaporation on Y axis.
12. The effect of surface area on rate of evaporation is noted
Effect of concentration on rate of evaporation:
1. Six beakers of same size is taken.
W1).
3. Six different heating mantles are arranged and the temperature is set to 80°C.
4. Different concentrations of NaCl (2%, 4%,6%,8%,10% and 20%) is prepared
5. 50 ml of prepared solution is transferred in the beakers.
6. All the beakers with solution weighed individually and the values are recorded as W2.(beaker +
Solution)
11. Rate of evaporation is calculated by using respective formula.
12. A graph is plotted by taking concentration of solution (%)on X axis and rate of evaporation on Y axis.
13. The effect of concentration on rate of evaporation is compared.
Effect of VISCOSITY on rate of evaporation:
1. Five beakers of same size are taken.
W1).
3. Five different heating mantles are arranged and the temperature is set to 80°C.
4. Different concentrations of glycerin in 100 ml water (2.5%, 5%, 7.5%, 10 %, and 12.5 %) are
prepared in different beakers.
Glycerin (ml) Water (ml) Concentration % v/v
2.5 97.5 2.5
5 95 5
7.5 92.5 7.5
10 90 10
12.5 88.5 12.5

5. 50 ml of prepared solution is transferred in the beakers.
6. All the beakers with solution weighed individually and the values are recorded as W2.(beaker +
Solution)
11. Rate of evaporation is calculated by using respective formula.
12. The effect of viscosity on rate of evaporation is compared.

I) Effect of surface area on rate of evaporation
Time of heating:
Rate of evaporation = Quantity of water evaporated/ Time of heating in minutes
ObSERvation table:
ParameterS 50 ml 100 ml 250 ml 500ml
Radius of Beaker
Surface area of the beaker (cm2)
Weight of empty beaker W1(g)
Weight of beaker with water W2(g)
Weight of water before evaporation ( W2- W1) a (g)
Weight of beaker + water aGer evaporation (W3) g
Weight of water aGer evaporation ( W3-W1) b ( g)
Weight of water evaporated (a-b) g
Rate of evaporation (a-b/30) g/min

II) Effect of concentration on rate of evaporation:
Rate of evaporation = Quantity of water evaporated/ Time of heating in minutes
ObSERvation table:
ParameterS 2% 4% 6% 8% 10% 20%
Concentration of solution (%)
Weight of beaker with solution W2(g)
Weight of solution before evaporation ( W2- W1)
a (g)
Weight of beaker + Solution aGer evaporation
(W3) g
Weight of Solution aGer evaporation ( W3-W1)
b( g)
Weight of water evaporated (a-b)g

III) Effect of viscosity on rate of evaporation:
Observation table:
ParameterS 2.5 % 5% 7.5 % 10 % 12.5 %
Weight of beaker with solution W2(g)
Weight of water before evaporation (W2- W1) a (g)
Weight of beaker + water aGer evaporation (W3) g
Weight of water aGer evaporation ( W3-W1) b( g)
Weight of water evaporated (a-b)g

RESULT:
The effect of surface area, concentration and viscosity n rate of evaporation is studied and the findings
are, The rate of evaporation.............with surface area.
The rate of evaporation.....................with concentration.
The rate of evaporation.....................with viscosity.

1. What is rate of evaporation?
2. Explain evaporation process?
3. Enlist factors influencing rate of evaporation.

Aim: To study the effect of time on rate of crystallization

RequiremenTS:
ChemicALS: Potassium nitrate, water.
ApparaTUS/ INStrument: Thermometer, water bath, tripod stand, test tube, stop clock.
ReferENCES:
1. Chemical Engineering by Badger and Banchero; Mc Graw Hill publication, New York.
New York.
Principle:
 Crystallization is the process of forming a crystalline material from a liquid, gas or amorphous solid.
The crystals thus formed have highly regular internal structure, the basis of which is called the crystal
lattice.
 All crystallization processes are aimed at creating a supersaturated solution or melt. The super
saturation is the driving force under whose influence new crystals are formed and present crystals grow.
 For most substances, the solubility increases with increasing temperature.
Procedure:
Effect of time on rate of cryStallization
1. 75 gm of potassium nitrate is accurately weighed (W1 g).
2. 100 ml of water is transferred into 250 ml beaker.
0
3. Beaker containing water is placed in constant temperature water bath maintained at 50 C.
4. Potassium nitrate is added into the water little by little, the solution is stirred with glass rod to
dissolve the solute.
5. The process is continued until saturated (with little excess of solutes)solution is formed.
6. Weight of potassium nitrate remained as weighed (W2 g). Difference in the weight W= (W1-W2 gm)
gives weight of potassium nitrate added into 100 ml water.
7. From this 10 ml of saturated solution are transferred into 9 beakers.
8. All beakers are placed into ice bath at once. Temperature of solution decreases suddenly due to
shock cooling forming supersaturated solution. Nucleation and crystal growth takes place.
9. AGer 10 minutes the solution of first beaker is filtered to collect the crystals.

10. This is repeated aGer 10 minutes thereaGer using the solutions of remaining beakers.
11. Al the crystals collected on the filter paper separately and are subjected for drying using dryer.
12. Weight of each sample of crystals is recorded.
13. A graph is plotted taking time on X axis and % weight of crystal on y axis.
ObSERvation table:
Time Weight of cryStal formed % Weight of cryStALS

(min) ‘b’ b/a X 100
10
20
30
40
50
60
70
80
90
a= weight of potassium nitrate present in 10 ml of water (Theoretical weight)
RESULT: The effect of time on rate of crystallization is ‐‐‐‐‐‐‐

1. What is crystallization?
2. Enlist the stages of crystallization.
3. Write the objectives of crystallization.

Aim: Steam distillation:- To calculate the efficiency of steam distillation

ReferENCES:
New York.
RequiremenTS:
ChemicALS: Turpentine oil.
ApparaTUS/ INStrumenTS: Distillation flask, steam generator, condenser, separating funnel, double
holed rubber cork, measuring jar, thermometer, bent tubes, weighing balance/weights etc.
Principle:
Steam distillation is a process used for separation of high boiling point substances from non- volatile
impurities. Important application of Steam distillation is high boiling point liquids can be distilled well below
their boiling points. It is the way of separating miscible liquid based on their volatilities. The boiling point of
products is minimized, permitting the constituents to be vaporised. The efficiency of Steam distillation is
effective than the simple distillation. Steam distillation is especially used for the separation of volatile oils at
low temperatures without decomposition.
ApplicaTIONS
 It is used in the isolation of essential oils, for use in perfumes.
 It is also useful to separate intermediate or final product during synthesis of complex compounds.
 It is widely used in petroleum refineries and petrochemical plants commonly referred as steam
stripping.
 It is also important in separation of fatty acids.
Procedure:
1. 30 ml of turpentine oil and 70 ml water is measured and transferred into distillation flask.
2. The flask is closed with two holed rubber cork and thermometer is inserted through one of the
holes and fixed.
3. Through the other hole, a bent tube of steam generator for the steam is fixed to pass into the
distillation flask.
4. Ensured the bent tube is reach almost near bottom of the flask but not touching the flask.

5. The side tube of the neck of the distillation flask is fixed to the condenser.
6. Further, the steam is allowed to pass into the distillation flask continuously from the steam generator.
7. The mixture gets heated. AGer some time it starts boiling.
8. The temperature T1 at which boiling occurs is noted.
9. Steam carries the vapour of oil and passes into the condenser where condensation takes place.
10. Condensate is collected into receiver for 15 minutes.
11. Oil is separated from water using separating funnel and volume / weight of oil and water is noted.
Experimental SEtup for Steam DIStillation
ObSERvaTIONS and CalculaTIONS:

Molecular weight of water: 18.016 (MW)
Molecular weight of turpentine oil: 276.283 (Mt)
o
Boiling point of mixture starts: 95.6 C
o
At 95.6 C vapour pressure of water: 647 mm of mercury (Pa)
Atmospheric pressure: 760 mm of mercury
o
Vapour pressure of turpentine oil: Atmospheric pressure- vapour pressure of water at 95.6 C
760 – 647 = 113mm of mercury (Pb)
Volume of the water in distillate: =
Volume of the turpentine oil in distillate: =
o
Density of water = 1 g/ml at 25 C
o
Density of the turpentine oil = 0.86 g/ml at 25 C
Weight of water aGer distillation (Wa) = volume of water X density of water = --------gm

Weight of turpentine oil aGer distillation (Wb) = volume of oil X density of oil = ---------gm
Practical yield = Wb /Wa
Theoretical yield:
Practical yield
Percentage efficiency of steam distillation X 100
= Theoretical yield

Percentage efficiency of steam distillation
=

1. Explain the principle of steam distillation
2. What are the applications of steam distillation
3. At what temperature organic liquids in steam distillation vaporize?
4. What type of substances are separated using steam distillation?

Aim: To determine Overall Heat Transfer Coefficient of water by heat exchanger.

ReferENCES:
New York.
RequiremenTS:
ApparaTUS/ INStrumenTS: Steam generator, glass condenser, measuring cylinder, Glass bottle, collecting
bowel, Thermometer, Bent tube, etc.
Principle:
When the feed of hot fluid is passed through one end of the apparatus and the cold fluid is passed through
the other end, this arrangement is known as counter current or counter flow method. Heat flow through
fluids takes place by heat convention. The rate of heat transfer through the fluids is determined using the
Overall Heat Coefficient of Liquids. i.e. the rate of heat transfer, Q= U At
The water condenser used in the laboratory for distillation is an best example for the counter current flow
of liquids and heat transfer. Thus, overall heat transfer coefficient is determined using water condenser.
The overall heat transfer co-efficient of a glass tube is mathematically expressed for a counter current
flow is U = Q / A  t
Where,
Q = Amount of heat transferred , W(J/s)
2
U= Overall Heat transfer co-efficient W/m .K
2
A = Surface area across which heat exchange takes place, m
t= Temperature drop
Where heat is transferred through steam to cold water through a glass surface, the total amount of heat
transferred is equal to either heat lost by steam or heat gained by water.
m1= mass of steam
t1= temperature drop between steam and
water S1= specific heat of water
L= Latent heat of vaporization of steam

The amount of heat lost by steam, (q1) = m1 s1 t1 + m1 L
Similarly, the amount of heat gained by circulating water (q2) = m2
s2 t2 Where m2 =mass of water circulated
S2 =specific heat of water
t2 = temperature rise
Average rate of heat transfer (Q) q1 + q2
= 2
t in the equation (1) is obtained by LMTD for counter current flow

ApplicaTIONS:
 Heat exchangers are used in many industries including, refrigeration, water waste treatment, wine
and beer making, petroleum refining, etc.
 In commercial aircraG they are used to take heat from engine's oil system to heat cold fuel.
 In pharmacy it is useful in crystallization, evaporation, distillation, etc.
Procedure:
1. A steam generator is selected and ensured for no leakage. Sufficient quantity of water is filled in it.
2. Condenser which is having the facility of circulating distillation column is selected.
3. Bend tube of steam generator is connected to the inlet of condenser tube.
4. The outlet of the condenser tube is connected to a collecting bowel in which condensed water is to
be collected.
5. Circulation of cold water around the inner tube of condenser is arranged by connecting it to a water
tap.
6. The outlet of the inner tube of the condenser is connected to water collecting drum.
7. Ensured that all connections are properly made before applying heat to generate steam.
8. Water in the steam generator is now heated and ensured the passage of steam through the
condenser tube.
9. The condensation process is allowed to continue for about 5 minutes.
10. Further the water circulation is stopped from inner tube of the condensate by stopping tap water
and put off the heating of water by means of putting off steam generator.
11. The circulating water from the exit and condensate are separately collected properly, avoiding
spillage.
12. The temperature of steam and condensate is noted, the difference gives the temperature drop 't1'.
13. The temperature of water at exit and entrance points are noted and difference gives temperature
rise 't2' for equation.
14. Volume of collected condensate is measured. (m1)
15. Volume of water collected is measured (m2)
16. Average rate of heat transfer (Q) using above equation is calculated and Overall Heat transfer Co-

efficient (U) determined.
17. Entire experiment is repeated by changing the speed of water.
18. Overall Heat Transfer Coefficient for this repeated experiment is also determined.
Average rate of Overall Heat Transfer Co-efficient is calculated by means of using following equation.
Average rate of heat transfer (Q) = q1 + q2
2
Experimental SEt up for determination of overall heat trANSfer co‐efficient
ObSERvaTIONS
I:‐ The amount of heat LOSt by Steam “q1” IS ,
“q1” = m1s1t1+ m1 L =
m1= mass of steam or condensate
= T1 = temperature of steam =
T2 = temperature of condensate =
t1 = temperature drop between steam and water
= s1 = specific heat of water = 4190 J/Kg
L =latent heat of vaporization of steam = 226.1 J/Kg
“q1” = m1S1t1+ m1 L =

II:‐ Amount of heat gained by circulating water “q2” IS
“q2” = m2s2t2
m2= mass of water circulated
= s2 = specific heat of water =
T1 = exit temperature of water =
T2 = temperature of water at inlet
= t2 =temperature rise =
“q2” = m2S2t2
Average rate of heat transfer (Q) = q + q

1 2
l = length of the condenser

= A = area of condenser =
2rl r = radius of
condenser
Overall heat transfers Co-efficient:
RESULT:
Overall heat transfer co-efficient “U” is = -----------

1. Name the various types of heat exchangers
2. What is the difference between counter current flow and parallel heat exchangers
3. Enlist different applications of heat exchangers.
4. Define heat exchanger.

Aim: To determine the radiation constant of Iron.

References:
Introduction to Chemical Engineering by Badger and Banchero; Mc Graw Hill publication, New York.
New York.
Requirements:
Apparatus/ INStruments: Iron cylinder with hole or cavity, thermometer, glass tripod stand/ wooden slab,
iron tripod stand, Bunsen burner, gas cylinder, match box or gas lighter, weighing balance, screw gauge and
tongs, etc.
Principle:
Heat transfer is a major unit operation in pharmacy. Heat flows from a region of high temperature to a
region of low temperature. Heat may flow by one or more of three mechanisms viz. Conduction, convection
and radiation.
Heat is lost from hot metal cylinder surface to surrounding atmosphere by means of conduction and
radiation. Heat transfer by radiation occurs, energy transfer through space by means of electromagnetic
radiation (waves). Thus a body acts as an emitter, than energy being transmitted through the intervening
spaces, and it is effective even in a perfect vacuum or inter-spacious space. The amount of thermal energy
radiated by a surface is increased rapidly with increasing temperature, when a heat flows by actual mixing
of warmer portions with cooler portions of the same material .This mechanism is known as Convection
A freely suspended body looses heat by conduction, convection and radiation until it reaches room
temperature. This is an equilibrium condition. The present experiment demonstrates the pattern of cooling
of hot body by combined convection and radiation. In this system, the heat loss through convection is
neglected, since movement of molecule is negligible. As the metal cylinder is freely suspended without any
contact with the metal the heat loss through conduction is minimum. For this reason, the metal cylinder is
placed on a glass tripod stand. Thus heat loss by radiation is highlighted. In conduction, the energy transfer
occurs by transmission of momentum of individual molecules.
The total amount of radiation emitted by black body may be calculated using Stephan Boltzman
4
law: q= b A T
where,
q = Energy radiated per second, W(or J/s) A = Area of radiating surface,
2 2 4
m T = Absolute temperature of radiating surface, K b = Constant, W/m .K
According to above equation the rate of heating depends upon the temperature and surface area of the
emitter. At the same time it also depends upon the absorption capacity of the material to be heated.
The difference in the temperature of hot body and the ambient is the temperature gradient for the heat loss
by radiation. The radiation constant is calculated using the following equation:
Where,
M= weight of cylinder (g)
S = specific heat of metal (iron), J/kg.K
= temperature gradient (rate of change of temperature, K/sec)
T1 = temperature of metal , K
T2 = room temperature, K
β = convection constant = 2.8
2
A = surface area of the cylinder in m
2 4
α = radiation constant (W/m .K )
Procedure:
1. A metal (iron cylinder) whose surface is smooth is cleaned and weighed on weighing balance and
average weight is recorded in the observation table.
2. The diameter and height of cylinder are measured and radius of the iron cylinder is calculated and
recorded in the observation table.
3. The thermometer is placed into cavity of iron cylinder and fixed to a stand using a thread (A simple
o
360 C thermometer can be used).
4. The iron cylinder is placed on tripod stand and heated with the help of Bunsen burner or with
o
heating device to above 300 C.
5. AGer reaching a constant maximum temperature, the metal cylinder is readily transferred to the
glass tripod stand / wooden slab using long tong without touching any surface.
6. Slowly the temperature of hot body decreases. The decrease in temperature is noted every 5
minutes interval and data is recorded in observation table.
7. A graph is plotted by taking time (minutes) on x- axis and temperature on y- axis.
8. Depending on the temperature at which the radiation constant is to be determined a tangent is
drawn at that temperature. The slope of tangent is calculated, which represents the rate of loss of
heat by hot body.
9. From the collected data the radiation constants is determined at specific temperature.

Experimental setup for determination radiation constant of metal cylinder
Graphical representation showing determination of slope
Graph: Influence of temperature on radiation constant

ObServations:
Parameters of metal cylinder:
Parameters of the metal Trial Average in Average in SI

cylinder 1 2 3 CGS system system
Mass of the cylinder “M” g
Diameter “d” cm
Height of the cylinder “h” cm
Radius of the cylinder “r” cm -- -- --
Surface area of the cylinder -- -- --

“A” =
o
Specific heat of iron “S” = 106 (at 25 C in J/kg.K)
Convection Constant “β” = 2.8
Room temperature, T2 =---------------K
Desired temperature T1 =---------------K
Slope =
Calculation for determination of “α” at particular temperaturES:

Use the following tables for tabulating the results:
Time Temperature Time Temperature Time Temperature

(minutes) (oC) (minutes) (oC) (minutes) (oC)

The radiation constant is calculated using the following equation:
RESULT:
Radiation constant “α” of Iron is =
Practical Questions (Assignment/Worksheet):

1. Explain the difference between absorptivity and emissivity
2. Define conduction, convection and radiation. Give one example of each.
3. State the Boltzman law of radiation heat transfer.
4. Define emissive power of body
5. Explain the principle involved in the determination of radiation constant of a metal.

Aim: To determine the radiation constant of Brass.

ReferENCES:
New York.
Requirements:
Apparatus/ INStruments: Brass cylinder with hole or cavity, thermometer, glass tripod stand/ wooden
slab, iron tripod stand, Bunsen burner, gas cylinder, match box or gas lighter, weighing balance, screw
gauge and tongs, etc.
Principle:
Heat transfer is a major unit operation in pharmacy. Heat flows from a region of high temperature to a
region of low temperature. Heat may flow by one or more of three mechanisms viz. Conduction, convection
and radiation.
Heat is lost from hot metal cylinder surface to surrounding atmosphere by means of conduction and
radiation. Heat transfer by radiation occurs, energy transfer through space by means of electromagnetic
radiation (waves).Thus a body acts as an emitter, than energy being transmitted through the intervening
spaces, and it is effective even in a perfect vacuum or inter-spacious space. The amount of thermal energy
radiated by a surface is increased rapidly with increasing temperature, when a heat flows by actual mixing
of warmer portions with cooler portions of the same material .This mechanism is known as Convection.
A freely suspended body looses heat by conduction, convection and radiation until it reaches room
temperature. This is an equilibrium condition. The present experiment demonstrates the pattern of cooling
of hot body by combined convection and radiation. In this system, the heat loss through convection is
neglected, since movement of molecule is negligible. As the metal cylinder is freely suspended without any
contact with the metal the heat loss through conduction is minimum. For this reason, the metal cylinder is
placed on a glass tripod stand. Thus heat loss by radiation is highlighted. In conduction, the energy transfer
occurs by transmission of momentum of individual molecules.
The total amount of radiation emitted by black body may be calculated using Stephan Boltzman
4
law: q= b A T
where,
q = Energy radiated per second, W(or J/s) A = Area of radiating surface,
2 2 4
m T = Absolute temperature of radiating surface, K b = Constant, W/m .K

According to above equation the rate of heating depends upon the temperature and surface area of the
emitter. At the same time it also depends upon the absorption capacity of the material to be heated.
by radiation. The radiation constant is calculated using the following equation:
Where,
M= weight of cylinder (g)
S = specific heat of metal (iron), J/kg.K
= temperature gradient (rate of change of temperature, K/sec)
T1 = temperature of metal , K
T2 = room temperature, K
β = convection constant = 2.8
2
A = surface area of the cylinder in m
2 4
α = radiation constant (W/m .K )
Procedure:
1. A metal (brass cylinder) whose surface is smooth is cleaned and weighed on weighing balance and
average weight is recorded in the observation table.
2. The diameter and height of cylinder are measured and radius of the iron cylinder is calculated and
recorded in the observation table.
3. The thermometer is placed into cavity of iron cylinder and fixed to a stand using a thread (A simple
o
360 C thermometer can be used).
4. The brass cylinder is placed on tripod stand and heated with the help of bunsen burner or with
o
heating device to above 300 C.
5. AGer reaching a constant maximum temperature, the metal cylinder is readily transferred to the
glass tripod stand using long tong without touching any surface.
6. Slowly the temperature of hot body decreases. The decrease in temperature is noted every 5
minutes interval and data is recorded in observation table.
7. A graph is plotted by taking time (minutes) on x- axis and temperature on y- axis.
8. Depending on the temperature at which the radiation constant is to be determined a tangent is

drawn at that temperature. The slope of tangent is calculated, which represents the rate of loss of heat
by hot body.
9. From the collected data the radiation constants is determined at specific temperature.

Experimental SEtup for determination radiation cONStant of metal cylinder
Graphical reprESENtation SHOWING determination of SLOPE
Graph: Influence of temperature on radiation cONStant

Observations:
ParameterS of metal cylinder :
Parameters of the metal cylinder Trial Average in Average in SI

CGS system system
1 2 3
Mass of the cylinder “M” g
Diameter “d” cm
Height of the cylinder “h” cm
Radius of the cylinder “r” cm -- -- --
Surface area of the cylinder -- -- --

“A” =
o
Specific heat of Brass “S” = 370 (at 25 C in J/kg.K)
Convection Constant “β” = 2.8
Room temperature, T2 =-----------K
Desired temperature T1 =-----------K
Slope =
Calculation for determination of “α” at particular temperatures:

Time Temperature Time Temperature Time Temperature

(minutes) (oC) (minutes) (oC) (minutes) (oC)

Result:
Radiation constant “α” of Brass is =

1. What is thermal radiation?
2. Differentiate between conduction and convection
3. Define absorptive power of body.

Aim: Determination of radiation constant of glass (unpainted and painted)

References:
New York.
Requirements:
Apparatus/ Instruments: Round bottom flask along with neck (500ml), glass tripod stands, digital
thermometer, tong, painted (white green coloured) round bottom flasks with long neck.
Principle:
Heat transfer by radiation involves the transfer of energy in the form of electromagnetic waves. These
become significant at higher temperatures. All solid bodies radiate energy when there temperatures are
above absolute zero. The radiant energy emitted by a hot body is expressed by Stefan Boltzmann law which
states that the rate of radiation emitted by a body.
4
Q= b A T
Where,
Q = Energy emitted per second W (or J/s)
2
A = Area of radiating surface, m
b = absolute temperature of the radiating surface,
2 4
K T= constant W/ m .k
According to above equation, the rate of heating depends on the temperature and surface area of the
emitter. At the same time, it also depends upon the absorption capacity of the material to be heated.
by radiation.
Radiation constant α is calculated using the following equation:
Total heat lost by the body = heat loss due to radiation + heat loss due to convection
OR
Radiation constant α is calculated using the following equation:

Where,
M1= mass of water W (Kg)
M2= mass of round bottom flask (unpainted / painted),
kg S1 = specific heat of water, J/Kg. K
S2= specific heat of glassr, J/Kg. K
T1= Temperature of metal body, K

T2 = Temperature of ambient (room temperature) K
β = convection factor
2
A = surface area of the heat transfer m
2 4
α = radiation constant (W/m . K )
All the values are determined experimentally and substitute in above equation to determine α (radiation
constant)
The special feature of the heat transmission by radiation is that radiant energy penetrates to a certain
distance in the material. Beyond a particular point, heat transfer by radiation becomes ineffective. For this
reason, formation of surface skin must be avoided. When glass apparatus is painted with silver oxide, the
rate of radiation decreases because painting acts as insulation by radiation.
Heat transfer is a major unit operation. Heat flows from a region of high temperature to a region of low
temperature. Understanding of heat transfer requires study of the mechanism & rate of process. Heat may
flow by one or more of 3 basic mechanisms.
1. Conduction: it is a process in which heat flow in a body is achieved by the transfer of the
momentum of the individual atoms or molecules without mixing.
Example: Flow of heat through the metal shell of a boiler t6akes place by conduction as far as solid
shell or wall is considered. This mechanism is limited to solid & fluids.
2. Convection: It is a process in which heat flow in a body is achieved by actual mixing of warmer
portion with cooler portion of the same materials.
Example: Heating by water by a hot surface (coil type water heater) is mainly convection.
Convection currents are responsible for winds, land/ sea breeze, ocean currents etc.
3. Radiation: It is the process in which heat flows through spaces by means of electromagnetic waves.
Example: A black surface absorbs most of the radiation received by it, it will transfer such absorbed
energy quantitatively into heat.
Thermal radiation :
Heat transfer by radiation is known as thermal radiation. All solid bodies radiate energy when their
temperature is above absolute zero.

Application:
Radiation energy is used in different processes, where heat is necessary.
For example, drying solid is attempted using microwave radiation, IR radiation, etc.
Procedure:
1. A round bottom flask (unpainted) is cleaned & dried.
2. The weight of the flask is determined (M2, kg) & reported
3. The diameter (D) of the round bottom flask is determined & reported.
4. The diameter (d) of neck of the flask is determined & reported.
5. Boiled hot water is prepared & separately measured volume of hot water is transferred (M1). The
external surface of round bottom flask is thoroughly dried & cleaned. The flask with hot water is
placed on the tripod stand.
0
6. Thermometer (110 C) is dipped till the centre of the flask & tied at the top to an iron stand.
7. Slowly the temperature of the hot body (water) decreases. The decrease in temperature is noted
every minute. The data are recorded.
8. A graph is plotted by taking time on X axis & temperature on Y axis. Normally a curve is obtained.
9. Depending on temperature at which radiation constant is determined, a tangent is drawn at that
temperature. The slope is calculated. This parameter is related to the rate of heat loss (dq/dt).
10. Radiation constant is determined at that temperature.
11. The same procedure is repeated with round bottom flask painted with silver oxide white colour or
green colour.
Experimental SEtup for determination radiation cONStant of unpainted /painted GLASS

Precaution:
1. The glass surface should not be touched with hands white taking readings
2. The care should be taken while transferring hot water quantitatively into the round bottom flask.
Observation Table
Parameter of the glass apparatus for heat transfer
Parameter of the round Trial Average in CGS SyStem Average in SI

bo†om FLASK SyStem
1 2 3
Weight M1 (gm)
Diameter of the flask, D

(cm)
Radius of flask, r1 (cm)
Diameter of neck, d (cm)
Radius of neck, r2 (cm)
Height , h (cm)
Surface area, A
Volume of hot water transferred, M1 = ml or gm kg

Heat loss by convection, β = 2.8
Specific heat of water, S1= 4190 J/kg.
K Specific heat of GLASS, S2= 500 J/kg.
K
Slope =

Calculation for determination of “α” at particular temperatures:
Time Temp. Time Temp. Time Temp. Time Temp.

Min. o
C Min. o
C Min. o
C Min. o
C
Result:
Radiation constant of glass (painted and unpainted) is =

1. What is principle involved in the determination of radiation constant of glass.
2. What is the effect of painting on glass on the radiation constant.

Aim:‐ Description of construction, working and application of pharmaceutical machineries.

ReferENCES:
rd
2. Cooper and Gunn's Tutorial pharmacy by S. J. Carter
1) Tablet ComprESSION Machine
Tablets are being formed by compressing the granules by using the compression machine. Tablet formed in
compression machine by pressing the granules in die with lower and upper punch. Tablet formation takes
place by the combined pressing action of two punches (lower and upper) and a die. Now it is possible to
produce more than 500,000 tablets per hour due to deferent's innovations to tablet compression machines.
Principle of Tablet ComprESSION Machine:
In the tablet compression machine main principle is compressing of the upper and lower punch in a die
hole, the hydraulic pressure plays a key role. This pressure is transmitted unreduced through the static fluid.
Any externally applied pressure is transmitted via static fluid to all the direction in same proportion. It also
makes it possible to multiply the force as needed. If we increase the hydraulic pressure more compressing
force on tablet then it becomes harder.
Single punch tablet comprESSION machine

StagES of Tablet ComprESSION
Different StagES of Tablet ComprESSION PrOCESS:

Tablet compression process is divided into four distinct stages. These stages include filling, metering,
compressing and ejection.
Tablet comprESSING Stage
Filling Formulation is overfilled at the compressing station
Metering Overfill is removed
ComprESSION Tablet is formed by pressure of punches within die
Ejection Tablet is ejected from die
1. Filling:
The filling stage of tablet compression process involves transfer of raw materials into position for tablet
compression. These raw materials have undergone prior processing by wet granulation, dry granulation
(roller compaction), sizing or other process. The final formulation is then blended to yield a homogeneous
blend. The blend then flows to the compressing machine punch-die cavity. The punch die cavity is
composed of punch die and lower punch. The position of lower punch within the die determines the
volume of the punch-die cavity. This volume must be appropriately sized for the weight of granulation to be
compressed into tablets. The granulation is overfilled on the die table (turret) to ensure complete filling of
the punch-die cavity volume.
2. Metering:
The metering stage of the tablet compressing process involves removal of excess granulation from the
compressing machine. This stage enables the exact weight (volume) of granulation to be compressed into
tablets. The exact weight of granulation is controlled by the height of the lower punch in the die. The height
of

the lower punch is controlled by the metering cam (also called the dosage cam). The lower punch is raised
to the appropriate level in the die to provide the exact weight of granulation in the punch-die cavity. The
excess granulation is scraped from the surface of the die table. The metering stage is similar to the method
used to measure flour when baking a cake. A measuring cup is first over-filled with flour; then a knife is
used to scrape off the excess. The exact amount of flour is then leG in the measuring cup.
3. ComprESSION:
The compression stage of the tablet compressing process forms the tablet. This stage involves bringing
together the upper and lower punches under pressure within the die to form the tablet. As the punches
enter the compressing stage, the upper and lower punches move between two large wheels called pressure
rolls. These pressure rolls push the punches together to form the tablet. The distance between the upper
and lower punches determines the thickness and the hardness of the tablet. When the punches are close
together, a thin and hard tablet is created. When the punches are farther apart, the tablet made is soGer
and thicker. The proper balance of thickness and hardness determines the optimum roll distance for any
specific product. These adjustments are made while keeping the tablet weight constant.
4. Ejection:
The ejection stage of the tablet compressing process involves removal of the tablet from the lower punch-
die station. In this stage, the upper punch retracts from the die cavity and rises above the turret table. Then
the lower punch rises in the die, which in turn pushes the tablet upward to the top surface of the die table
and out of the die cavity. A scraper (also called takeoff scraper or tablet rake-off) then pushes the tablet off
the die table away from the compressing machine into the collection container.
2) Fluidized bed dryer
Drying is very much important for wet granules for compression into the tablet and for modifying the
characteristics of viscous and sticky materials. Drying is commonly the last step in unit process before
compression into tablet form and packaging.
Principle: Fluidized bed dryer is better known by name
because hot air (gas) or ambient air is allowed to flow
upward at high pressure through a perforated bottom of
vessel containing bed of particulate solids. At the same
time the solution of adhesive is sprayed into the container.
It makes the particles become granulating that contains
adhesive. Being of unceasing dry through hot air, the
moisture in the granulating is evaporated. The process is
carried out continuously. Finally it forms ideal, uniform
and porous granules.
The velocity of hot air is more than the settling velocity of
the granules/particles by which they remain suspended in
stream of hot air. This condition is called fluidized state.
The hot air surrounds every granule/particle and
completely dries them.

CONStruction: Two types of FBD are available, vertical and
horizontal which are made up of stainless steel or
plastic. Vertical type is used for batch drying and
horizontal is used for continuous drying. A detachable
vessel is placed at the bottom of dryer for loading and
unloading of material. This vessel has perforated mesh
through which hot air with high pressure is passed. Bag
filters are placed above the vessel for collection of dried
material.
Bag filterS: These are placed above the drying vessel for the recovery of particles and dried material. Various
features of theses filter bags are:
1. These are made of different types of material or fabrics- cotton, nylon, polyester, satin,
polypropylene.
2. These can bear high pressure of hot air or high flow rates
3. Durable construction
4. Good resistance to wear and abrasion
5. These are available in different pore sizes, thickness, fabrics, permeability.
6. Anti-static fabrics are also available.
7. These are available in different sizes which can easily fit in equipment.
Working: The material to be dried is placed in detachable vessel at bottom of the dryer. The air is
introduced from below through the prefilter, which is heated by means of heaters installed therein.
Simultaneously fan is also allowed to work. As the velocity of air is increased, the bed begins to expand and
further increase causes turbulent motion of particles called fluidization. The granules/particles remain
suspended in air stream. Later on, a state of pressure is reached at which frictional drag on the
granules/particles is equal to the force of gravity. The particles rise in stream of air due to high velocity of
gas, this condition is called fluidised state.
ASSEMBLING:
 Unclamp the fixing bolts of retarding chamber and allow it to rest on the trolley. Take out trolley
along with the retarding chamber.
 Check and certify the suitability of the clean finger bag.
 Fix the loops of the finger to the hooks of the shaker.
 Place the bag in between the retarding chamber and fluidization chamber.

 Clamp the retarding chamber on the body with fixing bolts.

OPERATION:
· Loading
 Load the bowl with material to be dried.
 Take the product uniformly in the bowl to avoid lumps.
 Move the product bowl below the retarding chamber keeping the window in viewing position.
 Position the bowl.
 LiG the bottom of the FBD by moving the jack handle to the opposite side and seal the trolley to the
retarding chamber
 Check and ensure that there is no leakage.
 Set the timer and switch on heating and fluidization, maintaining the desired inlet air temperature.
 Stop drying at intervals of specified in BMR and dedust the finger bag by shaking it.
 Take out trolley and rake the granules to avoid formation of lumps.
 Watch the fluidized flow through the Perspex windows.
 Continue heating till required outlet air temperature is achieved. Air-dry if mentioned in BMR
 Put off the heaters and bring the timer to zero.
Unloading
 AGer drying is complete put off the main switch
 Shake the finger bag vigorously and dust retarding chamber.
 Unlock and withdraw the bowl.
AdvantagES of fluidized bed dryer:
1. Thermal efficiency is 2-8 times than tray drier
2. It is available in different sizes having drying capacity in range of 5- 250 kg/hour.
3. Free flowing granules/particles are made.
4. It can also be used for mixing the material with high efficiency.
5. It can be used for both batch and continuous drying.
6. Loading and unloading of material is very easy due to detachable vessel
7. Higher drying temperatures than tray and truck dryer.
Wipe out the body of FBD retarding chamber, trolley & bowl by using a clean dry lint free duster. Further dry
by running FBD at 70°C (without material) for 15 minutes.
3) Fluidized Bed Coater‐ WurSter Coater‐ Pellet Coater Fluidized bed SPRay coating
Principle‐
An alternative approach to pan coatings that provides the mixing and drying characteristics required by the
film coating process is to use fluid bed technology. Fluid bed technology helps in achieving fast and uniform
coating using air to mix, coat and dry the substrate at the same time. This technology originated from fluid
bed dryers
used for wet powder material drying operation. Fluid bed equipment was modified to coat tablets as an
alternative innovation. With the help of spray nozzles granulating liquid or coating solution is sprayed to
produces granules or coating of particles respectively and then dried with hot air.The particles are liGed
from the bottom and suspended in air stream. This condition is called fluidized state. A fluidized bed is a
bed of solid particles through which hot air is passed at high pressure through air distribution plate/bottom
of container.
CONStruction and working ‐
Fluid bed coating equipment later became popular for coating multiparticulate systems such as beads and
nonpareil seeds. The figure below shows diagrammatic representation of the fluid bed coating process by a
bottom spray method which is widely used to film coat multiparticulate systems.
Bo†om Spray Fluid Bed Coating (WurSter
Coating) Bo†om Spray Fluid Bed Coating (WurSter Coating)

 The drying inlet air is passed upwards through the bottom perforated plate into the fluid bed
chamber.
 This air passes inside and outside of the central cylinder (Würster column), which houses a spray
gun perpendicular to bottom plate, and parallel to the Würster column.
 The air is taken out of the equipment from the exhaust filters mounted on the top of the equipment.
 The material to be coated is loaded in the fluid bed chamber and fluidized.

 The inlet air is maintained at a certain velocity and temperature to help in both fluidization of the
material as well as its drying during the coating operation.

 The height of the Würster column is adjusted such that pellets above the bottom plate (referred to
as the Down-bed) are pulled in the Würster column due to the Venturi effect and pass through the
liquid spray of coating solution from the spray gun positioned parallel to the column within.
 When the material being coated reaches the expansion chamber (referred to as the Up-bed), its
velocity drops and it falls by gravity around the Würster column and is then recycled back to the
coating zone by Venturi effect.
Examples of Fluid Bed Technology Processes Include:
WurSter Process (Bottom Spray)
 Most commonly used type of fluid bed process for multiparticulate coating.
 In this process, there is a concurrent (same direction) movement of powder particles or pellets and
liquid spray.
 The coating process occurs within the Würster column.
Granulator Process (Top spray)
 Most commonly used type of fluid bed process for granulation.
 In this process, there is a counter current (opposite direction) movement of powder particles or
pellets and liquid spray.
Rotor Process (Tangential spray)
 Originally designed for the preparation of granulates (pellets), this process has also become
adapted for the film coating of multiparticulates.
 In this process, the powder particles or pellets move in a helical fashion due to spinning rotor disk
on the bottom of the equipment. The liquid is sprayed within the moving powder or pellets.
The existence of these three processing concepts has resulted in the major suppliers of fluid bed equipment
offering all three as standard inserts for a basic fluid bed processing unit.

Application & PrOCESS :
 Pellets and Granules coating and drying of particulate materials.
 It is ideal for heat sensitive and non heat sensitive products in Pharmaceuticals, Biotech,
Nutraceuticals, Cosmetic, Chemicals, Biochemical, Food, Dairy, Confectionery, Agrochemical, Herbals,
Ceramics, Detergents and Pharmaceuticals Institutes.
The equipment is used in application for following process.
 Aqueous or Solvent based solutions or suspensions
 Enteric Release coatings
 Controlled release coatings.
 Fine particle coatings
 Active layering.
4 ) Fluidized Energy mill
Fluidized Energy mill, also known as micronizers, or jet mills is a type of mill that consist of a hollow toroid
which has a diameter of 20-200mm depending on the height of the loop which can be up to 2m. A size-
reduction unit depending for its action on collisions between the particles being ground, the energy being
supplied by a compressed fluid, (e.g., air or steam) that enters the grinding chamber at high speed. Such
mills will give a product of 5 mu m or less; they have been used for the fine grinding. Interparticle attrition
that happens inside the tube of fluid energy mill is the principle of size reduction. It operates by particles
impaction and attrition. A fluid or milling gas, usually air or inert gas is injected as a high pressure jet
through nozzles at the bottom of the loop. The powder particles in the mill are accelerated to high velocity.
The kinetic energy of the air plus the turbulence created causes inter particle (particle-particle collision) and
particle-wall contact resulting in particle size between 2 and 10 micrometer. The fluidized effect transports
the particles to a classification zone where the size classifier retains the particles until sufficiently fine to be
removed.
The particle size and share are determined by;
 The speed of air/inert gas
 Feed rate and size
 The configuration of the mill
 Design of the classifer
 The position of the nozzle
 The impact between the feed and air

Construction:‐
It consists of a loop of pipe,which has a diameter of 20 to 200 mm , depending on the overall height of the
loop
,which may be upto about 2 m .There is an inlet for the feed and a series of nozzles for the inlet of air or an
inert gas. It also has an outlet with a classifier which allow the air to escape but prevents the particles to
pass until they become sufficiently fine.
The Fluid Energy Process:
Fluid Energy Mills are compact, versatile machines used for a number of operations such as size reduction,
drying, blending, coati ng and chemical reacti ons involving at least one solid material.
Fluid Energy Mills eliminate the limitations in conventional grinding machines. In Fluid Energy Mill there are
no moving parts and no grinding media. A source of compressed air or gas or high pressure super heated
steam is used to run the Mill.
Working:‐
The air or inert gas is introduced with a very high pressure through the nozzles .Solids are introduced into
air steam through inlet .due to high degree of turbulence, impact and attritional forces occurs between the
particles.The fine particles are collected through a classifier . Fluid energy mill reduces the particles to 1 to
20 micron. To get a very fine powder, even upto five micron, the material is pretreated to reduce the
particle size to the order of 100 mesh and then passed through fluid energy mill.
Pharmaceutical USES of Fluidized Energy mill
 Fluidized energy is used in milling thermolabile materials
 It is the choice of mill when higher degree of drug purity is required
 Fluidized energy mill is used for the fine grinding of frits, Kaolin, Zircon, titanium and calcium,
alumina.
AdvantagES of Fluidized Energy mill
 The machine has no moving parts and thus the tendency of contamination due to wear of parts is
minimize.
 The equipment is easily sterilized.
 Small particle size (between 2 and 10) is usually obtained at the end of milling.
 Thermolabile materials/heat sensitive substances such as sulphonamides,vitamins and
antibiotics.can be milled with little degradation since the heat produced by the process is nullified by the
cooling effect of the expansion of the compressed gas.
DISADVantagES of Fluidized Energy mill
 Tendency of forming aggregates or agglomerates aGer milling.
 Generation of amorphous content due to high energy impact.
 Formation of ultra-fine particles
5) Dehumidifier
Principle‐ A dehumidifier is a bit like a vacuum cleaner: it sucks in air from your room at one end, takes the

moisture out of it, and then blows it back out into the room again. The moisture drips through into a
collection

tank that you have to empty, from time to time. How is the moisture removed? That is where a
dehumidifier is more like an air conditioning unit (sometimes called an air-con or HVAC, which stands for
heating ventilating air conditioning unit), which, itself, works a bit like a refrigerator.
The compressor cooling system is the most important part of the condensation dehumidifiers. It allows for
condensing the steam and lowering water contents in the air. At the heart of the cooling system lies a
compressor which compresses and pumps the refrigerant, forcing it to circulate around the whole system.
The higher the pressure gets, the more the temperature grows. A compressed refrigerant (in gaseous state)
is transferred by a pipe to the condenser, where it is cooled down. The heat of the refrigerant is received by
the air around the exchanger (condenser). The refrigerant changes its state from gas to liquid due to its
pressure and the temperature drop. A condensed refrigerant runs through the de-watering filter, which
absorbs the steam that could find its way into the drier when its manufactured or maintained. AGer passing
through the filter, the liquid runs through a throttle (a capillary or an expanding valve), whose flow
resistance causes a pressure difference, that makes the refrigerant expand and evaporate. The evaporation
process takes place in the evaporator
Operation‐
1. Warm, moist air is sucked in through a grille on one side of the machine.
2. An electric fan draws the air inward.
3. The warm air passes over freezing cold pipes through which a coolant circulates. (Note: We've
simplified this part of the machine quite a lot. It's like a mini air-conditioner or refrigerator endlessly
circulating coolant with a pump and compressor.) As the air cools, the moisture it contains turns
back into liquid water and drips downward off the pipes.
4. Now free of moisture, the air passes over a heating element (similar to the one in a fan heater) and
warms back up to its original temperature.

5. Warm, dry air blows back into the room through another grille.
6. The moisture that was in the air originally drips down into a collecting tray (or bucket) at the bottom
of the machine.
7. A plastic float in the machine rises upward as the collecting tray fills up.
8. When the tray is full, the float trips an electric switch that turns off the fan and switches on an
indicator light telling you the machine needs emptying.
Procedure steps to dehumidify room. How does it work?
1. Moist air is drawn in from the room through a duct.
2. The air moves past a large rotating wheel made of water-absorbing material, which removes the
humidity.
3. The air is drawn by a fan operated by an electric motor.
4. Dry air is blown back out into the room.
5. An air duct underneath is kept hot by an electric heating element (yellow).
6. The moisture-absorbing wheel rotates through the heated air space and has hot air blown past it to
dry it out.
7. The air is sucked past by a fan and electric motor similar to the one up above.
8. The hot, wet air is blown out through an exhaust duct.
The whole operation is controlled by thermostats and humidity sensors so you can make the room as hot
and dry as you wish. The black lines you can see on the right and bottom of the picture mostly show electric
circuits controlling the machine. The main room thermostat is at the top, shown in gray.
Applications in Pharmaceutical Industry:‐
During the processing stage, most of the medicines are in powdered form and are highly hygroscopic.
Excess of moisture absorption leads to organic corrosion, biochemical reactions and
micro-organism growth on the product. Dehumidifiers help in keeping the required humidity parameters
for processing, drying, storing and transportation of medicines.
6) Hot air oven:
Principle
Sterilizing by dry heat is accomplished by conduction. The heat is absorbed by the outside surface
of the item, and then passes towards the centre of the item, layer by layer. The entire item will eventually
reach the temperature required for sterilization to take place. Dry heat does most of the damage by
oxidizing molecules. The essential cell constituents are destroyed and the organism dies. The temperature
is maintained for almost an hour to kill the most difficult of the resistant spores.
Construction:
Hot air oven is consist of double walled chamber of aluminium or stain less steel separated from the outer
case by a thick layer of insulation made up of fibre glass. Insulation is also filled in the hollow flanged door,
which carries an asbestos jacket that provides a tight seal. Heating is affected by a electrical heating
element and
thermostat automatically control temperature.
Temperature and time relation for hot air oven
Temperature( C) Time (h.)
140 3
150 2.5
160 2
170 1
180 0.5
Diagram:
7) Autoclave (MOISt Heat Sterilizer)

Autoclaves of different sizes from 5 litres to several hundred litres capacity are available in horizontal or
vertical designs.
CONStruction:
An autoclave have a body, an internal heating system, a container to hold material, its cover fixed with
pressure gauge, safety valve, pressure release valve etc. Lid is tightened with the help of screws and a
gasket seals the body and lid. A jacket, paddle liGer, timer, and indicator etc., are also provided with large
sized autoclaves. Autoclaves may be constructed of aluminum, mild steel, stainless steel or gun metal.
Industrial autoclave can
accommodate large trolley containing huge number of glassware's or large bioreactors.
Principle:
Moist heat destroys microorganisms by the irreversible denaturation of enzymes and structural proteins.
When water boils when its vapour pressure equals to that of the surrounding atmosphere. Hence in this
way steam is a gas, increasing its pressure in a closed system increases its temperature. As the water
molecules in steam become more energized, their penetration increases substantially. Saturated steam has
greater penetration power. When steam comes in contact with cooler surface it condenses to water and
gives up latent heat to that surface. The condensed water ensures moist condition for killing the microbes
present.
It is important to note that the sterilizing agent is the moist heat, not the pressure.
Diagram:
Temperature and time for autoclave

Pressure(lb/sq. inch) Temperature (C) Holding Time(min.)
10 115.5 30
15 121.5 20
20 126.5 15

Procedure:
 Pack the object to be sterilised in a material which does not create any obstacle for steam
penetration and removal of air. Pack the material in tubes, bottle and close with cotton stopper, flask
plugged with cotton or loosely applied screw cap. Wrapping cloth or plastic or KraG paper may be used for
wrapping the instrument.
 Place sufficient water upto the required level in the chamber and place the material on the
perforated tray just above it.
 Close the door to seal it completely. Open the manual discharge tap and start heating. Adjust the
safety valve to required pressure. The steam-air mixture is allowed to escape freely till all the air has been
displaced.
 Close the discharge tap and wait till the pressure is reached to the required level. When the holding
period is over, turn off the heater and allowed it to cool till the pressure on the gauge is equal to
atmospheric pressure. Open discharge tap slowly and the air allowed to enter in the autoclave. Finally open
the autoclave and unload.
PrecAUTIONS:
1. Check water level each time, the heating elements should remain immersed in the water.
2. Check spring of safety valve frequently and clean opening whenever necessary.
3. Opposite screws of the lid should be tightened simultaneously.
4. Do not over tighten the screws to avoid damage to the gasket
AdvantagES
1. Microorganisms are destroyed more efficiently by stearm sterilization than by dry heat sterilization
because of greater penetration power.
2. Method applicable to wide variety of material and for large lodge.
3. Spores are easily destroyed.
4. Nontoxic to patient, staff, environment.
5. Cycle easy to control and monitor.
DISADVantagES:
1. It is unsuitable for sterilization of powders and oils.
2. It cannot be used for sterilization of injections and articles, such as, plastics which get spoiled at 115-
0
116 C for 30 minutes.
3. Cannot be used for thermo labile material.
Application
1. The method is used for sterilization of surgical dressing and surgical instruments.
2. The containers and closures are sterilized by autoclaving.
3. It is used for the sterilization of a majority of official injections which can withstand the pressure of
15 lbs/sq.inch for 30 minutes.
Aim: Demonstration of Colloidal Mill, Planetary mixer, Fluidized bed dryer and Freeze dryer
References:
rd
2. Cooper and Gunn's Tutorial pharmacy by S. J. Carter.
Requirements:
Apparatus/ instruments: Colloidal Mill, Planetary mixer, Fluidized bed dryer and Freeze Dryer.
1. Colloidal Mill
Colloidal Mill is used to reduce the particle size of a solid present in different liquid forms or solid
forms of the pharmaceutical ingredients in pharmaceutical industry. Colloidal Mill reduces the size of
particles of solids that are suspended in a liquid, when a liquid suspended in another liquid, meaning that
they are immiscible, this machine is used alternatively to reduce the size of droplet.
Basic Parts:
It consists of an inlet hopper which is used to feed the material into the mill. It consists of a rotor and stator
which are used to reduce the particles size by applying the shearing force along with an outlet which is used
to discharge the reduced particles.
Construction:
A colloidal mill consists of a high speed rotor and a stator with conical milling surfaces between which is an
adjustable clearance ranging from 0.002 to 0.03 inches. The rotor speed is 3000 to 20000rpm. The material
to be ground should be pre milled as finely as possible to prevent damage to the colloidal mill. Rough
surfaced mill add intense eddy current, turbulence and the impaction of the particles to the shearing
action.
Principle:
The size reduction is affected due to shearing, when the material is passed between the narrow gap of
milling surfaces of rotor and stator. A rotor turns at high speeds of 3000 – 20000rpm. The high levels of
hydraulic shear applied to the process liquid disrupt structures in the fluid. The rotor and stator surface
covered with metal toothed coverings which cut and shear the solid. Higher shear rates leads to smaller
droplets of 1 micron. Based on a rotor rotating at high speed and very close to a conical stator, the particle
size is done by modifying the gap between the rotor and the stator.
Working of the Colloidal Mill:
The material is placed into the mill though the inlet hopper. It is then passed through the narrow gap
between the rotor and stator and thus reduced the fine particle size. A colloid mill is a hydraulic shear
producing device. The colloid mill works to reduce the size of the suspended droplets. The mill allows the
solid particles to become so small. The process of colloid milling is done through the addition of the heavier
liquid into the chamber of the mill that performs the shearing process. Once the heavier liquid has been
added the lighter material whether it

is a solid mass or a liquid of different viscosity is added to the material to start the mill. When the milling
portion of the function takes place, the materials are both stirred together within the mill at a high rate of
speed. In other model the stator remains constant and the rotor will do the function of rotation. It creates
the amount of hydraulic shear needed to break down the materials.
Colloidal mill
Pharmaceutical Applications:
1. The main use of a colloid mill is the dispersion of solid particles within a liquid.
2. It is frequently used to increase the stability of suspensions and emulsions.
3. It is used for the efficient emulsification, homogenization, dispersion and mixing during the course
of cutting, milling and shocking with high frequency.
4. It is used to reduce the particle size in suspension in a liquid or to reduce the droplet size of a liquid
suspended in another liquid. By applying high levels of hydraulic shear to the process liquid the
reduction is done.
5. Particles size of as small as 3 microns can be obtained by the colloidal mill.
6. Fibrous materials can be milled using rough surfaced rotor and stator.
2. Planetary Mixer
The single planetary mixer is used for mixing of dry and wet powders, light pastes, gels, and doughs. This
mixer is very popular in the food and bakery industry because of the simple construction, operation, and
relatively lower cost.
Construction & Operation
Planetary Mixer

The planetary mixer is so named because the mixing blade (commonly known as the beater) rotates in a
planetary motion inside the mixer bowl. The bowl of the single planetary mixer consists of an upper
cylindrical section and a lower hemispherical section. The mixer bowl is secured to a semi-circular frame
(also termed as “fork") at the time of mixing. The beater profiles are shaped to match the lower curved
surface of the bowl. The beater has two types of movements: it revolves on it own vertical axis at high
speed. At the same time, this vertical axis rotates around the centre of the bowl at a relatively lower speed.
Single planetary mixers are relatively inexpensive, versatile, and can be constructed in a range of sizes. The
popular features of this mixer are the possible use of multiple bowls and beater designs with the same
mixer assembly.
AGer the mixing is completed, the bowl is lowered and can be easily detached and removed from the mixer
assembly. The mixer bowl can be removed by either lowering it beneath the beater, or raising the beater
above the bowl. The liGing and lowering of the bowl is through a manual arrangement for small size mixers.
For larger units either the bowl is lowered beneath the motor or the drive system along with the beater is
raised above the bowl, using a motorized or hydraulically operated mechanical arrangement. The bowl can
be moved away from the machine using a suitable trolley with wheels.
The single planetary mixers are available in small sizes suitable for home kitchens to production size units
with capacities of 300 litres. The mixer motor may range from fractional horse power ratings for smaller
sizes to about 10 – 15 HP for the 300 litres mixer, depending on the material to be mixed.
Applications
The single planetary mixers with removable bowls is universally used in the food and bakery industry as they
are capable of preparing most batters and doughs, and they are oGen used for adjuncts such as icings.
The applications of the single planetary mixer are also common in the pharmaceutical, chemical, refractory,
and cosmetic industries.
3. Laminar flow: (Laminar Air Flow)

The air supplied to clean room must be filtered through High Efficiency Particulate Air (HEPA) Filter. The
HEPA filter must be positioned at the inlet to the clean room and pre-filters must be fitted upstream of the
HEPA filters to prolong the life of the final filter. Pleated fibre glass paper is used as filer medium. The filter
consists of a continuous sheet of filtration material, pleated with a corrugated separator in the HEPA filter.
Laminar air flow equipment can deliver clean air in a vertical, horizontal or curvilinear direction. Room air is
sucked into the equipment and passes through a pre-filter which removes large- sized air contaminants. A
blower then forces the pre-filtered air through a second filter system in the laminar air flow unit called a
High Efficiency Particulate Air (HEPA) Filter. The air emitted from laminar air flow equipment is claimed to
be 99.97% free from microbial contamination. This level is based upon the removal of dioctylphthalate
particles of size 0.3 μm and larger. The velocity of HEPA filter air is measured using an air velometer. Air
velocity at all parts of the filter should be 90 ±20 feet per minute (0.54 m/sec).
Quality control procedures must be adopted to evaluate and monitor the quality of laminar air flow. Air
qualities is evaluated using particle counter, microbial air samplers and settle plate techniques. The
efficiency of the HEPA filter is valuated by employing the Dioctylphthalate (DOP) TEST. This is a challenge
test for HEPA filters. Dioctylphthalate is volatile liquid which converts to a vapour or smoke, under pressure

having a size range 0.3-

0.4 μm. The DOP smoke is introduced at the supply plenum. A photometer probe scans the HEPA filter
surface and checks the leakage in the filter. Presence of DOP smoke is detected by the photometer. Sensors
are filled upstream and downstream of the filter to indicate the pressure differential across the filter. Alarm
system should be used to indicate failure in the supply or blockage.
NotES:
1. HEPA filter is not used for sterilization of a contaminated objects. It is only to maintain sterility or
cleanliness of an already sterile or clean object.
2. All surfaces of the laminar air flow must be disinfected before placing any item inside the hood.
3. All material must be disinfected/ sterilized prior to introducing such material onto the surface of the
laminar air flow workbench
4. Use the Ultraviolet rays for sterilization of surface of laminar air flow, before and aGer use. Don't
work in presence of UV Light.
5. Traffic in the area of workbench should be minimized and controlled.
6. All supply items should be arranged so that the work flow will provide maximum efficiency and order.
7. Laminar air flow should be certified and validated every 6 to 12 months.
Diagram :Vertical Laminar air flow bench

Diagram :Horizontal Laminar air flow bench
4. Freeze Dryer
Freeze dryer and lyophilizer are synonymous names for the same equipment. A freeze dryer executes a
water removal process typically used to preserve perishable materials, to extend shelf life or make the
material more convenient for transport. Freeze dryers work by freezing the material, then reducing the
pressure and adding heat to allow the frozen water in the material to sublimate.
Principle
The main principle involved in freeze drying is a phenomenon called sublimation, where water passes
directly from solid state (ice) to the vapor state without passing through the liquid state. The material to be
dried is first frozen and then subjected under a high vacuum to heat (by conduction or radiation or by both)
so that frozen liquid sublimes leaving only solid, dried components of the original liquid.
Working
Freezing Phase
Freeze dryers use various methods to freeze the product. Freezing can be done in a freezer, a chilled bath
(shell freezer), or on a shelf in the freeze dryer. The freeze dryer cools the material below its triple point to
ensure that sublimation, rather than melting, will occur. This preserves the material's physical form.
A freeze dryer most easily freeze dries large ice crystals, which can be produced by slow freezing or
annealing. However, with biological materials, when crystals are too large they may break the cell walls, and
that leads to less-than-ideal freeze drying results. To prevent this, the freezing is done rapidly. For materials
that tend to precipitate, annealing can be used. This process involves fast freezing, then raising the product
temperature to allow the crystals to grow.
Primary Drying (Sublimation) Phase
A freeze dryer's second phase is primary drying (sublimation), in which the pressure is lowered and heat is

added to the material in order for the water to sublimate. The freeze dryer's vacuum speeds sublimation.
The freeze dryer's cold condenser provides a surface for the water vapour to adhere and solidify. The
condenser also protects the vacuum pump from the water vapour. About 95% of the water in the material
is removed in this phase. Primary drying can be a slow process. Too much heat can alter the structure of the
material.
Secondary Drying (Adsorption) Phase
A freeze dryer's final phase is secondary drying (adsorption), during which the ironically-bound water
molecules are removed. By raising the temperature higher than in the primary drying phase, the bonds are
broken between the material and the water molecules. Freeze dried materials retain a porous structure.
AGer the freeze dryer completes its process, the vacuum can be broken with an inert gas before the
material is sealed. Most materials can be dried to 1-5% residual moisture.
Schematic diagram of Freeze dryer

Applications:
Pharmaceutical and Biotechnology
 Pharmaceutical companies oGen use freeze-drying to increase the shelf life of products, such as
vaccines and other injectables.
 By removing the water from the material and sealing the material in a vial, the material can be
easily stored, shipped, and later reconstituted to its original form for injection.
Food Industry
 Freeze-drying is used to preserve food and make it very lightweight.
 The process has been popularized in the forms of freeze-dried ice cream, an example of astronaut
food.
Technological Industry
 In chemical synthesis, products are oGen freeze- dried to make them more stable, or easier to
dissolve in water for subsequent use.
 In bio- separations, freeze-drying can be used also as a late-stage purification procedure, because it
can effectively remove solvents.
5. Spray drying

Spray drying is the transformation of feed from a fluid state into a dried particulate form by spraying the feed

into a hot drying medium. A spray dryer operates on convection mode. The principle of working is moisture
removal by application of heat to the feed product and controlling the humidity of the drying medium.
Spray dyer is composed of a huge round drying chamber with a small cone-shaped base made up of
stainless steel with the size of the drying chamber variations in between 2.5 to 9 m and also elevation is 25
m or even more. The spray disk atomiser is regarding 300mm in size and also turns at a rate of 3000 to
50000 changes each minutes.
Spray drying is a one-step steady system procedure that works with fluid atomization to generate droplets
that are dried to specific fragments when relocated in a warm aeriform drying form. A spray dryer is
composed of a feed pump, atomizer, air heating unit, air dispenser, drying chamber and also systems for
exhaust air cleansing and also powder recovery/separator.
A liquid feed entering the spray dryer undergoes a series of transformations before it becomes powder. The
changes are due to the influence of each of the four stages involved in spray drying, namely:
1. Atomization of the feed solution.
2. Contact of spray with the hot gas.
3. Evaporation of moisture.
4. Particle separation.
In the spray dryer the liquid to be dried is atomised into the good droplets, which are tossed readily into a
relocating stream of warm gas. The temperature level of the droplets is right away enhanced and also good
droplets obtain dried instantly through round fragments. This proces complets in a couple of secs prior to
the droplets get to the wall surface of the dryer. In the spray dryer the fluid to be evaporated is sprayed
through moisture. The min droplets are easily vaporized and also get turned into the solid fragments, which
are up to the bottom of the chamber. The vapours are moved into the separator in which the good drying
fragments that are brought together with the vapours are come apart and also gathered. Spray dryers are
readily available in several types and also deigns. A common spray dryer contain a drying chamber that is
similar to the cyclone separator, so in order to make sure the very good flow of an air to facilitate heating
and also mass transfer and to make sure that the dried fragments are divided by the centrifugal activity.
Process steps of spray drying. (1) Atomization. (2) Spray – hot air contact.

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1.

To evaluate size distribution of tablet granules by sieving method and construct

4. To dry calcium carbonate slurry and plot the drying curve.

13. To determine Overall Heat Transfer Coeﬃcient of water by heat exchanger.

14. To determine the radiation constant of Iron.

17. Description of construction, working and application of pharmaceutical

1 Pharmaceutical Engineering (SEM III)

2 Pharmaceutical Engineering (SEM III)

Mechanical Sieve SHAKer

3 Pharmaceutical Engineering (SEM III)

4 Pharmaceutical Engineering (SEM III)

5 Pharmaceutical Engineering (SEM III)

Practical QUESTIONS (ASSIGNMENt/WorkSHEEt):

7 Pharmaceutical Engineering (SEM III)

8 Pharmaceutical Engineering (SEM III)

9 Pharmaceutical Engineering (SEM III)

Degree of SIZe reduction Typical meTHODS ExAMPLES

Large pieces Cutter or compression mills Rhubarb

Coarse powders Impact mills Liquorice, cascara

Fine powders Combined impact and attrition mills Rhubarb, belladonna

Very ﬁne powders Fluid energy mills Vitamins and antibiotic

LawS governing energy and power requiremenTS of MILLS:

And from this can be derived the following laws:

9 Pharmaceutical Engineering (SEM III)

10 Pharmaceutical Engineering (SEM III)

11 Pharmaceutical Engineering (SEM III)

12 Pharmaceutical Engineering (SEM III)

Sieve Nominal Aperture Mean size Before size After size

Weight DIStribution AnalySIS of Sample – Before Size Reduction

Mean Weight of powder Per cent weight Wt. Size in (n *

Σn= 100 Σnd =

Mean diameter of the powder SAMPLE (before SIZe reduction), di = Σnd / Σn

13 Pharmaceutical Engineering (SEM III)

Σn= 100 Σnd =

Mean diameter of the powder sample (before size reduction), dn = Σnd / Σn

OBSERVATION AND CALCULATIONS

14 Pharmaceutical Engineering (SEM III)

BOND'S WORK INDEX:

di=Initial diameter of particle

RESULT & DISCUSSION:

15 Pharmaceutical Engineering (SEM III)

16 Pharmaceutical Engineering (SEM III)

22 Pharmaceutical Engineering (SEM III)

23 Pharmaceutical Engineering (SEM III)

Normality of oxalic acid solution, N1 =

 Preparation of SODIUM hydroxide (0.1 N) SOLUTION IP

Burette readings I II III

23 Pharmaceutical Engineering (SEM III)

Normality of sodium hydroxide solution,

Preparation of hydrochloric acid (0.1N) SOLUTION IP:

Standardization of hydrochloric acid (0.1N) SOLUTION IP:

Average volume, V3=…….

Normality of hydrochloric acid solution,

24 Pharmaceutical Engineering (SEM III)

Burette rEADINGS I II III

Average volume, x=…............ml

Average y=S(y -y)2=

Average y=S(y -y)2=