A SEMINAR REPORT ON

FREEZE DRYING
PREPARED BY :KARAN SHITOLE

GUIDED BY :MANJEET MUKHI

DEPARTMENT OF CHEMICAL ENGINEERING,

FACULTY OF TECHNIOLOGY & ENGINEERING,
THE MAHARAJA SAYAJIRAO UNIVERSITY OF BARODA.

2015-16

INTRODUCTION
Freeze drying is a relatively recent method of preserving food. It involves
freezing the food, then removing almost all the moisture in a vacuum chamber,
and finally sealing the food in an airtight container.
Freeze dried foods can be easily transported at normal temperatures, stored for a
long period of time, and consumed with a minimum of preparation. Once
prepared, freeze-dried foods have much the same look and taste as the original,
natural products.
The freeze-drying process was developed during World War II as a method of
preserving
blood
plasma
for
battlefield
emergencies
without
requiring refrigeration or damaging the organic nature of the plasma.
Because as much as 98% of the water content has been removed, the food is
extremely lightweight this significantly reduces the cost of shipping. Also as amount
of water is very less, it reduces the risk of contamination and growth of any bacteria
or yeast which require water as a medium.
This also makes it popular with boaters, hikers, astronauts etc.

http://science.howstuffworks.com/innovation/edible-innovations/freeze-drying.htm

THE PROCESS
The fundamental principle in freeze-drying is sublimation, the shift from a solid
directly into a gas.
Water freezes at 0 o C and boils at 100 o C at atmospheric pressure (1 atm) . But if
we increase the temperature above 0 o C while keeping the atmospheric pressure
below .06 atm , the water is warm enough to thaw, but there isn't enough pressure for
a liquid to form. It becomes a gas.
This is exactly what a freeze drying machine does.

http://science.howstuffworks.com/innovation/edible-innovations/freeze-drying.htm

 The material to be dried is kept on the shelves of the chamber , it is sealed and the
compressor begins to run to lower the temperature. The water present freezes on the
molecular level.
Vacuum pump is started in order to decrease the pressure so the frozen water is
directly converted to water vapor. Also small amount of heat is added to control the
process. This vapor is carried to the condenser and separated.

WANG Wei, CHEN Mo and CHEN Guohua .Issues in Freeze Drying of Aqueous Solutions. Chinese Journal of Chemical Engineering, 20(3) 551559
(2012).

TYPES OF FREEZING
The first one is when it forms an Eutectic mixture where the substance freezes at a
temperature less than that of water. Correspondingly we have Eutectic Temp (TC)
The second when is when it forms a glassy substance, very viscous before freezing .This is
called Glass Transition Temp (TG). It is not recommended.
All liquid material undergo either one of the above two freezing.

Rapid cooling results in small ice crystals, useful in preserving structures to be

examined microscopically, but resulting in a product that is more difficult to freeze dry.
Slower cooling results in larger ice crystals and less restrictive channels in the matrix
during the drying process.
WANG Wei, CHEN Mo and CHEN Guohua .Issues in Freeze Drying of Aqueous Solutions. Chinese Journal of Chemical Engineering, 20(3) 551559 (2012).

FREEZE DRYING METHODS

Manifold Drying :- Flasks, ampoules or vials are individually attached to the ports of a
manifold or drying chamber.

Batch Drying :- In batch drying, large numbers of similar sized vessels containing like
products are placed together in a tray dryer.
Bulk Drying :- The product is poured into a bulk pan and dried as a single unit.

Sandip Khairnar, Rajesh Kini2, Mallinath Harwalkar, Dr. Kishor salunkhe1, Dr.S.R.Chaudhari. IJRPS 2013, 4(1), 76 94. International Journal of Pharmacy and Science

MATERIALS USED IN FREEZE-DRYING

Agent

Examples

Buffer

Phosphate buffers tris, citrate, and histidine buffers.

Bulking Agents

sucrose or one of the other disaccharides

Stabilizer

Sucrose, Glucose, lactose, maltose

Tonicity Adjusters

sucrose, glycine, glycerol, sodium chloride.

Buffers are used in order to maintain pH of the solution.

Bulking Agents provide mechanical strength as well as form an elegant cake structure.
Stabilizer are used for stabilizing the solution throughout the process.
Tonicity Adjusters are used when the need for such a formulation may be dictated by
either the stability requirements of the bulk solution or those for the route of
administration.
WANG Wei, CHEN Mo and CHEN Guohua .Issues in Freeze Drying of Aqueous Solutions. Chinese Journal of Chemical Engineering, 20(3) 551559 (2012).

CASE STUDY :-
Comparison of drying process for apple peels:

Two batches of peels (10 kg per batch) were collected. Immediately after mechanical
peeling, the peel fractions (pieces around 5 5 mm, with some attached pulp) were packed
into polyethylene bags, frozen, transported to the laboratory, and stored in a freezer until
used. The sample corresponds to a pool of apples randomly chosen from different
commercial plantations from the same geographical zone.
M. Henrquez, S. Almonacid, M. Lutz, R. Simpson & M. Valdenegro. CYTA-Journal of food. 11:2, 127-13.5 Comparison of drying process for apple peels.

RESULTS AND DISCUSSION

Moisture content of F and S were 874.4 and 909.0 g/kg sample (wet basis),
respectively. The moisture content was similar in all the apple peel products,
independently of the drying system used , and ranged from 26.9 to 34.0 g/kg
(prepared with F) and from 28.8 to 30.3 g/kg (prepared with S).
The aW (activity of water) is a major determinant of the product stability, since
water acts as a solvent to support enzymatic and chemical reactions that influence
antioxidant stability, color, flavor, and nutritional value. It is used to predict the
stability and safety of foods with respect to microbial growth, rates of
deteriorative reactions, and chemical/physical properties.

M. Henrquez, S. Almonacid, M. Lutz, R. Simpson & M. Valdenegro. CYTA-Journal of food. 11:2, 127-13.5 Comparison of drying process for apple peels.

ADVANTAGES

Stored in dry state, so stability problem is few.

Product is dried without elevated temp.
Good for O2 & air sensitive drugs.
Rapid reconstitution time.
Constituents of dried material remain homogenously dispersed.
Product is process in the liquid form.
Storage of dry material is less expensive than solution form.
In some specialized laboratories, scientists are developing more sophisticated
processes that combine freeze-drying technology with electron microscopy,
biochemistry, and refined surgery.
At the same time, the cosmetics industry is increasing its use of lyophilization to
help prepare beauty masks, hair dyes, and sophisticated supports for face creams.
Chemical industries also are beginning to use freeze-drying to prepare refined
chemicals, catalysts, and selective filters. Cosmetic industry also uses this process
Freeze-drying can preserve food , increase its shelf life and make it very
lightweight.
If a freeze-dried substance is sealed to prevent the re absorption of moisture, the
substance may be stored at room temperature without refrigeration, and be
protected against spoilage for many years.

DISADVANTAGES

Volatile compounds may be removed by high vacuum.

Expensive unit operation because pumps are more expensive.
Stability problems associated with individual drugs.
Some issues associated with sterilization & sterility assurance of dry chamber &
aseptic loading of vials into chamber.
Freeze-drying is facing difficult challenges as the sensitivity, complexity, and
price of treated products steadily rise.
New antibiotics and drugs, immunological products, substances derived from
genetic engineering, high molecular weight proteins, and sophisticated peptides
are very fragile, difficult to freeze, and all highly sensitive to residual moisture
content.
Amorphous (glassy) materials do not have a eutectic point, but do have a critical
point, below which the product must be maintained to prevent melt-back or
collapse during primary and secondary drying.
Large objects take a few months to freeze-dry.
If too much heat is added, the materials structure could be altered.
Small ice crystals produce pores with lower volumesurface area, thus resulting
in lower diffusive flux and slower sublimation rates.