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FREEZE DRYING & FREEZE

CONCENTRATION

Satuan Operasi Industri Pangan IV


Ilmu & Teknologi Pangan UNS

Freeze drying or lyophilization is the removal of water by


sublimation from frozen state (ice). In this process, the
food is first frozen and then subjected to high vacuum,
whereby the water ice sublimates (i.e. evaporates directly,
without melting).
The water vapor released is usually caught on the surface
of a condenser at very low temperature.
As a physical phenomenon and a laboratory technique,
freeze drying was known already at the end of the 19th
century, but it did not develop into an industrial process
until after World War 2 ( Flosdorf, 1949 ; King, 1971 ).
The first commercial applications have been in the
pharmaceutical industry (antibiotics, cells, blood plasma
etc.), which still is the largest user of freeze drying.
Industrial freeze drying of foods started in the late 1950s.

In the food industry, interest in commercial freeze


drying arises from the superior quality of the freezedried products as compared with foods dehydrated
by other methods.
Freeze drying is carried out at low temperature, thus
preserving flavor, color and appearance, and
minimizing thermal damage to heat sensitive
nutrients.
Freeze drying is, however, an expensive method of
dehydration. It is economically feasible only in the
case of high added-value products and whenever the
superior quality of the product justifi es the higher
production cost

Sublimation of Water
Sublimation is the direct transition from solid state to
gaseous state without melting. Sublimation occurs at a
definite range of temperatures and pressures, depending on
the substance in question

The phase diagram of pure water indicates that


sublimation of water ice can occur only if the vapor
pressure and temperature are below those of the
triple point of water, i.e. below 611.73 Pa and 0.01C
respectively
Freeze drying occurs in two stages ( Pikal et al., 1990
; Oetjen, 1999 ). The first stage is sublimation drying
in which sublimation of the frozen water (ice
crystals) occurs. Normally, most of the water in the
food is removed at this stage.
The second stage is desorption drying during which
most of the water adsorbed on the solid matrix is
removed. Typically, freeze drying is carried to a final
moisture content of 13%

The rate of ice sublimation dw/dt is:

Let us consider heat transfer first. The rate of heat


supply q (J/s) must be equal to the rate of
sublimation (kg/s), multiplied by the latent heat of
sublimation s (J/kg):

On the other hand, q is given by the rate of


conductive transport from the slab surface to the
sublimation front through the dry layer:

Combining equations (23.3) and (23.2) and


integrating from z = 0 to z = Z (total thickness of the
slab, m), we obtain:

Freeze Concentration
When a solution or a liquid food is frozen, water is
separated from the rest of the solution as crystals of
pure water ice. Subsequently, the mixture can be
separated into ice and a concentrated solution.
Since freeze concentration occurs without heating
and without boiling, the thermal damage and loss of
volatile aroma that characterize evaporative
concentration are completely avoided.
Thus, freeze concentration is, in theory, particularly
suitable for heat sensitive liquid foods containing
volatile aromas. Coffee extracts, fruit juices and their
recovered essences would be natural candidates for
freeze concentration.

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