DOSAGE FORM DESIGN I

Heat Transfer, Drying & Sublimation

Mr. Rajesh
 Learning Outcomes
• At the end of this topic, students should be able to :

Explain the principles of heat transfer, drying & sublimation

Describe the types of equipments used in drying &

mechanisms of drying

Explain the selection of appropriate equipments for drying

materials
 Topics
1. Definitions of heat & flow
2. Mechanisms of heat transfer

3. Non - thermal methods of drying

4. Purpose of drying

5. Behavior of Solids During Drying

6. Different types of dryers

 Heat Transfer
• Heat: Heat is a form of energy.

• Sources of heat is used for industrial scale operations

- Steam
- Electric power

• Heat Transfer:

Heat flow from high temperature regions to low

temperature regions
 Application

• Heat transfer process is observed in the following

pharmaceutical operations:

- Evaporation Heat Transfer

- Distillation Mechanisms
- Drying
- Granulation
1. Conduction
- Crystallization
2. Convection
- Sterilization
3. Radiation
Conduction
• Heat flow/transfer by momentum of individual atoms or
molecules without mixing
Eg: heat transfer in copper wire

• Conduction is limited to solids

Convection
• Heat flow by mixing of warmer portions with cooler portions of
the same material
Eg: heat transfer in water or any solution

• Restricted to the flow of heat in fluids (liquids/ gases)

Radiation
• Heat flows through space by means of EM waves (energy
transfer)
• Eg: Sun light
 Heat Transfer
• These 3 mechanisms may operate simultaneously

• Case:
• In oven, hot air is circulated by fan so as to transfer heat by
forced convection

• Simultaneously, heat is transferred from the shelf to the

material in contact (conduction)

• Heat also radiates from hot walls of the oven

• Heat can flow only when there is a temperature gradient,

i.e., heat flows from a hot surface to a cold surface

• Rate = driving force/resistance

 • Driving force: Temperature difference

- The greater the temperature drop, the greater will be

the rate of heat flow
- The flow of heat will also depend on the conductivity
of the materials through which it is flowing
- Eg: Conduction of heat is faster through an iron rod
than through a wooden log

Thickness of the surface (m)

Resistance 
constant X surface area
= L/ Km A Fourier’s law
 Drying
• The removal of a liquid (small portions) from a material by the
application of heat

- It is accomplished by the transfer of a liquid from a

surface into an unsaturated vapor phase

• Drying and Evaporation are distinguishable merely by the

relative quantities of liquid removed from the solid
 Drying
• Non-thermal methods of drying.

• The expression of a solid to remove liquid (the squeezing

of a wetted sponge)

• The extraction of liquid from a solid by use of a solvent

• The desiccation of moisture from a solid by placing it in

a sealed container with a moisture-removing material
(silica gel in a bottle)
 Purpose of Drying

• Drying is used in pharmaceutical manufacturing as a unit

process in the preparation of granules, which can be
dispensed in bulk or converted into tablets or capsules

- Another application is found in the processing of

materials

- Eg:
- Dried aluminum hydroxide
- Spray drying of lactose
- preparation of powdered extracts
1.To reduce bulk/weight – lower the cost of
transportation/storage

2. Aids in the preservation of animal & vegetable drugs by

minimizing mould/bacterial growth in materials

3. Facilitating comminution by making the dried substance

far more friable than the original water-containing drug

4. Dried products often are more stable than moist ones

5. The drying reduces the chemical reactivity

 Drying of Solids
The moisture in a solid can be expressed on a wet-
weight or dry-weight basis

Loss on Drying (LOD):

Loss on drying, commonly referred to as LOD, is an expression of

moisture on a wet-weight basis
% LOD = (weight of water in sample / total weight of the
sample) x 100
 Moisture Content

The moisture in a wet solid is that calculated on a dry-

weight basis. This value is referred as moisture content, or MC:

%MC = (weight of water in sample /

weight of dry sample) x 100

If exactly 5 g of moist solid is brought to a constant

dry weight of 3 g:

%MC = (5 – 3 / 3) x 100 = 66.7%

Whereas LOD = (5 – 3/ 5) x 100 = 40%

 Behavior of Solids During Drying
When a wet solid is first placed in a drying oven, it begins to
absorb heat & increases in temperature

At the same time, moisture begins evaporating & thus tends

to cool the drying solid

After a period of initial adjustment, rates of heating &

cooling become equal & temp. of the drying material
stabilizes

This period of initial adjustment is shown as segment AB in

Figures
 Drying Curves

A Critical
Moisture
B
Content
Second
Critical
C Point

D Equilibrium
Moisture Content
E

First Falling
Rate Period

DRYING TIME
 Drying Curves

Critical Moisture Content

B C

Second Critical Point

Equilibrium
First Falling Moisture Content
Rate Period

E
MOISTURE CONTENT
 Drying Curves
At point B, the temperature is stabilized & remains constant
as long as there is a film of moisture remaining at the surface
of the drying solid

Between points B & C, the moisture evaporating from surface

is replaced by water diffusing from the interior of the solid at
a rate equal to the rate of evaporation

The rate of drying is constant & time BC is the constant rate

period
At point C, surface water is no longer replaced at a rate fast
enough to maintain a continuous film

Dry spots begin to appear & rate of drying begins to fall off
The moisture content at which this occurs is referred to as the
critical moisture content
Between points C & D, number & area of dry spots continue
to grow & rate of drying falls steadily

The time CD is referred to as the first falling rate period

At point D, the film of surface water is completely evaporated,

& rate of drying depends on rate of diffusion of moisture to
surface of solid

Point D is referred to as the second critical point

Between points D & E, rate of drying falls even more rapidly
than first falling rate & time DE is called second falling rate
period
 When the drying rate is equal to zero, starting at point
E, the equilibrium moisture period begins, & solid is in
equilibrium with its surroundings, i.e., its temp &
moisture content remain constant

Continued drying after this point is a waste of time &

energy

• Dryers may classified as:

1. Static bed dryers – Tray dryer
2. Moving bed dryers – Drum dryer
3. Fluidized bed dryers- Fluid bed dryer

4. Pneumatic dryers – Spray dryer

 Tray Dryer
Tray dryers are sometimes called shelf, cabinet, or
compartment dryers

This dryer consists of a cabinet in which the material to

be dried is spread on tiers of trays

The number of trays varies with the size of the dryer

Ovens/Dryers of laboratory size may contain as few as

three trays, whereas larger dryers often hold as many as
twenty trays
Each tray is square or rectangular & about 4 to 8 square
feet in area

Trays have at least 1.5 inches clearance

The trays used have solid, perforated, or wire mesh

bottoms
 H

T: Tray, H: Heater, F: Fan, S: Air inlet, E: Air outlet

 Fluidized bed dryer
Gas is allowed to flow upward through a bed of
particulate solids at a velocity greater than the settling
velocity of the particles,
solids are buoyed up & become partially suspended in the
gas stream
The resultant mixture of solids & gas behaves like a
liquid & the solids are said to be fluidized

The important factor is that it produces good contact

between air and solid particles
 Working:

The air is heated to required temp in an air heater &

flows upward through wet material, which is contained
in a drying chamber fitted with a wire mesh support at
the bottom

The air flow rate can be adjusted & a bag collector filter
is provided at the top of the drying chamber to prevent
carry over of fine particles

Dryer capacities range from 5 kg to 200 kg & average

drying time is about 20 to 40 min
Applications

The fluidization technique is efficient for the drying of

granular solids, because each particle is completely
surrounded by the drying gas
Advantages
1.Gives high drying rate-15 times faster
than tray dryer
2.Drying takes place from individual
particles
3.Can be used for drying any powdered
material but mostly used for drying
granules
 Spray dryer

Spray dryers can handle only fluid materials such as

solutions, slurries & thin pastes
The cyclone spray dryer is the most commonly used.

The spray drier provides a large surface area for heat and mass
transfer by atomizing the liquid to small droplets

Typically, a liquid product concentrate is pumped to the atomizing

device where it is broken into small droplets

These are sprayed into a stream of hot air, so that each particle
dries to a solid particle

 The dry powder is separated from the moist air in

cyclones by centrifugal action.
Spray dryer
 Drum Dryer
It consists of a drum 0.75–1.5 m in diameter & 2–4 m in
length, heated internally, usually by steam & rotated on
its longitudinal axis
The liquid is applied to the surface and spread to
a film
Firstly, the drum dips into a feed pan
As the drum starts rotating; the spreader spreads
the liquid evenly; the drying rate is adjusted by using
suitable speed of rotation and drum temperature

Finally, the product is scrapped from the surface of

the drum by means of a knife scraper
Drum Dryer
Specialised drying methods
Freeze Dryer
Many products deteriorate if dried in air at normal
atmospheric pressures

Freeze drying depends on the phenomenon of

sublimation, whereby water passes directly from
solid state(ice) to the vapor state without passing
through the liquid state
The material to be dried is first frozen & then
subjected to a high vacuum (to drop the pressure
below the triple point) so that the frozen liquid
sublimes leaving solid, dried components of original
liquid
Application:

Blood serum, plasma, antibiotics, hormones, bacterial

cultures, vaccines & many foodstuffs are dehydrated by
freeze drying also referred to as lyophilization

The dried products can be readily re-dissolved or re-

suspended by addition of water prior to use
Reference
L.Lieberman and H.A.Lachman, Theory and Practice of
Industrial Pharmacy