DRYING

DEFINITION
• ‘’A process in which the liquid is removed from a material by the
application of heat and is accomplished by the transfer of a liquid from a
surface into an unsaturated vapor phase’’
• This applies to the removal of small amount of water from moisture
bearing table salt as well as recovery of table salt from sea by
evaporation.

METHODS OF DRYING
• There are many non-thermal methods of drying:
1) Expression: of a solid to remove liquid.
2) Extraction: of liquid from a solid by use of solvent.
3) Adsorption: of water from a solvent by the use of desiccants.
4) Absorption: of moisture of gases by passing through sulfuric acid
(𝐻2 𝑆𝑂4 )
5) Desiccation: of moisture from solids by placing it in a sealed
container with a moisture Removing material, (silica gel in a bottle)

THEORY
• It is an important process in almost all the pharmaceutical industries.
There is hardly any pharmaceutical plant engaged in the manufacture of
tablets or capsules, that does not use dryers.
• Drying is commonly last stage of the process before packing and has a
considerable effect on the properties of the product which may prevent
the deterioration, produce a readily soluble or free flowing product.
• Drying involves both heat and mass transfer operation. Heat must be
transferred to the material to be dried in order to supply the latent heat
required for vaporization of moisture. Mass transfer is involved in the
diffusion of water through the material to the evaporating surface, in
the subsequent evaporation of water from the surface and in the
diffusion of the resultant vapor into the passing air stream.

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 • Drying involves:
- Heat transfer
- Mass transfer

HEAT TRANSFER
• Heat must be transferred to the material to be direct in order to supply
the latent heat required for the vaporization of the moisture, (phase
change). The rate of vaporization of the liquid film from the surface of
the material being dried depends upon:

dw q
=
dQ(t) λ

- Where, dw/dt = rate of evaporation, 1b of H2O/hr, q = overall

rate of heat transfer, λ = latent heat of vaporization of water.
• Heat transfer takes place by:
- Conduction
- Convection
- Radiation
• It means overall rate of heat transfer depends upon the sum of rate of
heat transfer by c, r, and k

S; q = qc + qr + qk
dw
= qc + qr + qr/pi
dt
- Where, qk, qc and qr are the rate of heat transfer by conduction,
convection and radiation, respectively.

MASS TRANSFER
• Mass transfer involves:
- Diffusion of water through the surface to the evaporation surface.
- The subsequent evaporation of water from the surface.
- The diffusion of resultant vapor into the passing air stream.
• Rate of diffusion of vapor into passing air stream depends on following
factors:
- Area of evaporating surface (A)
- Humidity difference (Hs-Hg)

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 So,

dw
∝ A (Hs − Hg)
dt
dw
= KA (Hs − Hg)
dt
- Hs = absolute humidity of surface, Hg = absolute humidity of air
- Where, K = coefficient of mass transfer, is not a constant but
depends upon volume of air stream passing over the surface as:

k ∝ V𝑛

k = C V𝑛

- Where, V = volume, C = proportionality constant, n = fractional

exponent.
• After the start of drying there will be a production of initial adjustment.
After that, the rate of evaporation of liquid from the surface is equal to
the rate of diffusion of liquid from the body of solids. Which depends on
rate of heat transfer. So, the rate of heat transfer becomes equal to the
rate of mass transfer.

qc + qr + qk = KA (Hs − Hg)
dw
Rate of diffusion = K′A (Hs − Hg)
dt
METHOD TO INCREASE RATE OF DRYING
• From the above equation we can increase the rate of by following ways:
- By increasing qC: the rate of convection heat transfer qC can be
increased by increasing the air flow rate and raising the air inlet
temperature.
- By increasing qr: the rate of radiation transfer can be speed up by
introducing the high temperature radiant heat source into the
drying chamber.
- By increasing qk: by reducing the thickness of material being dried
and by allowing it to come in contact with the raised temperature
surface.

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 - By increasing K: increasing the air volume also speeds up the rate
of drying by increasing the coefficient of mass transfer K.
- By increasing (Hs-Hg): if inlet air is determined, humidity gradient
can be increased which is other mean of speeding up the rate of
drying.

GENERAL CLASSIFICATION OF THE DRYERS

CLASSIFICATION BASED ON METHOD OF SOLID HANDLING
I. STATIC BED DRYERS
• Tray & Truck Dryers • Belt Dryers
• Vacuum Shelf Dryers • Drum Dryers
• Tunnel Dryers
II. MOVING BED DRYERS
• Turbo Tray Dryers • Vacuum Tumble Dryers
• Rotary Dryers • Pan Dryers
• Vibratory Conveyor
Dryers
III. FLUIDIZED BED DRYERS
• Vertical Dryers • Horizontal Dryers
IV. PNEUMATIC DRYERS
• Spray Dryers • Flash Dryers
V. SPECIALIZED DRYERS
• Freeze Dryer

CLASSIFICATION BASED ON HEAT TRANSFER MODE

I. CONVECTION
• Flash Dryer • Cabinet Dryer
• Spray Dryer • Tunnel Dryer
• Fluid Bed Dryer • Rotary Dryer
II. CONDUCTION
• Drum Dryer • Rotary Dryer
• Agitated Pan Dryer • Tray Dryer
III. RADIATION
• Infrared Shelf Dryer • Sun Dryer
IV. DIELECTRIC
• Microwave Oven • Radiofrequency Dryer
• Microwave Tunnel

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V. COMBINED MODES
• Microwave Convective Dryer
• Infrared Convective Dryer

1. STATIC BED SYSTEM

I. TRAY AND TRUCK OR SHELF DRYERS
• They are also known as cabinet or compartment dryers. There are
usually hot air ovens.

PRINCIPLE

• In these types of dryers there is no static relative movement among the

solid particles being dried. Only a fraction of a total number of particles
is directly exposed to the heat sources.
• The exposed surface can be increased by decreasing the thickness of the
bed.

DESIGN AND WORKING

TRAY DRYERS

• Tray dryers consist of a cabinet in which the material to be dried is

spread on trays. The number of trays varies with the size of dryer.
• Dryers of laboratory size may contain as few as three trays.

TRUCK DRYER

• Truck dryer is one in which the trays are located in trucks which can be
rolled into and out of the drying cabinet in pharmaceutical industries.
Truck dryers are preferred over tray dryers because of convenience in
loading and unloading the drying cabinets.

TYPES OF TRAY DRYERS

DIRECT DRYER

• Most tray dryer used in pharmaceutical industry are direct dryers, in

which heating is accomplished by the forced circulation of large volume
of heated air.

INDIRECT DRYER

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 • They utilize heated shelves inside the drying chamber to evaporate the
moisture which is then removed by vacuum pump. The preferred
energy source for heating the drying air used on pharmaceutical
products are steam or electricity. Steam is preferred over electricity
because steam energy is cheaper.

ADVANTAGES

• Drying by tray dryer is a batch process rather than continuous drying in

industry, batch drying is preferred because each batch can be dried
separately.
• Same equipment can be used for drying a wide variety of materials.
• Used for damp solid material drying.

DISADVANTAGES

• Only few particles are exposed to heat.

• Electricity cost is high.

II. TUNNEL DRYER

• It is a modification of tray dryer in which oven Is replaced by a long
tunnel.

OPERATION

• The material to be dried is entered at one end and the dried material is
collected at the other end of the tunnel. The trays containing the wet
material is loaded on trucks which have an automatic speed control.
• In the multiple belt conveyer system, the partially dried material which
has completed one side moves automatically from the end of 1st
conveyer on to the 2nd conveyer moving in opposite direction. In this
way the product may successfully travel five times along the tunnel
before its discharged at the other end of the tunnel.

ADVANTAGES AS COMPARED TO TRAY DRYERS

• It is semi continuous in operation and can be used for the large-scale

production.

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 2. MOVING BED SYSTEM
I. TURBO TRAY DRYERS
PRINCIPLE

• Drying particles are partially separated so that they flow over each
other. Motion may be induced either by gravity or mechanical agitation.

DESIGN AND WORKING

• Turbo dryer consist of a series of rotating angular

trays arranged in vertical stack. Heated air is
circulated over the trays by turbo-type fans. Wet
mass fed through the roof of the dryer and is leveled
by a stationary wiper. After about 7-8 of the
revolution the material being dried onto the tray
below where it is again spread and leveled. The
same procedure is continued throughout the height
of the dryer until the dried material is discharged at
the bottom.

ADVANTAGES

• Because turbo dryers continuously expose new surfaces to air, drying

rates are considerably faster than tray dryers.

DISADVANTAGES

• Expensive, Complicated.

II. ROTARY DRYERS

• The rotary dryer is modified form of tunnel dryer in which particles are
passed through a rotating cylinder, counter current to stream of heated
air. Due to the rotation of cylinder, the material is turned over and
drying takes place from individual particles and not from a static bed.
• The cylindrical shell is mounted with a slight slope so as to discharge the
material and make the operation continuous. Baffles or flights in the
shell may increase the rate of drying.

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 3. FLUIDIZED-BED SYSTEMS
• If a gas is allowed to flow upward through a bed of particulate solids at a
velocity greater than the settling velocity of the particles and less than
the velocity for pneumatic conveying, the solids are buoyed up and
become partially suspended in the gas stream.
• The resultant mixture of solids and gas behaves like a liquid, and the
solids are said to be fluidized.
• This is used for the granular solids because each particle is surrounded
by the drying gas.

PRINCIPLE

• Solid particles are partially suspended in an upward moving gas stream.

The particles are lifted and then fall back in a random manner, so that
the resultant, mixture of solid and gas acts like a boiling liquid and the
solid are said to be fluidized.
• This technique is very useful and efficient and it is used for drying
granular solids because each particle is surrounded by the drying gas.

TYPES OF FLUIDISED BED DRYERS

VERTICAL HORIZONTAL

• Used for batch drying. • Used for continuous drying.

DESIGN

• It consist of stainless-steel chamber

with a perforated bottom into which
the wet material to be dried is placed.
For loading and unloading, the drying
chamber is removed from the unit.
The air is introduced from below
which is heated by means of heaters
fitted there in and it is then passed
through the powder by means of fan
fitted in the upper part of the
apparatus.

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REQUIREMENT

• The requirement is that:

- Granules are not so wet that they stick together on drying.

WORKING

• The air is heated to the required temperature and its flow rate is
adjusted as the velocity of air is increased, the bed begins to expand.
• Further increase in velocity beyond this point will cause rapid expansion
of the bed and particles will begin to show turbulent motion.

FLUIDISATION

• The particles are not in direct contact with each other and efficient heat
exchange take place between the particles and the following air. The
moist air is carried away rapidly.

PURPOSE

• The purpose of this SOP is to describe the procedure to be followed

while operating the Fluid Bed Dryer to achieve the following objectives:
- To fulfill the GMP requirement.
- For personnel and machine safety.
- For efficient operation.
- To ensure proper washing and cleaning of equipment to produce
quality products.

SCOPE

• This SOP is valid for the Production department of SRP Plant.

PERSONNEL

• Wear mask, gloves and specified gown during all operations.

PRECAUTIONS

• During drying if lumps are observed, switch off the dryer. Take out the
trolley and paddle the product container, so to break the lumps and
level the product bed in the trolley.

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 • Observe that granules should not be over fluidized so as to avoid
attrition of granules.

STARTING

• Connect the air and electric supply.

• Load the Fluid Bed Dryer Bowl with product.
• The quantity should be appropriate for good fluidization.
• Introduce trolley into the space meant for it properly.
• Assure that bowl is well fitted in its space in the dryer.

RUNNING

• Adjust the drying temperature.

• Check that the product is completely fluidized then reduce the air flap
level until fluidization is just maintained.
• Observe that the granules are in fluidized state.
• If needed, press the shake device so as to maintain fluidization.
• Close the air flap and switch off the dryer, press shake device so if any
product that is remained in the filter should slide down into the trolley.
• Take out the trolley and observe the granules.
• Transfer the dried granules or material from Fluid Bed Dryer trolley into
polyethylene lined labeled drums.

ENDING (CLEANING)

• After completion of drying process, remove the trolley from dryer.

• Collect the dried granules in polyethylene lined labeled drums by means
of scoop.
• Clean and wash the trolley with hot water.
• Clean thoroughly inner and outer side of dryer with clean duster.
• In case of product change over, remove the filter ring and clean it.
• Wash the top and bottom of dryer thoroughly with hot water to remove
the traces of previous product.
• Also wash the trolley with hot water.
• Finally rinse with purified water.

ADVANTAGES

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 • They are efficient as 5-200kg material can be dried within 20-40 mins
compared with 24 hours in tray dryers
• Drying takes place from individual particles and not from whole bed
• The temperature of fluidized bed dryer can be controlled
• A free-flowing product is produced
• Due to short drying time unit has high output
• No caking or agglomeration
• Drying from all sides and not only surface.

DISADVANTAGES

• Complicated
• Skilled persons are required
• Too wet granules stick together
• Overheating causes brittle granules and tablet defects occur.
• Many organic powders develop electrostatic charges during fluidization
so efficient electrical earthing is necessary.

4. PNEUMATIC BED SYSTEM

SPRAY DRYERS
• They are used for drying only liquid materials such as solution, slurries,
pastes and suspensions.

PRINCIPLE

• In this method, the liquid is dispersed as fine droplets into a moving

stream of hot air, where they are evaporated rapidly before reaching the
wall of chamber. The product dries into a fine powder which is collected
into a collection system.

DESIGN

• All spray dryers consist of following components:

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 - Feed delivery system
- Drying chamber
- Solid gas separator
- Atomizer
- Heated air supply
- Product collector
- Cyclone

WORKING

• The liquid to be dried is fed to atomizer by use of suitable pump. The

rate of feed adjusted in such a way that each droplet of sprayed liquid is
completely dried before reaching the walls of drying chamber and yet
the dried powder is not overheated in the process.
• The inlet air temperature is kept constant. Too high temperature can
result in improper drying. Similarly, excessive feed rates will lower the
outer temperature due to which the material will be collected on the
walls of the chamber.
• The disc of atomizer D is driven by an air turbine and spins at 35000 rpm.
Air is introduced with help of fan which is heated by means of electric
heaters to a maximum temperature of 350℃. The spray droplets from
atomizer come in contact with the hot air.
• The droplets rapidly evaporate in the drying chamber. The dried powder
is separated from the gas in cyclone separator and collected in
container.

ADVANTAGES

• Liquid material can be dried

• Drying is very rapid and fast
• Thermostable substances can easily be dried
• Sterile solution can be dried
• The dried powder will have uniform particle size and shape
• Powder formed has good flow properties
• Labor cost are low
• Material up to 200 kg per hour can be handled.

DISADVANTAGES
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 • The equipment is very bulky and costly
• There is a lot of wastage of heat.

5. SPECIALIZED DRYERS
FREEZE DRYING
• It is process by which water is removed from the liquid product after it is
frozen by sublimation. Hence this is also known as FREEZE DRYING or
SUBLIMATION.

PRINCIPLE

• Liquid is first frozen to ice before application of vacuum to avoid

frothing, then sublimation of frozen ice is carried out under reduced
pressure.
• The vaporization of ice occurs only at the surface; hence the frozen ice is
exposed to large surface area.

PROCEDURE

• Freeze drying on large scale may be carried out by freezing the product
in a container kept on the shelf of a chamber by circulating a refrigerant
like ammonia or ethylene glycol from the compressor through the pipes
fitted along the series of shelf.
• When freezing is complete; vacuum is applied to the chamber which has
been previously chilled by means of circulating the refrigerant from
large compressor.
• Heat is then supplied to the product by heating coils. The process is
continued till the product is dry and a spongy solid material is left
behind which is collected in container.

APPLICATIONS

• For the manufacturing of certain pharmaceuticals or biological products

which are thermolabile.
• For drying blood plasma, vitamins, hormones, enzymes and antibiotics,
thus preserving these for years.
• Freeze dried products have definite physical properties as compared to
other products derived by other methods.

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 • Freeze dried products are more stable and are readily soluble.

DISADVANTAGES

• Slow process
• Very costly

6. VACUUM DRYERS
• Also known as vacuum oven. It consists of jacketed vessel. It has to
withstand vacuum in the oven and steam present in the jacket.
• Oven and dryer can be loaded with air-tight seal. It is connected to a
vacuum pump through a condenser and receiver.
• At a vacuum of 0.03 to 0.06 bar water boils at 350℃.

ADVANTAGES

• Very suitable for heat sensitive products

• Porous and friable product is obtained
• Valuable solvents can be recovered

DISADVANTAGES

• Heat transfer may be low and non-uniform

• Limited capacity
• Labor and running costs are high
• Finely divided powder may be drawn into the vacuum pump.

APPLICATIONS OF DRYING
• Drying is an important process which is used by almost all the
pharmaceutical industries.
• Drying has following applications in pharmacy:
1. For the preparation of granules which can be dispensed in bulk,
compressed in the form of tablets or filled in capsules.
2. For the preparation of certain products like dried aluminum
hydroxide, dried lactose cad powdered extracts.
3. For reducing the bulk and weight of powder and thus reducing the
cost of transportation and storage.
4. Vegetable drugs are dried before extraction to facilitate grinding
and to avoid deterioration on storage.
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 5. As dried products are more stable than moist ones so stable
products are produced by drying.
6. Drying has the considerable effects on the properties of product
and it produces a readily soluble and free flowing products.
7. Thermolabile substances can be dried using spray dryer.

DRYING OF SOLIDS
1. LOSS ON DRYING
The moisture in a solid can be expressed on a wet weight or dry weight
basis. On wet weight basis, the water content of a material and is calculated
as a percentage of weight of the wet solid. whereas on the dry weight basis,
the water is expressed as a percentage of weight of the dry solid. The term
loss on drying is an expression of moisture content on a wet weight basis,
calculated as:

Weight of water in sample

%LOD = ⨯ 100
Weight of wet sample

2. MOISTURE BALANCE
• The LOD of a wet solid is often determined by the use of moisture
balance, which has a heat source of rapid heating and a scale calibrated
in percent LOD.
• A weigh sample is placed on a balance and is allowed to dry until a
constant weight is achieved. The water lost by evaporation is read
directly from the percent LOD scale. It is assumed that there are no
other volatile materials present.

3. MOISTURE CONTENT
• Another measurement of the moisture in a wet solid is that calculated
on a dry weight basis. This value is referred to as moisture content or
MC, calculated by:

Weight of water in sample

%MC = ⨯ 100
Weight of dry sample

• LOD value can vary in any solid fluid mixture from slightly above 0 to
above 100%. But the MC value can change from slightly above 0 and

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 approach infinity. Thus, percent MC is a far more realistic value than
LOD, in the determination of dryer and capacity.

BEHAVIOR OF SOLIDS DURING DRYING

• It helps in determine:
- Time required to dry a certain batch in given dryer
- Size of dryer required for certain drying process.
• It is done by using a cabinet with a weighing scale provided that
conditions are of a large dryer and are properly simulated. The
information's obtained in drying in such an environment can be plotted
on a graph between moisture contents and drying rate.

1. INITIAL ADJUSTMENT
• When a wet solid is first placed in an oven, it undergoes initial
adjustment to the environment. During the production, it absorbs heat
and at the same time losses some moisture. Drying rate begins to
increase.

2. CONSTANT RATE PERIOD

• Temperature remains constant, moisture evaporating from solid surface
is replaced by more moisture which diffuses through capillary force, as a
result drying rate remains constant.

3. FIRST FALLING RATE PERIOD

• At this point, the speed at which moisture evaporates from the surface
exceeds the speed at which moisture diffuses to surface from the
bottom. Hence, a continuous drying cannot be maintained. As a result,
dry spots are formed. The moisture content at which this occurs is
termed as “Critical Moisture Content” With the passage of time, the no.
of dry spots keeps on increasing. Hence, during this stage, rate falls
steadily. This period is also termed as unsaturated surface drying.

4. SECOND FALLING RATE PERIOD

• The whole solid surface dries out and the rate of drying depends upon
diffusion of the moisture to the surface which is very low. Therefore,
rate of drying falls even more sharply than in the previous period. Point
D is referred to as 'second critical point’

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 5. EQUILIBRIUM MOISTURE CONTENT
• Drying rate = 0, then an equilibrium is attained between moisture
content in the solid and in the air. There cannot be any further loss of
moisture and any further heating will be useless.

GRAPH BETWEEN MOISTURE CONTENTS AND DRYING RATE

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 COMMINUTION (SIZE REDUCTION)

MILLING
• “Milling is the mechanical process of reducing the particle size of solids.”
• Various terms (commination, crushing, disintegration, dispersion,
grinding, and pulverization) have been used synonymously with milling
depending on the product, equipment and the process.
• Milling equipment is usually classified as coarse, intermediate or fine
according to the size of the milled product.

WHY MILLING? / IMPORTANCE OF MILLING

• Milling or grinding offers a method by which these particles can be
produced.
• The surface area per unit weight, which is known as the specific surface,
is increased by size reduction. In general, a 10-fold increase in surface
area has been given by a 10-fold decrease in particle size. This increased
surface area affects:

I. DISSOLUTION AND THERAPEUTIC EFFICACY

• Dissolution and therapeutic efficiency of medicinal compounds that
possess low solubility in body fluids are increased due to increase in the
area of contact between the solid and the dissolving fluid.

EXAMPLES
• The control of fineness of griseofulvin led to an oral dosage regimen half
that of the originally marketed product.
• In inhalational products, the size of particles determines their position
and retention in the bronchopulmonary system.
• Transdermal delivery is also facilitated by particle size reduction.

II. EXTRACTION
• Extraction or leaching from animal glands (liver and pancreas) and crude
vegetable drugs is facilitated by communition. The control of particle
size in the extraction process provides for more complete extraction and

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 a rapid filtration rate when the solution is filtered through the mare.

III. DRYING
• The drying of wet masses may be facilitated by milling, which increases
the surface area and reduces the distance that the moisture must travel
within the particle to reach the outer surface. Micronization and
subsequent drying also increases the stability because the occluded
solvent is removed.

EXAMPLE
• In the manufacture of compressed tablets by wet granulation process,
the sieving of the wet mass is done to ensure more rapid and uniform
drying.

IV. FLOWABILITY
• The flow property of powders and granules is affected by particle size
and size distribution. The freely flowing powders and granules in high-
speed filling equipment and tablet presses produce a uniform product.
For suspensions of high disperse phase concentration, reduction in
particle size leads to increase in viscosity.

V. MIXING OR BLENDING
• The mixing or blending of several solid ingredients of a pharmaceutical is
easier and more uniform if the ingredients are of approximately the
same size. This provides a greater uniformity of dose.
• Solid pharmaceuticals that are artificially colored are often milled to
distribute the coloring agent to ensure that the mixture is not mottled
and uniform from batch-to-batch. Even the size of a pigment affects its
color.

VI. FORMULATION
• Lubricants used in compressed tablets and capsules function by virtue of
their ability to coat the surface of the granulation or powder. A fine
particle size is essential if the lubricant is to function properly.

VII. RATE OF ABSORPTION

• Smaller the particle size quicker and greater will be the rate of

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 absorption. For example: rectal absorption of aspirin from a theobroma
oil suppository is also related to particle size.

VIII. EMULSION STABILITY

• Stability of emulsions is increased by decreasing the size of oil globules.
E.g. microemulsions are more stable.

IX. FILLING EQUIPMENT

• The flowability of powders, granules in high speed filling equipment and
in tablets presses is dependent upon size of particles.

X. LUBRICANTS
• A fine particle size is necessary if a lubricant is to function properly in
compressed tablets or capsules.

DISADVANTAGES OF SIZE REDUCTION

• Loss of aromatic and volatile ingredients: On grinding aromatic and
volatile content of crude drugs maybe lost ducts elevated temperature.
• Increased oxidation and reduction: Increased surface area due to size
reduction when exposed to atmospheric conditions may result in
oxidation and hydrolysis of the product.
• Caking in suspension due to small particles.
• Decrease in flow ability due to decrease in particle size.
• Very fine particles are not favorable for tablet preparation.
• Surface gets charged and particles aggregate.
• Some drugs degrade on milling.
• Some drugs melts upon milling due to increased temperature during
milling.
• Polymorphism occurs and crystal’s habit is changed.

FACTORS INFLUENCING MILLING

I. HARDNESS
• It is the surface property of the materials in general; harder the material
difficult is to reduce the size. However, if the material is very hard and
brittle also the size reduction may present no special problem.

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 II. TOUGHNESS
• A soft but tough material may present more problems in size reduction
then hard and brittle substances. E.g. a blackboard chalk can be broken
more easily than a rubber. Toughness can be reduced by treating the
material with liquefied gas such as nitrogen.

III. ABRASIVENESS
• It is the property of hard materials. During grinding of some very
abrasive substances, the final powder may become contaminated with
more than 0.1% of metal worn from grinding mill.

IV. STICKINESS
• It may cause considerable difficulty in size reduction as materials may
adhere to grinding surfaces or the meshes of screen may become
choked. Complete dryness helps milling. Addition of inert substances
could be assistance e.g. addition of kaolin to sulfur and DDT has been
advantageous.

V. SOFTENING TEMPERATURE
• Heat generated during milling can cause some substances to melt thus
causing problems. E.g. gummy or resinous substances.

VI. MATERIAL STRUCTURE

• Material structure may have lines or weakness along which the material
splits to form flake like particles.

VII. MOISTURE CONTENT

• In general, materials should be dry or wet; not merely damp. For dry
grinding less than 5% moisture is suitable when for wet grinding more
than 50% moisture is suitable.

VIII. PHYSIOLOGICAL EFFECT

• For potent drugs e.g. podophyllum, hormones, small amount of dust
may affect the operators, thus and enclosed mill should be used.

IX. PURITY REQUIRED

• When high degree of purity of product is designed, apparatus causing
wear off the grinding surface should be avoided.

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 X. SIZE OF FEED MATERIAL
• For very fine product it may be necessary to carry out the size reduction
in several stages depending upon the size of feed material. E.g.
preliminary crushing followed by coarse grinding and then fine grinding.

XI. BULK DENSITY

• The capacities of most batch mills depend on volume, thus the output of
machine is related to bulk density of the substances.

PARTICLE SIZE DISTRIBUTION (PSD)

• The particle-size distribution (PSD) of a powder, or granular material, or
particles dispersed in fluid, is a list of values or a mathematical function
that defines the relative amount, typically by mass, of particles present
according to size.
• It has a specific range i.e. between 1-100um. Average is always taken out
by mean and median.

EXAMPLE
• For a powder if we take reference of 10um then D10 = 10% particles are
of 10um and remaining 90% are greater than 10um (coarse powder)
• D50 = 50% particles are of 10um and remaining 50% are greater than
10um (fine powder)
• D90 = 90% particles are of 10um and remaining 10% are greater than
10um (very-fine powder)

SIZE ANALYSIS
• Particle size analysis, particle size measurement, or simply particle sizing
is the collective name of the technical procedures, or laboratory
techniques which determines the size range, and/or the average, or
mean size of the particles/ particle size distribution in a powder or liquid
sample.

SIEVING
• Sieving is the most widely used method for measuring particle size
distribution because it is inexpensive, simple, and rapid with little
variation between operators. Although the lower limit of application is

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 generally considered to be 50 microns, micromesh sieves are available
for extending the lower limit to 10 microns.
• A sieve consists of a pan with a bottom of wire cloth with square
openings. The procedure involves the mechanical shaking of a sample
through a series of successively smaller sieves and the weighing of the
portion of the sample retained on each sieve. The type of motion
influences sieving: vibratory motion is most efficient, followed
successively by side-tap motion, bottom-tap motion, rotary motion with
tap, and rotary motion.
• The B.P. specifies five grades of powder are:

Grade of powder Sieve through which all particle must pass

Coarse 10
Moderately coarse 22
Moderately fine 44
Fine 85
Very fine 120
NUMBER OF SIEVES
• This is the number of meshes in a length of 25.4 mm (1in) in each
direction parallel to the wires.

OTHER METHODS
• Sedimentation Methods
• Elutriation Techniques
• Microscopic Sizing and Image Analysis
• Electrical Impedance Method
• Laser Diffraction Methods

THEORY OF COMMINUTION
STRESS-STRAIN CURVE
• Compression at any point along the line below the yield value, the
material
will go back and returns to its original shape and this is called elastic
deformation. However, compression above the yield value will result in
plastic deformation in which the substance break down and not go back
to its original shape after removing stress.

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GRIFFITH THEORY
• The Griffith theory of cracks and flaws assumes that all solids contain
flaws and microscopic cracks, which increase the applied force according
to the crack length and focus the stress at the atomic bond of the crack
apex.
• The Griffith theory may be expressed as:

Yϵ
T=√
c

• Where, T is the tensile stress, Y is the Young's modulus, 𝜖 is the surface

energy of the wall of the crack and c is the critical crack depth required
for fracture

ENERGY OF COMMINUTION
• The energy required to reduce the size of particles is inversely
proportional to the size raised to some power. This general differential
equation may be expressed mathematically as:

dE C
=− n
dD D
• Where, dE is the amount of energy required to produce a change in size,
dD, of unit mass of material, and C and n are constants.

KICK'S LAW
• In 1885, Kick suggested that the energy requirement, E, for size
reduction is directly related to the reduction ratio (D1/D2). Kick's theory
may be expressed as:
D1
E = Cln
D2
• Where, D1 and D2 are the diameters of the feed material and discharged
product, respectively. The constant C may be regarded as the reciprocal
efficiency coefficient.
• Kick's equation assumes that the material has flaws distributed
throughout its internal structure that are independent of the particle
volume.

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RITTINGER'S LAW
• In 1867, von Rittinger proposed that the energy required for size
reduction is directly proportional to the increase in specific area surface
as expressed by the following relationship:

𝐸 = 𝑘1 (𝑆2 − 𝑆1 )
• Where, k1 denotes the relationship between the particle surface and
diameter, and S1 and S2 are the specific surface before and after milling,
respectively.
• In terms of particle diameters:
1 1
E = C′ [ − ]
D2 D1
• It is most applicable to brittle materials. Rittinger’s theory ignores
particle deformation before fracture although work is the product of
force and distance.

BOND'S LAW
• In 1952, Bond suggested that the energy required for size reduction is
inversely proportional to the square root of the diameter of the product.
This may be expressed mathematically as:

Wt α 1/√D2
• Where, Wt is the total work of comminution in kilowatt hours per short
ton of milled material, and D2 is the size in micrometers through which
80% by weight of the milled product will pass.

MILLING RATE
• The mass and size of particles and the time in the mill affect the milling
rate. It has been reported that batch milling of brittle materials in small
mills follows the first-order law. The original particles are fractured to
produce first-generation particles, which are then fractured to produce
second-generation particles, which are also fractured, and so on.

MECHANISM OR COMMINUTION
• Mills are equipment designed to impart energy to the material and

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 cause its size reduction. There are four main methods of effecting size
reduction, involving different mechanisms:

I. CUTTING
• It involves application of force over a very narrow area of material using
a sharp edge of a cutting device.

II. COMPRESSION
• In compression, the material is gripped between the two surfaces and
crushed by application of pressure.

III. IMPACT
• It involves the contact of material with a fast-moving part which imparts
some of its kinetic energy to the material. This causes creation of
internal stresses in the particle, there by breaking it.

IV. ATTRITION
• In attrition, the material is subjected to pressure as in compression, but
the surfaces are moving relative to each other, resulting in shear forces
which break the particles.

EQUIPMENTS
• A mill consists of three basic parts:
- Feed chute, which delivers the material
- Grinding mechanism, usually consisting of a rotor and stator
- A discharge chute.
• The principle of operation depends on cutting, compression, impact
from a sharp blow, and attrition. In most mills, the grinding effect is a
combination of these actions.

OPEN-CIRCUIT MILLING
• If the milling operation is carried out so that the material is reduced, to
the desired size by passing it once through the mill, the process is known
as open-circuit milling.

CLOSED-CIRCUIT MILL
• A closed-circuit mill is the one in which the discharge from the milling
chamber is passed through a size-separation device or classifier and the
oversize particles are returned to the grinding chamber for further

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 reduction of size. Closed-circuit operation is most valuable in reduction
to fine and ultra-fine size.

CLASSIFICATION TREE OF MILLS

Mills

Cutting Compression Impact Attrition Homogenization

Cutter Roller Hammer Pin Simple
Colloid Ball Silver son
Edge and end Vibro-energy Ultrasonic
runner Fluid energy High pressure
Spiral jet Microfluidizer
Low-pressure cyclone

1. CUTTER MILL
PRINCIPLE
• The basic principle of cutter mill is Cutting and shearing.

CONSTRUCTION
• The rotary knife cutter has a horizontal rotor with 2
to 12 knives spaced uniformly on its periphery turning
from 200 to 900 rpm and a cylindrical casing having
several stationary knives. The bottom of the casing
holds a screen that controls the size of the material
discharged from the milling zone.
• A disc mill consists of two vertical discs, each may be
rotating in the opposite directions (double-runner
disc mill), or only one may be rotating (single-runner
disc mill), with an adjustable clearance. The disc may be provided with
cutting faces, teeth, or convolutions. The material is pre-milled to
approximately 40-mesh size and is usually suspended in a stream of air
or liquid when fed to the mil.
• Cutting mills are used for tough, fibrous materials and provide a
successive cutting or shearing action rather than attrition or impact.

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WORKING
• Feeding of particle in the mill through the hopper. Milling is done
through the movement of rotating knives against stationary knives. Size
reduction occurs by fracture of particles between two sets of knives. The
screen retains the particles until a sufficient degree of size reduction
occurs.

OPERATION
• The feed size should be less than 1 inch in thickness and should not
exceed the length of the cutting knife. For sizes less than 20-mesh, a
pneumatic product-collecting system is required. Under the best
operating conditions, the size limit of a rotary cutter is 80-mesh.

USES
• Used to obtain a coarse degree of size reduction of soft materials such as
roots and peels before its extraction.
• Cutter mill is used for size reduction of tough & fibrous material like
animal tissues, medicinal plants, and plant parts. It is also used in the
manufacture of rubber, plastics and plastic material.

LIMITATIONS
• Not used for friable materials.
• The fed size should be less than 1 inch thick & should not exceed the
length of the cutting knife.
• The material is pre-milled and is usually suspended in a stream of air or
liquid when fed to the mill.

2. ROLLER MILLS
PRINCIPLE
• Roller mills consist of two to five smooth rollers operating at different
speeds. Thus, size reduction is effected by a combination of compression
and shearing action.

CONSTRUCTION AND WORKING

It consists of one or more rollers and is commonly used. Of these, the three-
roller types are preferred. In operation, rollers composed of a hard, abrasion-
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resistant material, and arranged to come into close
proximity to each other are rotated at different rates.
Depending on the gap, the material that comes
between the rollers is crushed, and also sheared by the
difference in rates of movement of the two surfaces.
USES
• For crushing seeds before extraction of fixed oil
• Used to crush soft tissue to help in penetration of solvents.

VARIANTS
• Multiple smooth rollers or corrugated, ribbed, or saw-toothed rollers
can provide cutting action also

3. COLLOID MILL
PRINCIPLE
• The basic principle of colloid mill is compression and shearing.

CONSTRUCTION
I. ROTOR AND STATOR
• A high-speed rotor, fixed to the housing with a
shaft. Rotor moves at the speed of 3000-20,000
rpm. Rotor is with conical milling surfaces. Just
under the rotor, there is stator.
• Rotors and stators may be either smooth-
surfaced, or rough-surfaced. With smooth-
surfaced rotors and stators, there is a thin,
uniform film of material between them which is
subjected to maximum amount of shear. Rough-surfaced mills add
intense eddy currents, turbulence, and impaction to the shearing action.
Rough-surfaced mills are useful with fibrous materials because fibers
tend to interlock and clog smooth-surfaced mills.
II. MOTOR
• It rotates the rotor.
III. ADJUSTABLE CLEARANCE

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 • The gap between rotor and stator is fitted with adjustable clearance that
can be adjusted from 0.002-0.03 inches.
IV. HOPPER
• Just above the rotor, is a hopper for material input.
V. OUTLET
• In the periphery of housing, is an outlet for discharge of material.

WORKING
• It works on the principle of shearing consisting of conical rotor and
stator. A colloid mill consists of a high-speed rotor (3,000 to 20,000 rpm)
and a stator with conical milling surfaces between which an adjustable
clearance ranging from 0.002 to 0.03 inches is present.
• The material to be grounded should be pre-milled as finely as possible to
prevent damage to the colloid mill. The reduced material is then fed into
the machine through a hopper which is thrown outward by centrifugal
action. As the material pass through a narrow gap between rotor and
stator its size is reduced.

USES
• These are used primarily for the comminution for solids and dispersion
of suspensions containing wetted solids and preparations of viscous
emulsions.

ADVANTAGES
• Products with particle size less than 1um can be obtained.
• Useful for preparing pharmaceutical syrup, emulsions, lotions, ointments
and creams.
• Size reduction is always carried out in the presence of liquid.

DISADVANTAGES
• Not applicable for processing dry materials.
• Materials need to be milled previously.
• Suspensions may be aerated due to colloid mill.

4. EDGE-AND END-RUNNER MILL

EDGE RUNNER MILL

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OTHER NAMES
• Chaser mill

PRINCIPLE
• It is basically a mechanical pestle and mortar for large scale production.
The basic principle of Edge-runner Mill is compression due to the weight
of the pestle and shear.

CONSTRUCTION
• It consists of the following parts:
- Rollers
- Shafts
- Bed or base
- Adjustable clearance
• The edge-runner mill consists of one or two heavy
granite or cast-iron wheels or mailers mounted on a horizontal shaft and
standing in a heavy pan.
I. ROLLERS
• Two heavy, steel or granite wheels revolve or chase each other on a
steel or granite the base giving the name chaser mill. The stone may be
as heavy as six tons and having a diameter of 0.5 to 2.5m.
• The large size roller may weigh up to 6 tons.
II. SHAFTS
• The rollers are mounted on a horizontal shaft and turns around a vertical
shaft.
III. BED OR BASE
• Made up of steel or granite. Usually the wheels are rotated but
sometimes the base is made to rotate.
IV. ADJUSTABLE CLEARANCE
• The height between the rollers and the base determines the particle size
of the material hence the fineness of the particles can be increased or
decreased by adjusting the height.

WORKING
• The material is fed into the center of the pan and is worked outward by

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 the mulling action. Milling occurs by compression, due to the weight of
the muller, and by shearing.
• Both mills operate at slow speeds on a packed bed. Both produce
moderately fine powders and operate successfully with fibrous
materials. Wet grinding with very viscous materials such as ointments,
pastes are also possible.

USES
• Edge runner mill is used for grinding tough materials to fine powder. It is
still used for plant-based products.

ADVANTAGES
• Simple to operate, require less attrition.
• Easy maintenance
• No problem of jamming
• Used to reduce size of extremely tough and fibrous roots and barks.

DISADVANTAGES
• Require more floor space than other commercial machines
• Output is less
• Cannot accommodate wet grinding.

END RUNNER MILL

• End runner mill is used for grinding tough materials to fine powder. It is
suitable for fine grinding.

PRINCIPLE
• It works on the principle of crushing and shearing.

CONSTRUCTION
• The end-runner mill is similar in principle and
consists of a rotating pan or mortar made of cast
iron or porcelain. A heavy pestle is mounted
vertically within the pan in an off-center position.
• It consists of following parts:
I. MORTAR

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 • A moveable mortar made up of steel or granite.
II. PESTLE
• Made up of same material as that of mortar. It is dumble shaped and
heavy. It is mounted eccentrically in mortar through a hinged joint.
Pestle is free to rise and fall in mortar.
III. MOTOR
• It is needed to rotate the mortar.
IV. SCRAPPER
• Scrapper is attached to the mortar which constantly removes the
material from the pestle and thus returning them back to the mortar.

WORKING
• The material to be ground is put in the mortar, which is rotated
mechanically. The pestle rotates itself by friction. The material is crushed
and rubbed between the pestle and the rotating mortar. The scrapper
removes the sticking material from the pestle and returns back to the
mortar for grinding. The ground material is passed through the sieve to
get the powder of required size.

PHARMACEUTICAL APPLICATIONS
• They are used for reduction of tough and fibrous materials.
• Used also for coarse materials.
• Used for the reduction of roots and barks to form the powder.

ADVANTAGES
• Suitable for reducing particle size of coarse materials.
• Completely simple as compared to complex mills

DISADVANTAGES
• Output is less.
• More time consuming

5. HAMMER MILL
OTHER NAMES
• Fitz Patrick comminutor

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PRINCIPLE
• The basic principle of hammer mill is impact.

CONSTRUCTION
• The hammer mill is an impact mill using a
high-speed rotor (up to 10,000 rpm) to
which a number of swinging hammers are
fixed. A universal mill employs a variety of
rotating milling elements such as a pin
disk, wing or blade beater, turbine rotor,
or hammer-type rotor, in combination
with either a matched pin disk (that may
or may not rotate), or perforated screen or stator.
• Criticality: The screens that retain the material in the milling chamber
are not woven but perforated. The particle size of the discharged
material is smaller than the screen hole or slot, as the particles exit
through the perforations on a path approximately tangential to the
rotor. Efforts to strengthen a screen by increasing its thickness influence
particle size. For a given rotor speed and screen opening, a thicker
screen produces a smaller particle, which is also illustrated in Fig.

WORKING
• The material is fed at the top or center, thrown out centrifugally, and
ground by impact of the hammers or against the plates around the
periphery of the casing. The clearance between the housing and the
hammers contributes to size reduction. The material is retained until it is
small enough to fall through the screen that forms the lower portion of
the casing. Particles fine enough to pass through the screen are
discharged almost as fast as they are formed.
• Some internal classification can be achieved by appropriate selection of
milling tools. The particle size that can be achieved will depend on the
type of milling tool selected, rotor speed (calculated as tip speed it the
outermost rotating part), and solid density in the mill or solid feed rate.

CRITICAL SPEED

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 • Comminution is effected by impact at peripheral hammer speeds of up
to 7,600 meters per minute, at which speed most materials behave as if
they were brittle. In the preparation of wet granules for compressed
tablets, a hammer mill is operated at 2,450 rpm with knife edges, using
circular or square holes of a size determined by what will pass without
clogging (1.9 to 2.54 cm). In milling the dried granulation, the mill is
operated at 1,000 or 2,450 rpm with knife edges and circular holes in the
screen (0.23 to 0.27 cm).
• Speed is crucial. Below a critical impact speed, the rotor turns so slowly
that a blending action rather than comminution is obtained. This results
in overloading and a rise in temperature. Microscopic examination of the
particles formed when the mill is operating below the critical speed
shows them to be spheroidal, indicating not an impact action, but an
attrition action, which produces irregularly- shaped particles.
• At very high speeds, there is possibly insufficient time between
hammers for, the material to fail from the grinding zone. In wet milling
of dispersed systems with higher speeds, the swing hammers may lay
back with an increased clearance. For such systems, fixed hammers
would be more effective.

FACTORS AFFECTING PARTICLE SIZE OF A PRODUCT

• Rotor speed
• Feed rate
• Type and number of hammers
• Clearance between hammers and chamber wall
• Discharge opening of screens

EXAMPLES
• Afex comminuting mill
• Fitz comminuting mill

PHARMACEUTICAL APPLICATIONS
• The hammer mill can be used for almost any type of size reduction. Its
versatility makes it popular in the pharmaceutical industry, where it is
used to mill dry materials, wet filter-press cakes, ointments, and slurries.

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 • A hammer mill can be used for granulation and close control of the
particle size of powders.
• They are used for preparation of wet granules for compressed tablets.
• They can be used for grinding of fibers.
• They can be used for crystalline material.
• Used in powdering the barks, leaves, roots, crystals and filter cakes.

ADVANTAGES
• They are simple to install and operate, the operation is continuous.
• They are rapid in action and many different types of materials can be
ground with them.
• There is no chance of contamination due to abrasion of metal from the
mill because no surfaces of the mill move against each other.
• The particle size of the material to be reduced can be easily controlled
by changing the speed of the rotor, hammer type, shape & size of the
screen.
• They are easy to clean and may be operated as a closed system to
reduce dust and explosion hazards.

DISADVANTAGES
• Heat buildup during milling is more, therefore, product degradation is
possible.
• Hammer mills cannot be employed to mill sticky, fibrous and hard
materials.
• The screens may get clogged. Wearing of mill and screen is more with
abrasive materials.

6. PIN MILL
PRINCIPLE
• The basic principle of pin mill is attrition.

CONSTRUCTION
• Pin mills Consist of two horizontal steel plates
with vertical projections arranged in concentric
circles on opposing faces and becoming more

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 closely spaced towards the periphery. The projections of the two faces
intermesh.

WORKING
• The feed is introduced at a controlled rate to the milling chamber
through the center of the stator and is propelled through intermeshing
rings of rotor and stator pins by centrifugal motion. The passage
between the pins leads to size reduction by impact and attrition. The
material is collected in the annular space surrounding the disks and
passes to a separator. The large volumes of air drawn through the mill
are discharged through the separator. The final particle size achieved in
a pin mill is governed by the rotor speed, solids feed rate, and air flow
rate through the mill.
• Smaller particles can be generated by maxi-mizing the rotor tip speed
and minimizing both product feed and air flow rate. The fineness of the
grind may be varied by the use of disks with different dispositions of
pins. As equipment scale is increased, maintaining rotor tip speed is one
reliable way to achieve milled particle sizes comparable to small-scale
results.

ADVANTAGES AND DISADVANTAGES

• Absence of screens and gratings provides a clog-free action.
• This type of milling is typically able to achieve smaller average particle
size than wet rotor-stator milling.
• The machine is suitable for grinding soft, non-abrasive powders, and low
milling temperatures permit heat-sensitive materials to be processed.

7. BALL MILL
OTHER NAMES
• Jar mill

PRINCIPLE
• The basic principle of ball mill is impact and attrition.

VARIANTS OF SIMPLE BALL MILL

TUBE MILL

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 • The tube mill as its name implies has a long narrow cylinder and can
grind to a finer product than the conventional ball mill.

PEBBLE MILL
• If pebbles are used, it is known as a pebble mill.

ROD MILL
• If rods or bars are used, it is known as a rod mill. The rod mill is
particularly useful with sticky material that would hold the balls together
because the greater weight of the rods causes them to pull apart.

HANDING MILL
• The ball mill may be modified to a conical shape and tapered at the
discharge end. If balls of different size are used in a conical ball mill, they
segregate according to site and provide progressively finer grinding as
the material flows axially through the mill.

CONSTRUCTION
• The ball mill consists of a horizontally rotating hollow
vessel of cylindrical shape with the length slightly greater
than its diameter. The mill is partially filled with balls of
steel or pebbles, which act as the grinding medium.

BALLS
• The balls act as grinding medium. Balls are usually made up of stainless
steel or steel and occupy about 30 to 50% of the volume of cylinder.
• Balls are made up of:
- Porcelain - Nylon
- Flint - Rubber

METALLIC FRAME
• The cylindrical vessel is mounted on a metallic frame.

HANDLE
• It is needed for rotating the cylinder.

WORKING
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 • The material to be grounded is put into the mill through the lid. The mill
is rotated at a slow speed for appropriate time until the desired size
reduction is achieved. The product is then taken out and passed through
the suitable sieve to get powder of desired size range.
• Most ball mills utilized in pharmacy are batch-operated, however,
continuous ball mills are available, which are fed through a hollow
trunnion at one end, with the product discharged through a similar
trunnion at the opposite end. The outlet is covered with a coarse screen
to prevent the loss of the balls.

CRITICAL SPEED
• The critical speed of a ball mill is the speed at which the balls just begin
to centrifuge with the mill.
• In a ball mill rotating at a slow speed, the balls roll 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 onto the material with an impact action, which is
responsible for most size reduction. If the speed is increased sufficiently,
the balls are held against the mill casing by centrifugal force and revolve
with the mill.

critical speed = 76.6/√D

• Improving the efficacy of ball mill
• Efficiency of a ball mill is increased as amount of material is increased
until the space in the bulk volume of ball charge is and then, the
efficiency of milling is by further addition of material.
• Increasing the total weight of balls of a given size increases the fineness
of the powder. The weight of the ball charge can be increased by
increasing the number of balls or by using a ball composed of a material
with a higher density.
• Optimum milling conditions are usually obtained when the bulk volume
of the balls is equal to 50% of the volume of the mill, variation in weight
of the balls is normally affected by the use of materials of different
densities. Thus, steel balls grind faster than porcelain balls, as they are
three times denser.

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 • Wetting agents may increase the efficiency of milling and physical
stability of the product by nullifying electrostatic forces produced during
comminution. For those products containing wetting agents, the
addition of the wetting agent at the milling stage may aid size reduction
and reduce aggregation.

USES
• Used for either wet or dry milling
• Ball mill at low speed is used for milling dyes, pigments and insecticides.
• Stainless steel balls are preferred in production of ophthalmic and
parenteral products.

ADVANTAGES
• Ball mill has the advantage of being used for batch or continuous
operation.
• In a batch operation, unstable or explosive materials may be sealed
within an inert atmosphere and satisfactorily ground.
• Ball mills may be sterilized and sealed for sterile milling in the
production of
• The installation, operation, and labor costs involved in ball milling are
low.

DISADVANTAGES
• The ball mill is very noisy machine.
• Ball mill is a slow process.
• Soft, tacky, fibrous material cannot be milled by ball mill.

8. FLUID-ENERGY MILL
OTHER NAMES
• Jet mill or micronizer

PRINCIPLE
• The basic principle of fluid-energy mill is impact and attrition.

CONSTRUCTION
• A fluid-energy mill consists of following parts:

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 - Venturi injector
- Nozzles
- Grinding chamber
- Discharge outlet
- Cyclone separator
- Bag collector
• The design of the fluid-energy mill provides
internal classification, which permits the finer
and lighter particles to be discharged and the
heavier oversized particles, under the effect of centrifugal force, to be
retained until reduced to a small size.

WORKING
• In the fluid-energy mill or micronizer, the material is suspended and
conveyed at high velocity by air or steam, which is passed through
nozzles at pressure of 100 to 150 pounds per square inch (psi). The
violent turbulence of the air and steam reduces the particle size chiefly
by inter-particular attrition. Air is usually used because most
pharmaceuticals have a low melting point or are thermolabile. As the
compressed air expands at the orifice, the cooling effect counteracts the
heat generated by milling.
• The material is fed near the bottom of the mill through a venturi injector
(A). As the compressed air passes through the nozzles (B), the material is
thrown outward against the wall of the grinding chamber (impact) (C)
and other particles (attrition). The air moves at high speed in an elliptical
path carrying with it the fine particles that pass out of the discharge
outlet (D) into a cyclone separator and a bag collector. The large
particles are carried by centrifugal force to the periphery, where they
are further exposed to the attrition action.

USES
• It is used to reduce particle size of antibiotics and vitamins.
• Moderately hard materials can be processed for size reduction.
• Ultra-fine grinding can be achieved.

ADVANTAGES

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 • Powders with all particles below a few micrometers may be quickly
produced by this method.
• Cooling effect of grinding fluid as it expands in the chamber
compensates for the moderate heat generated during grinding process.
• Narrow range of particle size produced.
• No abrasion of the mill.
• For very sensitive materials, an inert gas can be used.
• Useful for thermolabile substances e.g. vitamins and enzymes.

DISADVANTAGES
• The disadvantage of high capital and running costs may not be so serious
in the pharmaceutical industry because of the high value of the
materials which are often processed.
• One drawback of this type of mill is the potential for build-up of
compressed product in the mill or on the classifier. This can affect milled
particle size by changing the open volume in the mill or open area in the
classifier, especially if classifier vanes or gas nozzles become plugged or
blocked.

9. DISINTEGRATOR
PRINCIPLE
• It works on the principle of impact and grinding.

CONSTRUCTION
• It consists of:
- Chamber
- Disc and shaft
- Sieve
- Hopper
• The disintegrator consists of a drum
shaped chamber made up of steel. In the chamber, there are four steel
beaters fixed to a disc through which passes a shaft which rotates at a
higher speed up to 5000-7000 rpm. The tower part of the chamber is
filled with a desired number sieve which can be easily attached or
detached. A hopper is attached at the upper surface of the chamber.

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WORKING
• The drug to be comminuted is fed into the chamber through the hopper
where it is broken by the direct blow of the beaters and by the impact of
the material, which is thrown with a great force against the surface of
the chamber. The reduced particles pass through the sieve of desired
size.

ADVANTAGES
• Can be used for powdering very bard drugs.
• Used for powdering crude vegetable drugs.
• Can be used for milling the ointments and for mixing the powdered
ingredients.

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 MIXING

DEFINITION
“Mixing is a process that tends to result in a randomization of dissimilar
particles within a system.” (OR)
“The process in which two or more than two components in a separate or
roughly, mixed conditions is treated in such a way that each particle of anyone
ingredient lies as nearly as possible to the adjacent particles of other
ingredients is called mixing.”

OBJECTIVES OF MIXING
• To ensure uniformity of composition between mixed ingredients.
• To initiate or enhance physical or chemical reactions e.g. diffusion and
dissolution.
• To improve single phase and multiple phase system.
• To control heat and mass transfer.

RESULT OF MIXING
• When two or more than two miscible liquids are mixed true solutions
are obtained.
• When two immiscible liquids are mixed in the presence of emulsifying
agent, emulsions are produced.
• When a solid is mixed in a vehicle a solution is obtained.
• When an insoluble solid is mixed in a vehicle a suspension is obtained.
• When a solid/liquid is mixed in a semisolid base/ointment suppositories
are produced.
• When two or more than two solids are mixed together a solid dosage
form is obtained.

TYPES OF MIXTURES
1. POSITIVE MIXTURES
• Spontaneous, irreversible and complete mixing of two or more than two
gases or miscible liquids through diffusion, without the expenditure of
energy results in a positive mixture.
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 2. NEGATIVE MIXTURES
• These are formed when insoluble solids are mixed with a vehicle to for a
suspension or when two immiscible liquids are mixed to form emulsion.
• These mixers require a high degree of mixing with external force.

3. NEUTRAL MIXTURES
• The components of neutral mixers do not have the tendency to mix
spontaneously but once mixed, they do not separate out immediately
e.g. ointments, pastes.
• Neither mixing nor de-mixing unless system is acted upon by an external
energy input.

DEGREE OF MIXING
• Degree of mixing is defined in terms of standard deviation.

xy
Standard deviation = √
N
• Here,
- x and y are proportions of the major and minor constituents, N is
the number of particles in the sample taken.
• Mixing of powder should be continued until the amount of active drug
that is required in a dose is with in ± 35° of that found by assay in a
representative number of sample doses.

MECHANISM OF MIXING
• In all type of mixers mixing is achieved by applying one or more of the
following mechanisms:

1. CONVECTIVE MIXING
• During convective mixing, transfer of groups of particles in bulk take
place from one part of the powder bed to another.

2. SHEAR MIXING
• During shear mixing, shear forces are created within the mass of the
material by using agitator arm or a blast of air.

3. DIFFUSIVE MIXING
• During this mixing, the material are tilted so that the gravitational forces

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 causes the upper layers to slip and diffusion of the individual particles
take place over newly developed surfaces. Mixing occur by diffusion
process by random movement of particle within a powder bed and
cause them to change their relative position.

CLASSIFICATION OF MIXING EQUIPMENTS

POWDER MIXERS / SOLID MIXERS
1. Pestle and Mortar
2. Spatula
3. Sieves
4. Tumbler Mixers
a) Cube Mixers c) Double Cone/H type
b) V Mixers d) Y Mixers
5. Agitator Mixers
a) The Ribbon Blender d) Paddle Mixer
b) Helical Flight Mixer e) Granulating Mixer
c) Monastery Blender f) Trough Mixer

FLUID MIXERS / LIQUID MIXERS

1. BATCH MIXERS
a. Shaker Mixer
b. Impellers
i. Propeller Mixer
ii. Turbine Mixer
- Pitched Blade Turbine
- Curved Blade Turbine
- Disk Style Turbine
iii. Paddle Mixer
- Simple Paddle
- Gate Paddle
- Anchor Paddle
- Helix Paddle
c. Air Jets
d. Fluid Jets
2. CONTINUOUS MIXERS
a. Baffled Pipe Mixers

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 b. Mixing Chamber
c. Continuous Mixing Tank

SEMI-SOLID MIXERS
1. Agitator Mixers / Kneaders
2. Shear Mixers / Mulling Mixers
3. Ultrasonifiers

POWDER MIXING

INTRODUCTION
• Powder mixing is a process in which two or more than two solid
substances are mixed in a mixer by continuous movement of particles.
• It is a neutral type mixing and is one of the most common operations
employed in pharmaceutical industries for the preparation of different
types of formulations e.g. powders, capsules.

FACTORS AFFECTING POWDER MIXING

1. MIXING FACTORS
• Powder mixing operation is quite different from that of liquid. Following
factors must be considered:
A. VOLUME
• Sufficient space should be provided during mixing for dilation of the bed
overfilling of the mixer reduces the efficiency of mixing. The mixer
should not be full to the brim.
B. MIXING MECHANISM
• The mixer selected for mixing must apply suitable shear forces and
convective movement so that the whole of the material passes through
the mixing area.
C. DURATION OF MIXING
• Mixing of powders must be done for optimum time for any particular
situation.
D. HANDLING OF MIXED POWDERS
• After mixing the powders, they should be handled in such a way that the
separation of ingredients in minimized.
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 • Sometimes vibration caused by subsequent manipulation, transport,
handling or use is likely to cause segregation.

2. PHYSICAL PROPERTIES / FACTORS

A. MATERIAL DENSITY
• If the density of mixing ingredients is different, the denser material will
sink through the lighter one forming a layer at the bottom resulting in
improper mixing.
B. PARTICLE SIZE
• Variation in particle size can lead to segregation since smaller particles
can fall through the voids between the larger particles.
C. PARTICLE SHAPE
• Spherical shape of particle is ideal for mixing the powders and any
deviation from this shape leads to difficulty in mixing. However, once the
mixing has been done, the particles with irregular shapes can interlock
with each other, reducing the chance of segregation.
D. PARTICLE ATTRACTION
• Some particles exert electrostatic charges due to which the particles of
one powder may attract to particles of another powder leading to
aggregation of particles.
E. PROPORTION OF THE MATERIALS TO BE MIXED
• It is easy to mix powders if they are available in equal quantities but it is
difficult to mix small quantities of powders with large quantities of other
ingredients or diluents.

MECHANISM OF POWDER MIXING

• Powder mixing proceeds by a combination of one or more underlying
mechanisms:

1. CONVECTIVE MOVEMENTS OF POWDER BED

• It is caused by an invasion of powder bed that occurs due to the
movement of relatively larger mass of material from one part of powder
bed to another. It is analogous to bulk transport. It is done by means of
blades, paddles and screws.

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 2. SHEAR MIXING
• When shear occurs between regions of different composition and
parallel to their interface, it reduces the scale of segregation by thinning
the dissimilar layers.
• Shear occurring in a direction normal to the interface of such layers is
also effective since it too reduces the scale of segregation.
• In addition, large or irregular grains of powder tend to be expelled from
regions of high shear through a mechanism shear induced migration.

3. DIFFUSE MOVEMENTS (DISPERSION)

• The random motion of powder within a particular bed cause them to
change position relative to one another. Such an exchange of position by
single particles results in reduction of the intensity of segregation. Most
efficient mixers operate to induce mixing by all three mechanisms.
Diffusion is rate limiting mechanism for powder mixing.

EQUIPMENTS FOR POWDERS MIXING

1. PESTLE AND MORTAR
• It is the most commonly used equipment for small scale mixing,
especially in compounding prescriptions. In this method, particle size
reduction and mixing is done in a single operation.

2. SPATULA
• This method is relatively insufficient but is used when compaction
produced by pestle and mortar method is undesirable.

3. SIEVES
• Sieves are generally used for breaking the loose aggregates of powders
in pre or post mixing operation so as to increase overall effectiveness of
a blending technique. Sometimes powder may have to be passed a
number of times through the sieve to get a homogenous powder.

4. TUMBLER MIXER (BLENDER)

• These mixers are used for large scale mixing or batch mixing of powders.
The efficiency of tumbling mixer is highly dependent on the speed of
rotation. Rotation that is too slow that does not produce the desired
intense tumbling or cascading motion nor does it generate rapid shear
rates. The rotation that is too rapid tends to produce centrifugal force
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 sufficient to hold the powders to the sides and thereby reducing
efficiency. Speed of rotation commonly ranges from 30-100rpm.
• The optimum rate of rotation depends upon:
- Size and the shape of tumbler
- Type of material being mixed
• Tumbler mixer consists of a container which is mounted so that it can be
rotated about an axis. The resulting tumbling motion is accentuated by
means of baffles or simply by virtue of shape of container.
• Mostly an eight-angle shaped tumbler is used with baffles on each side.
Granules are twisted, flowing along the angle of baffle and mixed again
by the center short baffle. It can give best mixing result.

PRINCIPLE
• The mixers work on the principle of:
- Convective movement
- Shear mixing

WORKING
• In tumbler mixers rotation of vessel imparts movement to the materials
by tilting the powders until the angle of surface exceeds the angle of
repose when the surface layers of particles go into a slide and the
material is tumbled, rolled and folded e.g. in case of Y-cone blender.
• Plain of shear is always changing throughout the mass and the moving
material is constantly re divided and recombined.

CONSTRUCTION
METALLIC CONTAINER
• It consists of metallic vessel of various shapes rotating about its mid-
point on horizontal axis. Depending upon shape of vessel, they could be:
I. Cube mixer III. Double cone mixer
II. V mixer IV. Y mixer

MOTOR
• Horizontal axis is rotated with the help of motor.
I. CUBE MIXER

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 • It consists of a cube shaped stainless steel drum which is connected to
motor, blades are also attached inside the container to reduce the size.
The cube has an opening in front with screw nuts. It is good for wet
granulation mixing.
II. TWIN SHELL BLENDER V-SHAPED
• This is most popular mixer used in industry. When this is rotated, the
material is collected in the bottom of V, splits into two portions when V
is inverted. This design is quite effective because shear forces are
enhanced. Facilitate asymmetric rotation.
III. H-TYPE MIXERS / DOUBLE CONE MIXER
• It consists of mixing blades which rotates inside the pan with the help of
electric motor. Material is put in the pan and mixed by rotating blades.
Cover of pan is transparent and operation can be viewed.
IV. Y-CONE BLENDER
• It has a shallow drum with conical portion, the smaller end of which
provides discharge opening and longer end has two cylindrical portions
mounted approximately at right angles to each other.

WORKING
• Sliding material is deflected by inclined curved surface as there is
continuously changing angle to achieve the current in both vertical and
horizontal directions which is essential feature of efficient mixing.
• The gentle force is free from attrition it does not breakup crystal shape
and does not result in change of particle size and neither does it
generates heat.
• In case of Y-shaped cone blender, 2-fold force/reaction occurs;
- Rolling and folding movements
- Continuous dividing and recombining of powder.
• By its unique geometrical consideration; all internal substances blend
with each other.

ADVANTAGES
• Tumbler mixers are designed for rapid, economical blending of powders,
colors, resins, granules etc.
• It does not change the particle size distribution

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 • It has useful application in pharmaceutical food, cosmetics production,
detergents, insecticides and explosive materials
• It does not break up the crystal shape
• It can be used for heat sensitive materials.

DISADVANTAGES
• It cannot perform wet mixing.
• Cube mixer is less efficient than paddle mixer.

5. AGITATOR MIXERS
PRINCIPLE
• The mixing is done by means of mixing screws, paddles or blades. The
high shear forces are setup during the process which break the lumps or
aggregates and produce homogenous mixture.
• They consist of a stationary container, with a horizontal or vertical
agitator moving inside it. The agitator may take the form of blade,
paddles or screws.
• They are used for mixing of wet solids. Also used for sticky or plastic
state.

TYPES
• Well known mixers of this type include:
1. The ribbon blender 4. Paddle mixer
2. Helical flight mixer 5. Granulating mixer
3. Monastery blender 6. Trough mixer
I. RIBBON BLENDER
• It is also known as conventional mixer. It consists of a horizontal
cylindrical tank usually opening at the top and fitted with helical blades.
The blades are mounted on a shaft through the long axis of the tank and
are often of both right- and left-hand twist.
• It is used for dry granules, wet granules, dry powders and semi-solids.

CONSTRUCTION
• TROUGH
- These are stationary container of welded stainless steel and of
such shapes ass to eliminate the cervices, trough are robust and

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 polished from inside and outside so that they may rapidly be
cleaned.
• LID WITH COVER
- A polished stainless-steel lid is fitted with a safety grind with an
inspection cover.
• RUBBER GASKET
- Lid seats on the trough with a rubber gasket and held together
with two toggle fasteners.
• AGITATOR
- Mixer is fitted with a polished stainless-steel paddle type agitator
which is suitable for dry or moistened material. In cases where
mass becomes sticky, special agitator ribbon blender are
recommended.
• AGITATOR SHAFT
- It passes through the long axis of tank. The shaft entering the
trough is sealed by means of gasket so that dust can be avoided
and lubricant from bearing can effectively be preventing from
reaching and contaminating the mixture. When shaft is rotated,
the material is picked up by the helical blades which are then split
back.
• MOTOR
- It is fitted with a 3-phase gear motor unit that rotates the shaft.

WORKING
• The material to be mixed is put in the mixer and mixed for optimum
time period. Then the lid lifted by hand for discharge. The lid is fitted
with an electrical limit switch which prevents the agitator being in
motion with the lid raised.
II. HELICAL FLIGHT MIXER
• Powders are lifted by a centrally located vertical screw and allowed to
cascade to the bottom of the tank.
III. TROUGH MIXERS
• These are most commonly in the form of trough in which an arm rotates
and transmits shearing force to particles.

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FACTORS AFFECTING MIXER SELECTION
1. MEASURE OF DEGREE OF MIXING
• In case of powder mixing, mixer selection also depends on quantitative
measure of the degree of mixing. This is generally accomplished by the
arbitrary choice of a statistical function that indicates the uniformity of
composition of the powder bed.

2. TIME AND POWER CONSUMPTION

• Unlike most liquid mixers, solid mixers can be made to produce good
mixtures, when they are operated incorrectly, simply by mixing for a
long period of time. The mixture reaches an equilibrium state of mixing
that is the function of speed of operation of mixer.
• Minimum power is that required to operate the mixer for the time
necessary to reach a satisfactory steady state.

3. PHYSICAL PROPERTIES OF MATERIAL

• Physical properties of material greatly influence the selection of mixers.

4. ECONOMIC CONSIDERATIONS
• Economic considerations should be taken before selecting a mixer.

FLUID MIXING

INTRODUCTION
• Liquid mixing may be divided into two groups:
1. MIXING OF LIQUID AND LIQUID
- Mixing of two immiscible liquids
- Mixing of miscible liquids
2. MIXING OF SOLIDS AND LIQUIDS
- Mixing of liquid and soluble solids
- Mixing of liquid and insoluble solids

THEORY
• Mixing occurs in two stages:
1. LOCALIZED MIXING
- In which shear applied to the particles of the liquid.
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 2. GENERALIZED / BULK MIXING
- Sufficient to take all the particles of the materials through the
shearing zone so as to produce a uniform product.

1. MIXING OF LIQUID AND LIQUID

A. MIXING OF TWO MISCIBLE LIQUIDS
• Mixing of two miscible liquids is caused by diffusion. Simple shaking and
stirring is enough but if the liquids are not readily miscible or if they have
very different viscosities then electric stirrer may be used.

B. MIXING OF TWO IMMISCIBLE LIQUIDS

• When two immiscible liquids are mixed together in the presence of an
emulsifying agent, an emulsion is formed. For the production of a stable
emulsion, mixing must be continuous without ceasing because the
components tend to separate out if continuous work is not applied on
them.

2. MIXING OF LIQUIDS AND SOLIDS

A. MIXING OF LIQUIDS AND SOLUBLE SOLIDS
• In this case, soluble solids are dissolved in a suitable liquid by means of
stirring. It is a physical change.

B. MIXING OF LIQUIDS AND INSOLUBLE SOLIDS

• When insoluble solids are mixed with a vehicle, a suspension is produced
which is an unstable system the ingredients of a suspension out when
allow to stand for some time therefore to get a good suspension a
suitable suspending agent should be used.

MECHANISM OF FLUID MIXING

• Fluid mixing involve more than one following mechanisms.

1. BULK TRANSPORT
• The movement of relatively large portion of the material being mixed
from one location of the system to the constitutes bulk transport. This is
usually accomplished by means of paddles, revolving blades or other
devices within the mixer arranged so as to move adjacent volumes of
the liquid in different direction thereby shuffling the system in different
directions.
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 2. TURBULENT FLOW
• The phenomenon of turbulent mixing is a direct result of turbulent fluid
flow, which is characterized by a random fluctuation of fluid velocity at
any given point within the system. With turbulence, the fluid has
different instantaneous velocities at different locations at the same
instant of time and such velocity differences within the body of fluid
produce a randomization of fluid molecule, therefore turbulence is an
effective mechanism.

3. LAMINAR MIXING
• When two dissimilar liquids are mixed through laminar flow, the shear
that is generated stretched the interface between them. If the mixer
employed folds the layer back upon themselves, the number of layers
and hence the interfacial area between them increases exponentially
with time. If the mixer employed operates by simply stretching the fluid
layers without any significant folding force, an exceedingly long time is
required for the layers of different fluids to reach molecular dimensions.

4. MOLECULAR DIFFUSION
• The primary mechanism responsible for mixing at molecular level is
diffusion resulting from thermal motion of molecules. The process is
described quantitatively in terms of Fick’s first law of diffusion;

dm dc
= −DA
dt dx
• Where,
- D = diffusion coefficient, A = area of interface, dc/dx =
concentration gradient across the interface.
• The rate of transport of mass (dm/dt) across an interface of area A is
proportional to the concentration gradient (dc/dx) across the interface.

EQUIPMENTS FOR FLUID MIXING

• There are two types of equipment;

A. BATCH MIXING
• When the material to be mixed is limited in volume it is called batch
mixing. It is a feasible method. A system for batch mixing commonly
consists of two primary components:
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 - A tank or other container suitable to hold the material being
mixed.
- A means of supplying energy to the system so as to bring about
rapid mixing.
• Power may be supplied to the liquid mass by means of:
- Impellers: propellers, turbines and paddles are employed as
impellers
- Air jets
- Fluid jets

B. CONTINUOUS MIXING
• The process of continuous mixing produces an uninterrupted supply of
freshly mixed material and is often desirable when very large volume of
material is to be handled. It can be accomplished in two ways:
- In a tube or pipe (baffled pipe) through which the material flows
and in which there is a very backflow or recirculation.
- In a chamber (mixing chamber) in which a considerable amount of
hold up and recirculation occurs.

BATCH MIXERS
1. SHAKER MIXERS
• In these mixers, the material present in the container is agitated either
by an:
- Oscillatory motion (For small scale mixing) (Lab scale)
- Rotatory movement (For large scale work) (Industrial scale)
• These have limited use in industries.

2. IMPELLERS
• The distinction between impeller types is often made on the basis of
type of flow pattern they produce, or on the basis of shape and pitch of
blades. There are 3 basic components which produce flow patterns.
I. RADIAL COMPONENTS
• Radial components work in a direction vertical / perpendicular to the
impeller shaft.
II. AXIAL COMPONENTS
• It acts parallel to impeller shaft.
III. TANGENTIAL COMPONENTS
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 • It acts in a direction that is a tangent to the circle of rotation round the
impeller shaft.

CLASSIFICATION
I. PROPELLER MIXERS
• Propellers characteristically produce axial flow parallel to their axis of
rotation. Propellers are most effective when they can be run at high
speed in liquids of relatively low viscosity. Not used foe liquids whose
viscosity is greater than 50poise or 500 centi-poise.
• Propellers are effective of mixing viscous liquids e.g. glycerin and castor
oil.

CONSTRUCTION
• The agitator consists of a shaft to which many blades are attached
(usually three blades). The size of agitator is small as compared to the
size of container. The propeller rotates at a very high speed which is
8000rpm.
• The propeller pitch is defined as the distance of axial movement per
revolution. If no slippage occurs, usually the pitch is approximately equal
to the propeller diameter. The blades of the propeller do not have
constant pitch throughout the length sometimes high speed of propeller
may lead to undesirable vortex formation and entrapment of air.
(aeration)
• This problem can be avoided by:
- Attaching propeller shaft off set from the center.
- Mounting the propeller shaft from the side of vessel.
- Using push, pull propellers. In this two propellers of opposite pitch
are attached on the same shaft so that their rotatory effects are in
the opposite directions and cancel each other.
- Using baffles; which are generally vertical strings attached to the
side of vessel.
- Using vessel of shape other than a cylinder.
- It may be mounted at an angle.

USES

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 • They are useful in the preparation of suspensions of solids in liquid (if
solid contents are less than 10%)

DISADVANTAGES
• They are not used for liquids having viscosities more than 5000
centipoise.
• Not have constant pitch throughout the length.
• It is not useful when considerable shear is needed e.g. emulsification
II. TURBINE MIXER
• Turbine may produce radial or tangential flow or combination of these.
Majorly radial movement because of more shear.

CONSTRUCTION
• Turbine mixer uses a circular disk impeller to which many short (straight
or curved) vertical blades are attached. Most turbine impellers have flat
blades. Turbines having tilted blades produce an axial discharge quite
similar to that of propellers.
• The turbine impeller is rotated at a lower speed than propeller and the
ratio of the impeller and container diameter is low. It rotates at a speed
of 50-200rpm. Turbine impellers give rise to greater shear forces which
can be further increased by diffusion ring so that the discharged liquids
must pass through perforations.

TYPES OF TURBINE MIXERS

• Pitched blade turbine
• Curved blade turbine
• Disk blade turbine

USES
• Turbines can be operated satisfactorily in fluids 1000 times more viscous
than fluids in which propellers of comparable size can be used.
• Useful in the preparation of emulsions.
• Useful if solid contents are up to 60%.
III. PADDLE MIXERS
• Paddle produce tangential flow. Since circulation is primarily tangential,
the concentration gradient in the axial and radial directions may persist
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 even after prolonged operation. These mixers are effective in mixing
viscous liquids or semisolids which tend to sling to the surface.
• One of the promising hybrids of paddle mixer is dispersion. It has coaxial
blades one for macro mixing and other for micro mixing. Counter
rotation of macro-micro mixing element with variable speed is useful for
mixing extremely viscous materials, materials with high solid content, for
emulsification and homogenization. The equipment generates maximum
shear without vortex formation and minimal air entrapment.

CONSTRUCTION
• It uses an agitator consisting usually of flat blades attached to a vertical
shaft and rotating at a low speed of 50rpm or less. Paddles for more
viscous liquids generally have a number of blades often shaped to fit
closely to the surface of vessel, avoiding “deep-spots” and deposited
solids.
• Diameter of shaft is 50-80% of the diameter of mixing. Width of blade is
1/6th to 1/10th of its length.
• It is suitable for mixing thus liquids having viscosities of 1000 centipoise.
Gate paddles can be used for viscous liquids.
• The blades have a large surface area in relation to the container in which
they are employed; an aperture that permits them to pass close to the
tank wall.

TYPES OF PADDLE MIXERS

• Simple paddle • Anchor paddle
• Gate paddle • Helix paddle

DISADVANTAGES
• They are ineffective in suspending heavy solids because of absence of
axial flow.
IV. PLANETARY MOTION MIXERS
• Impart planetary mixing action that rotates on its own axis but also
travels in a circular path round the mixing vessel. The diameter of
agitator is not more than half to 2/3 of the diameter of vessel.
• The double rotation of element and its offset position reduces the dead
zone and avoids vortex formation.
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USES
• It is used for more viscous liquid mixing

3. AIR JETS
CONSTRUCTION AND WORKING
• In this apparatus air or any other gas is passed through a liquid at
surface level. The air bubbles rise and as a result, fluid at the bottom of
container is also forced to rise. Thus, may be better accomplished by
using tube. Hence mixing of different sections of liquids occurs. The
intense turbulence generated by jet produces intimate mixing.

USES
• Air jets are used for low viscosity, non-foaming, non-volatile and non-
reactive liquids.

4. FLUID JETS
• These are somewhat similar to sir jets but instead of air one of the
mixing component is pumped into other at high pressure. Thus, mixing is
achieved.

WORKING
• When liquids are to be pumped into a tank for mixing, the power
required for pumping often can be used to accomplish the mixing
operation, either partially or completely. In such a cases liquids are
pumped through nozzles arranged to permit good circulation of material
through the tank.
• Behave like propellers. Generate turbulent flow axially.

USES
• These are used for liquid/liquid mixing.

CONTINUOUS MIXERS
• Following are the examples of continuous mixing devices.

1. BAFFLED PIPE MIXERS

• It induces turbulence in fluid. However, recirculation is desirable when
overall fluctuations occur in the material fed to the mixer. In this, mixing

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 takes place mainly through mass transport in directions normal to that
of primary flow. Mixing in such system requires the careful control of
feed rate of raw materials if the mixture of uniform composition is to be
obtained.

2. MIXING CHAMBER WITH INDUCED RECIRCULATION

• It also induces the turbulence in fluids. However, recirculation is
desirable when overall fluctuations occur in the material fed to the
mixer. Since these fluctuations cannot be eliminated by simple
transverse mixing in a pipe.

3. CONTINUOUS MIXING TANK WITH VERTICAL SIDE WALL BAFFLES

• It consists of two zones one is above and second is below the impeller.
Net effect of such a device is similar to that obtained by the operation of
two tanks.

SEMI-SOLID MIXING

INTRODUCTION
• The process of missing solids in viscous fluids to achieve semi-solid
consistency as that of paste or dough is called semisolid mixing.
• Semi-solids: As the percentage of solid is increased or if highly viscous
fluids are employed, the solid-liquid system takes the consistency of a
paste or dough.

THEORY
• In mixing an insoluble solid with a liquid, a number of stages can be
observed as the liquid content is increased.
- Pellet and powder state
- Pellet state (when small amount of liquid is added powder balls up
and form pellet)
- Plastic state (mixture become homogenous)
- Sticky state (paste like material due to continuous incorporation
of liquid)

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 - Liquid state (decreased consistency, and increased rate of
homogenization)

EQUIPMENT FOR SEMI-SOLID MIXING

• Mixers for semi-solids may be divided into three main groups.

1. AGITATOR MIXER/ KNEADERS

• The agitator arms are designed to give a pulling and kneading force and
the shape and movement is such that material is cleaned from all sides
and all corners of the mixing vessel.

PRINCIPLE
• Kneaders operate by pushing masses of all materials past each other and
by squeezing and deforming them at the same time. Such mixers usually
have counter rotating blades or heavy arms that work the plastic mass.
Shear forces are generated by the high viscosity of mass and are
effective in disaggregation as well as distribution of solids in the fluid
vehicle.

SIGMA ARM MIXERS

• The shape of mixer blades resemble sigma “σ”. They are commonly used
for handling semisolids of plastic consistency.

CONSTRUCTION AND WORKING

• The two blades rotate towards each other and operate in a mixing vessel
which has a double trough shape, each blade fitting into a trough. The
two blades rotates at a different speeds, one usually about twice the
speed of other, resulting in a lateral pulling of the material and division
into the two troughs, while the blade shape and difference in speed
causes end to end movement.
• As with many other mixers, the vessel is jacketed for heating or cooling
and the blades can be hollow for the same purpose.
• The most common mixers used for handling of semi-solids and plastic
consistency are sigma arm and sigma blade mixers.

USES

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 • This form of mixer can handle even the heaviest plastic materials and
products such as pill masses, tablet, granule masses and ointments are
mixed usually.

2. SHEAR MIXERS/ MULLING MIXERS

• Mulling mixers are efficient in desegregation of solids but are typically
insufficient in distributing the particles uniformly through the entire
mass. These devices are suitable for mixing of previously mixed material
of uniform composition but containing aggregates of solids; is suitable
for mixing in these devices. If segregation occurs during milling, a final
remixing may be necessary.

PRINCIPLE
• The basic principle lies in the production of shear forces but the general
overall mixing efficiency is poor.

3. ROLLER MILL/ SHEAR MILL

• It consists of one or more rollers. The three rollers type seems to be
preferred. Rotor rotates at a speed of 3000-15000rpm

CONSTRUCTION AND WORKING

• In operation, rollers composed of a hard abrasion resistant material and
arranged to come into close proximity to each other are rotated at
different rates of speed. Material coming between the rollers is sheared
due to the difference in rate of movement of the two surfaces. The
material passes through from the hopper between rollers and is reduced
in size in the process.

USES
• Preparation of ointments, pastes and other semi-solids preparations.

4. ULTRASONIFIERS
• Limited output
• Very expensive
• Used in laboratory purposes i.e. emulsions and suspensions of high
consistency.

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 5. COLLOID MILL
• On the principle of high shear, which normally generate between the
rotor and the stator of mill. Speed of rotor is 3000 to 20,000 rpm.
Initially colloid mill is used for comminution of poorly wetted solid
suspensions and viscous emulsions.

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 FILTRATION AND CLARIFICATION

INTRODUCTION
FILTRATION
• Filtration may be defined as the separation of solid from a fluid by
means of a porous medium that retains the solid but allows the fluid to
pass.
• It leads to optically transparent liquid free from insoluble solids, colloidal
hazes or insoluble liquid.
CLARIFICATION
• This term is used when the solids present in the liquid is very small
(<1%), and filtrate is required product.

DIFFERENT TERMS
FEED OR SLURRY
• The suspension of solids and liquid to be filtered is called as feed or
slurry.
FILTER MEDIUM
• Porous medium through which slurry is forced to pass.

FILTER CAKE
• The solid collected on the filter medium is called as filter cake.

FILTRATE
• The clear liquid which passes through the filter is called filtrate.

CAKE FILTRATION
• When solids collected on the filter medium is the desired product then
the process is known as cake filtration.

FACTORS AFFECTING FILTRATION

• Filtration is affected by the characteristics of the slurry, including:
1. The properties of the liquid, such as density, viscosity, and
corrosiveness.
2. The properties of solid, for example, particle shape, particle size,
particle size distribution, and rigidity or compressibility of solid.

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 3. The proportion of solids in the slurry.
4. Whether the objective is to collect the solid, the liquid, or both.
5. Whether the solids have to be washed free from the liquid or a
solute.

RATE OF FILTRATION
• All other things being equal, the object of the operation is to filter the
slurry as quickly as possible.
• The factors affecting rate of filtration is known as Darcy’s law and may
be expressed as:
dv 𝑃
=𝐾𝐴
dt 𝜇𝑙
- Where, V = volume of filtrate, t = time of filtration, K = constant
for the filter medium and filter cake, A = area of filter medium, P =
pressure drop across the filter medium and filter cake, u =
viscosity of the filtrate and l = thickness of cake.
FACTORS AFFECTING RATE OF FILTRATION
I. PERMEABILITY COEFFICIENT
• The constant (K) represents the resistance of both the filter
medium and the filter cake. As the thickness of the cake increase,
the rate of filtration will decrease. Also, the surface area of the
particles. the porosity of the cake, and rigidity or compressibility
of the particles could affect the permeability of the cake.
II. AREA OF FILTER MEDIUM
• The total volume of filtrate flowing from the filter will be
proportional to the area of the filter. The area can be increased by
using larger filters. In the rotary drum filter, the continuous
removal of the filter cake will give an infinite area for filtration.
III. PRESSURE DROP
• The rate of filtration is proportional to the pressure difference
across both the filter medium and filter cake.
• The pressure drop can be achieved in a number of ways:
GRAVITY
- A pressure difference could be obtained by maintaining a
head of slurry above the filter medium. The pressure
developed will depend on the density of the slurry.

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 VACUUM
- The pressure below the filter medium may be reduced
below atmospheric pressure by connecting the filtrate
receiver to a vacuum pump and creating a pressure
difference across the filter.
PRESSURE
- The simplest method being to pump the slurry into the filter
under pressure.
CENTRIFUGAL FORCE
- The gravitational force could be replaced by centrifugal
force in particle separation.
IV. VISCOSITY OF FILTRATE
• It would be expecting that an increase in the viscosity of the
filtrate will increase the resistance of flow, so that the rate of
filtration is inversely proportional to the viscosity of the fluid.
• This problem can be overcome by two methods:
a. The rate of filtration may be increased by raising the
temperature of the liquid, which lowers its viscosity.
However, it is not practicable if thermolabile materials are
involved or if the filtrate is volatile.
b. Dilution is another alternative, but the rate must be
doubled.
V. THICKNESS OF FILTER CAKE
• The rate of flow of the filtrate through the filter cake is inversely
proportional to thickness of the cake. Preliminary decantation
may be useful to decrease the amount of the solids.

FILTER MEDIA
• The surface upon which solids are deposited in a filter is called the
“Filter medium”
• Properties of ideal filter medium:
1. It must be capable of delivering a clear filtrate at a suitable
production rate.
2. It must withstand the mechanical stresses without rupturing or
being compressed.
3. No chemical or physical interactions with the components of the
filtrate should occur.
4. It must retain the solids without plugging at the start of filtration.
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 5. Sterile filtration imposes a special requirement since the pore size
must not exceed the dimension of bacteria or spores.
CLASSIFICATION OF FILTER MEDIA
I. WOVEN FILTERS
• These include:
a. Wire screening.
b. Fabrics of cotton, wool and nylon.
• Wire screening e.g. stainless steel is durable, resistance to
plugging and easily cleaned.
• Cotton is a common filter, however, Nylon is superior for
pharmaceutical use, since it is unaffected by mold, fungus or
bacteria and has negligible absorption properties.
II. NON- WOVEN FILTERS
• Filter paper is a common filter medium since it offers controlled
porosity, limited absorption characteristic, and low cost.
III. MEMBRANE FILTERS
• These are basic tools for micro-filtration, useful in the preparation
of sterile solutions. These filters are made by casting of various
esters of cellulose, or from nylon, Teflon, polyvinyl chloride. The
filter is a thin membrane with millions of pores per square
centimeter of filter surface.
IV. POROUS PLATES
• These include perforated metal or rubber plates, natural porous
materials such as stone, porcelain or ceramics, and sintered glass.
FACTORS AFFECTING IN THE SELECTION OF FILTER MEDIA
• While selecting the filter media the following factors must be taken into
considerations
- Size of the particles to be filtered.
- Amount of the liquid to be filtered.
- Nature of the product to be filtered i.e. a solution suspension or a
viscous preparation.
- Purpose of filtration i.e. only to get clear preparation or to get a
clear sterile preparation.

FILTER AID
• Usually, the resistance to flow due to the filter medium itself is very low
but will increase as a layer of solids builds up, blocking the pores of the
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 medium and forming a solid cake.
• The objective of the filter aid is to prevent the medium from becoming
blocked and to form an open, porous cake, so reducing the resistance to
flow of the filtrate. The particles must be inert, insoluble,
incompressible, and irregular shaped.
- If too little filter aid is used, the resistant offend by the filter cake
is greater than if no filter aid is used, because of added thickness
to the cake.
- If high amounts of filter aids arc added, the filter aid merely adds
to the thickness of the cake without providing additional cake
porosity.
- At low concentration of filter aid, the flow rate is slow because of
low permeability.
- As the filter aid concentration increases, the flow rate increases
and peaks off. Beyond this point the flow rate decreases as the
filter aid concentration is increased.
• Filter aids may be used in either or both two ways:
1. PRE- COATING TECHNIQUE: By forming a pre-coat over the filter
medium by filtering a suspension of the filter aid.
2. BODY- MIX TECHNIQUE: A small proportion of the filter aid (0.1-
0.5 %) is added to the slurry to be filtered. This slurry is
recirculated through the filter until a clear filtrate is obtained,
filtration then proceeds to completion.
• The following filter aids may be used:
- Diatomite (Kieselguhr), obtained from natural siliceous deposits.
- Perlite, it is an aluminum silicate.
- Cellulose and Asbestos.

INDUSTRIAL FILTERS
Four groups may be listed:
1. Gravity filters 3. Pressure filters
2. Vacuum filters 4. Centrifugal filters
1. GRAVITY FILTERS
• Employing thick granular beds are widely used in water filtration e.g.
Sand Filter.
• This device is composed of two chambers, the upper chamber, and the
lower chamber. The upper chamber is the part where you pour in your
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 contaminated water, and the lower chamber will then be the finish line
where your contaminated water is now turned into filtered water.
• The Gravity Water Filter is perfect because of its convenience, and it
does no longer require plumbing or electricity for it to function.
WORKING
• The upper chamber of the gravity water filter
contains an element that takes care of the
filtering process of your contaminated water.
Basically, that element is composed of
microscopic pores that disable the
contaminants and other pollutants to pass
through it, which leaves only the water to be
able to pass through that microporous element
going to the lower chamber. Now, you had your filtered water
which is ready and made safe for drinking.
ADVANTAGES
• The gravity water filtration system is effective and efficient. It is
simple and very functional.
• There are various sizes to choose from, depending on your needs.
• It requires less maintenance. It only needs filter replacement once
or twice each year, depending on the suggestion of the
manufacturer.
• The system does not need electricity.
DISADVANTAGES
• The parts of the gravity water filter can be costly especially for
those who are in tight budget.
• Limited filtration capacity.
• Some gravity filter takes time to clean the water, while others can
do the cleaning really quick.
TYPES OF GRAVITY WATER FILTERS
a. Ceramic Gravity Water Filter.
b. Stainless Steel Gravity Water Filter.
c. Gravity Bag Water Filter.

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 2. VACUUM FILTERS
• Vacuum filters operate practically at higher pressure differentials
than gravity filters.
• Rotary vacuum filter and the leaf filter are most extensively used.
I. THE LEAF FILTER
• The leaf filter is consisting of a frame enclosing a drainage
screen or grooved plate, the whole unit being covered with
filter cloth.
• The outlet for the filtrate connects to the inside of the frame,
the general arrangement is shown in the Fig. which represents
a vertical section through the leaf. The frame may be circular,
square or rectangular shapes.
OPERATION
- The leaf filter is immersed in the slurry and a receiver and
a vacuum system connected to the filtrate outlet.
ADVANTAGES
i. The slurry can be filtered from any vessel.
ii. The cake can be washed simply by immersing the filter in a
vessel of Water.
iii. Removal of the cake is facilitated by the use of reverse air flow.
Fig. Filter leaf
iv. The filter can be modified by employing a suitable number of
unites.
v. The leaf filter is most satisfactory if the solids content of the slurry
is not too high, 5 % being a suitable maximum.
vi. Labor costs for operating the filter are comparatively moderate.

• An alternative method is to enclose the filter leaf in a special vessel into

which the slurry is pumped under pressure. A number of leaves are
connected to a common outlet, to provide a large area for filtration e.g.
Sweetland filter.

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 II. ROTARY VACUUM FILTER (ROTARY FILTER)
• In large –scale operation, continuous
operation is sometimes desirable, and it may be
necessary to filter slurries containing a high
proportion of solids.
• The rotary filter is continuous in operation and has a
system for removing the cake that is formed, so, it is
suitable for use with concentrated slurries.
• It is a metal cylinder mounted horizontally, the curved surface being a
perforated plate, supporting a filter cloth. Internally, it is divided into
several sectors and a separate connection is made between each sector
and a special rotary valve.
OPERATION
• The drum is immersed to the required depth in the slurry, which is
agitated to prevent settling of the solids, and vacuum is applied to
those sectors of the drum which is submerged.
• A cake of the desired thickness is produced by adjusting the speed
of rotation of the drum. Each sector is immersed in turn in the
slurry and the cake is then washed and partially dried by means of
a current of air.
• Finally, pressure is applied under the cloth to aid the removal of
the cake.
• Removal of the washed and partially dried cake is affected by
means of a doctor knife.
RESIDUAL CAKE
• The suspended solids deposits on the filter drum as a cake and as
rotation continues, vacuum holds the cake at the drum surface. This is
followed by washing and further drainage in drying zone.
• As the cake moves towards the discharge point, it may be scraped from
drum or it may be supported by strings until it breaks free under
gravitational forces (cake removal zone).
• The cake discharge may be done through a scraper, belt, roll or a string.
Scraper discharge mechanisms will suit cake that could be scraped
readily.
- Roller discharge mechanisms are better for thixotropic cakes.

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 - A string discharge filter is useful in the manufacturing of
antibiotics when removal of cake of mould mycelia is necessary.
SUMMARY OF THE PROCESS
• The drum is dipped into the slurry and vacuum applied to the
outlet, which is connected to the filtrate receiver. When the cake
has formed, the cake drained or partially dried by vacuum.
• The drum is sprayed with water to wash the cake. Retaining the
vacuum connection drains the cake and produces partial dryness
then, removed by a doctor knife.
• When the solids of the slurry are too much that the filter cloth
becomes blocked with the particles, a pre-coat filter may be used.
A pre-coat of filter aid is deposited on the drum prior to the
filtration process.
ADVANTAGES
• The rotary filter is automatic and is continuous in operation, so
that the labor costs are very low.
• The filter has a large capacity, so it is suitable for the filtration of
highly concentrated solutions.
• Variation of the speed of rotation enables the cake thickness to be
controlled.
• Pre-coat of filter aid could be used to accelerate the filtration rate.
DISADVANTAGES
• The rotary filter is a complex piece of equipment, with many
moving parts and is very expensive.
• In addition to the filter itself, some accessories are connected, e.g.
a vacuum pump, vacuum receivers, slurry pumps and agitators are
required.
• The cake tends to crack due to the air drawn through by the
vacuum system, so that washing and drying are not efficient.
• Being a vacuum filter, the pressure difference is limited to 1 bar
and hot filtrates may boil.
• It is suitable only for straight- forward slurries
USES

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 • The rotary filter for continuous operation on large quantities of
slurry.
• Suitable for slurry contains considerable amounts of solids in the
range 15-30%.
• Examples of pharmaceutical application include the collection of
calcium carbonate, magnesium carbonate, and starch, and the
separation of the mycelium from the fermentation liquor in the
manufacture of antibiotics.
3. PRESSURE FILTERS
• Due to the formation of cakes of low permeability, many types of
slurry require higher pressure difference for effective filtration
than can be applied by vacuum techniques.
• Pressure filters are used for such operations.
• However, high operational pressures, may prohibit continuous
operation because of the difficulty of discharging the cake whilst
the filter is under pressure.
• Examples are the
- Sweetland filter
- Plate and frame filter press.

PLATE AND FRAME FILTER PRESS

• This press is made up of two units,
known respectively as plates and
frames, with a filter medium, usually
filter cloth, between the two.
• The frame is open, with an inlet for
the slurry, while the plate has
grooved surface to support the filter
cloth, and with an outlet for the filtrate.
OPERATION
• The slurry enters the frame from the feed channel.
• The filtrate passes through the filter medium on to the surface of the
plate while the solids form a filter cake in the frame.
• The filtrate then drained down the surface of the plate, between the
projections on the surface and escapes from the outlet.

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