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# Institution of Chemical Engineers
Trans IChemE, Vol 78, Part C, December 2000

A COMPARISON OF EVAPORATIVE AND CONVENTIONAL

FREEZING PRIOR TO FREEZE-DRYING OF FRUITS
AND VEGETABLES
S. GHIO, A. A. BARRESI and G. ROVERO
Dipartimento di Scienza dei Materiali ed Ingegneria Chimica, Politecnico di Torino, Torino, Italy

A
detailed comparative analysis was carried out on freeze-drying coupled with an
evaporative freezing and a conventional freezing step, using on-line monitoring of
several fruit and vegetable weights vs. time. The experimental work was based on the
use of two weighing cells: a traditional one and a prototype capacitive balance. The work
showed that process rates differed because of product texture, water and sugar content, cooling
temperature and freezing velocity. Different water release mechanisms were identiŽ ed.

Keywords: evaporative-freezing; freeze-drying; process kinetics; residual water; fruits;

vegetables.

INTRODUCTION been improved by concentrating the liquid before spraying

Through the passage of time, people have learned that water
removal increases the storage stability of perishable
products. Recent scientiŽ c studies have shown that water,
as the dominant component of foods, provides the critical
environmental factor necessary for the ubiquitous biologi-
cal, biochemical and biophysical processes that degrade
foods and ultimately make them unŽ t for human consump-
tion. Any reduction in water content that retards or inhibits
such processes will give a major contribution to food
preservation.
Preserving biological products by reducing their water
content can be achieved by several dehydration techniques.
Among these methods, freeze-drying is considered as the
reference process for manufacturing high-quality dehydrated
products. That is due to the peculiar freeze-drying condi-
tions: sublimation of ice coupled with a low process
temperature. The main advantages of the process are the
preservation of most of the initial raw material properties
such as shape, appearance, taste,  avour, texture, biological
activity, etc. and the high re-hydration capacity of the freeze-
dried products. Indeed, the use of freeze-drying in food
industries is restricted to high added-value products such as
coffee, teas, ingredients for ready-to-eat foods (vegetables,
pasta, meat, Ž sh, etc.), several aromatic herbs and speciality
foods.
Generally the freezing step is carried out in a stream of
cold air or by conduction using refrigerated plates: it is
acknowledged as a slow step in the freeze-drying process.
Rapid freezing of liquid foods was investigated by
Mumenthaler and Leuenberger1–2. In their work the product
was sprayed into a cylindrical tower in which refrigerated
coils were also inserted. The dried product thus obtained
was characterized by lower  avour than the normal freeze-
dried product, even though the  avour retention may have
it into the tower. An alternative rapid freezing method can
be obtained by auto-evaporation: evaporative freezing by
vacuum-drawing on batches was applied both to solids and
liquids3–5. Choosing between rapid freezing and slow freez-
ing depends on the product’s characteristics. Generally the
faster the freezing rate, the smaller the ice crystals and
hence, the longer the primary drying period. This has the
advantage of giving a higher Ž nal product quality. However,
each process and product has its own speciŽ cations.
If a biological material with very moist surfaces is
considered, reducing the pressure from atmospheric to
below the value corresponding to the vapour pressure at
the material surface, facilitates evaporating water from the
exposed surfaces. The water retained in the material Ž rst
cools and then freezes by an almost adiabatic evaporation,
provided the residual pressure is lower than the saturated
vapour pressure of water. The evaporation of the moisture
requires considerable latent heat and produces rapid cooling.
Freezing under vacuum is signiŽ cantly affected by the
material piece size and the degree of vacuum. Different
methods of evaporative freezing are described by Mellor3,
who also reported some applications. This technique is often
damaging to the product appearance and structure; positive
exceptions are materials with a high moisture content at the
surface. In fact, some ebullition may occur during the
pressure reduction period; large cracks may subsequently
form.
The main applications of freeze-drying coupled with
evaporative freezing are provided by the food industry.
Higher freezing velocity and lower maintenance and equip-
ment costs are the major advantages of this drying method;
in addition, a signiŽ cant fraction of the water content
undergoes evaporation by the end of the freezing stage,
thus avoiding the energy consuming step required by the
removal of the latent heat of solidiŽ cation followed by the

187
188 GHIO et al.
provision of the heat of sublimation. A value of one seventh
of the total water is reported by Rey6, although even higher
values can result, depending on the nature of the material. It
has to be kept in mind, however, that processing costs are
only a part of total production costs in the food industry,
particularly for fruits and vegetables. This is because rinsing
and sometimes bleaching the raw material, cutting it into
pieces (slices, chips, dices, etc.), loading and discharging the
dryer, selecting the Ž nal product, packaging and storing are
required regardless of the process. The quality of the Ž nal
product is generally good when compared to hot-air dried
products, the main advantage being appearance,  avour
retention and rapid re-hydration. The fresh colour of the
product is maintained and the shape is only slightly chan-
ged. So, in many cases the special product advantages
outweigh the extra production costs incurred.
Very few data have been published on evaporative freez-
ing, and little information is available on this step and its
in uence on the whole process, especially with regard
to fruit and vegetables processing7. The aim of this work
is to evaluate the behaviour of different kinds of fruits and
vegetables, by correlating the duration of the freezing step
and the amount of water removed with the characteristics of
the raw material. Some fundamental aspects, such as the
drying rate during the evaporative freezing step and the
freezing rate, have also been investigated.
EXPERIMENTAL SET-UP
Apparatus
The experimental apparatus was derived from a commer-
cial Lyovac GT2 freeze-drier by Leybold, modiŽ ed to
improve its performances and with instrumentation to
permit on-line monitoring of weight loss and product
temperature during the process. The cylindrical drying
chamber contains a heating=cooling plate (not used in the
evaporative freezing experiments), and a round tray of
suitable size.
Two weighing devices were used: the Ž rst one was derived
from an analytical balance after separating the weighing cell
(placed inside the lyophilization chamber) from its electro-
nic components (located outside); the relative tests are
characterized by a mass range in the order of a few hundred
of grams of material. Due to the sensitivity needs and
response stability required by process kinetics determina-
tion, a prototype capacitive balance was then conceived,
constructed and tested to meet the drastic speciŽ cations
typical of freeze drying. The experiments carried out using
this instrument were more accurate, even though the mass of
the material dried was of one order of magnitude smaller.
Details and characteristics of this innovative instrumentation
are provided elsewhere8,9.
The lyophilization chamber was insulated and separated
by a butter y valve from the condensation chamber,
upstream of a vacuum pump. The maximum condensation
capacity was as high as 3 kg of ice in 24 h; the mini-
mum operating temperature of the condenser as low as
¡80 C; while the absolute pressure in the freeze-drier was
maintained at values lower than 6 Pa. A Pirani sensor was
installed to measure the pressure in the drying chamber. The
temperature of the plate was monitored by means of a
thermal resistance, while several bare joint micro-thermo-
couples could be inserted into the product. Further details of
the experimental set up are given elsewhere8,10.
Procedure
Experiments were carried out on different types of fruits
and vegetables: apricots, plums, prickly pears, bananas,
cherry tomatoes, mushrooms (cepes) and apples. The Ž rst
Ž ve types were simply divided into two pieces and not
peeled; small mushrooms were frozen in their original shape
(a quite typical market requirement), whereas apples were
cut into small sticks (10 10 70 mm) to study the freezing
rate and compare the process rate using evaporative freeze
drying and the conventional technique. Average water and
sugar contents of the different products, taken from the
literature, are given in Table 1.
Each evaporative-freezing run was carried out according
to the following procedure: Ž rst the material was prepared
and weighed, then placed onto the aluminium tray in the
drying chamber and tiny thermocouples were inserted into
the product, in different fruit pieces. After closing the
vacuum chamber, the condenser and the vacuum pump
were switched on to start the evaporative freezing process.
Several thermocouple outputs were recorded during each
run. The run was stopped at the end of the drying process
when steady weight output was observed.
Traditional freezing by conduction was carried out in a
few runs using the equipment cooling plate, in order to
investigate the in uence of the freezing step on process
length and product characteristics. Duplicate runs were
carried out to check reproducibility.
RESULTS AND DISCUSSION
Figure 1 shows the typical variation of the temperature of
the product during evaporative-freezing runs: in this case
apple chips (10 10 mm cross section) were processed. The
position of the two thermocouples inserted into the apple
stick is also shown. The sharp initial decrease of the product
temperature corresponds to the freezing due to water
evaporation. As shown in the Ž gure, the temperature
measured by two micro-thermocouples, placed at different
depths, appears to decrease during the freezing step with the
same rate in the outer material portion and in the core. Up to
now it has not been made clear whether the cooling in the
internal position occurs because of local evaporation or is
due to thermal conduction in the solid state. In any case the
heat transfer mechanism is very fast as cooling rates
exceeding several C=min were recorded. While the thermo-
couple in the internal position still shows some cooling, the
temperature in the upper position begins to increase because
of heat transfer from the outside and due to the fact that the
drying process begins to slow down. After the end of the
Table 1. Average water and sugar contents of fruit and vegetables.
Water, % Sugar, %
Apple (Pyrus malus) 85.6 11.0
Apricot (Prunus armeniaca) 86.3 6.8
Banana (Musa sapientium) 76.8 15.5
Plum (Prunus domestica) 87.5 10.5
Cepe (Boletus edulis) 92.0 –
Tomato (Lycopersicon esculentum) 94.2 2.8
Trans IChemE, Vol 78, Part C, December 2000
 A COMPARISON OF EVAPORATIVE AND CONVENTIONAL FREEZING 189

Figure 2. Comparison between traditional freeze-drying and the evapora-

tive-freezing process of apple sticks.

that in the conventional freezing, upon switching on the

Figure 1. Product temperature during an evaporative-freezing run with
apples. The position of the thermocouples in the sample is shown below the
graph.
cooling step, the upper thermocouple denotes a higher
temperature, either due to the fact that the primary drying
front has already retreated and passed the thermocouple
position by the end of the freezing step or because it is more
exposed to heat transfer from the outside. The data shown in
Table 2 conŽ rm that the apples lost about one third of their
weight in less than half an hour. Some products (such as
plums and tomatoes), characterized by a texture softer than
apples, tend to swell and expel their constitutive solutions
violently during the rapid freezing, as a sign of vaporization
within the bulk.
As expected (see Figure 2), the freezing rate is higher in
the evaporative freezing than in the standard freezing carried
out using cooling plates, since the heat is transferred during
the preliminary freezing step by convection, radiation and
conduction, transfer phenomena somehow limited by the
physical conditions of the process11; on the contrary,
evaporative freezing depends on the intrinsic latent heat
demand promoted by fast vacuum evaporation. Also, the
lowest temperatures achieved with the two techniques are
different as a consequence of the different heat transfer
mechanisms involved in the freezing step. It can be noted
vacuum pump (after 2.7 h), an additional rapid freezing step
is promoted by vacuum sublimation. Evaporative freezing
and conventional freezing temperature proŽ les vs. time are
compared. The Ž rst technique brought the product to
complete drying in less than 13 h, while the other process
required about 10 extra hours to get the product to the same
temperature as the surroundings, as a sign of completion of
the endothermic phenomenon. Moreover, conventional freez-
ing caused the product to reach a much lower temperature
(¡52 C compared to ¡20 C), even lower than the cooling
plate’s temperature (¡45 C), which is a sign of an extra
contribution provided by some evaporative cooling on the
outside of the chip when the vacuum pump was switched on.
The effect of pressure on the freezing step is shown in
Figure 3. Apricots were used in a process characterized by a
very slow pressure reduction in the Ž rst half hour: evapora-
tive freezing was induced to reach fruit solidiŽ cation; then
with a further rapid decompression, a subsequent evapora-
tive freezing allowed the product to reach a low temperature
until the product had the potential to lose weight rapidly. In
this case the temperature sensor, placed well inside the
product, actually represented the mean fruit temperature.
Similarly, the weight vs. time proŽ le depended on the
chamber pressure with two-step dynamics.
Figure 4 shows the temperature variation and weight loss
during the evaporative freezing for some products, charac-
terized by different texture, water and sugar content. It is
demonstrated that the water evaporation mechanisms
controlled the freezing rate: mushrooms, characterized by

Table 2. Process parameters for freeze-drying using evaporative freezing.

Freezing step
Total Total
Fruits process time weight loss Tmin Time Weight loss
and vegetables h % C h %
Apple 15 85 ¡21 0.5 33
Apricot 53 85 ¡16 1.17 23.8
Prickly pear 20.75 89 ¡25 0.92 33.2
Plum 31 72 ¡17 1.3 27.1
Cepes 8.55 91 ¡25 0.38 32.8
Tomato 32.67 94 ¡26 0.43 22.7
Figure 3. Effect of the pressure on the freezing step: apricot halves.

Trans IChemE, Vol 78, Part C, December 2000

190 GHIO et al.

gives it a valuable advantage over standard freeze-drying,

because it signiŽ cantly reduces the amount of heat to be
supplied.
Typical drying rates for three vegetables are given in
Figure 5. These proŽ les were obtained using a standard
weighing cell that supported the product tray which, despite
the low accuracy, was satisfactory for obtaining the process
kinetics. Very high initial values were observed, especially
for those products such as mushrooms and prickly pears in
which water evaporation occurs very easily, while signiŽ -
cantly lower values were observed, for example in plums, as
discussed above. All products showed a period in which the
drying rate decreases very slowly or was almost constant;
even though the process velocity still remained substantially
different according to their relative ease in water release, the
differences between different products are much smaller
than in the previous step. In standard air-drying the opposite
behaviour is generally observed: Ž rst a constant rate is
shown and then a decreasing rate takes place. In that case
the Ž rst step is due to free water diffusion in the product,
while here a massive water expulsion occurs by the differ-
ence of pressure inside and outside the product.
Figure 6 makes a comparison between freeze-drying with
evaporative-freezing and conventional freezing. The use of
the capacitive balance allowed better resolution and accu-
Figure 4. Comparison of the evaporative freezing of some fruits and
racy in the evaluation of the drying rate (see Figure 7). The
vegetables: product temperature (upper graph) and percentage weight loss evaporative freezing was characterized by an initial peak
(referred to the fresh product); note that a signiŽ cant fraction of water is (about half an hour long), then a slowly decaying rate
eliminated during the relatively short freezing step. extending up to about 8 h. With conventional freezing
there was no water removal until the vacuum pump was
started, then after a short transient the release of water
a Ž brous and tubular texture, lost water in an extremely
rapid fashion under vacuum and reached the lowest
measured temperature in approximately six minutes. Subse-
quently this low temperature was maintained for a while
thanks to their high water content (uniform ice retreating
from their capillary texture, with heat transfer as a control-
ling factor to drying). The data reported in Table 2 and in
Figure 4 conŽ rm the mechanism assumption.
Prickly pears also had a relatively fast freezing and initial
drying rate, as a consequence of their grainy texture; after
the Ž rst hour the drying rate reduced, because water diffu-
sion was affected by sugars migration on the outer fruit
portion.
The swelling and the eruption of constituent liquors for
tomatoes and plums built up a limiting action as far as the
Figure 5. Initial drying rate of prickly pears, plums and cepes (kg water=kg
drying kinetics are concerned: the cell expanded foam, as a fresh product h¡1).
further resistance to mass transfer, prevented the diffusion of
water vapour into the gas bulk. This phenomenon became
further limiting for plums due to their high sugar content
(see data in Table 1).
Bananas were not successfully freeze-dried; during the
evaporative freezing step the temperature stabilized at about
¡5 C and a weight loss of only about 30% was obtained
after 75 h. It can be argued that complete freezing did not
occur: this may be due to the very high sugar content of this
fruit, above 15% with about 2.4% amid, which hinders ice
formation.
In general, as shown in the lower graph in Figure 4,
during the freezing step and the initial stage of the evapora-
tive drying the fraction of moisture that may leave the
product can be estimated at between 0.2 and 0.4 of the Figure 6. Comparison of weight loss and residual water of apple sticks
total. This is a boost to the evaporative drying process which using conventional and evaporative freezing.

Trans IChemE, Vol 78, Part C, December 2000

 A COMPARISON OF EVAPORATIVE AND CONVENTIONAL FREEZING
Figure 7. Variation of the drying rate of apple sticks with evaporative and
conventional freezing versus time (upper graph) and weight loss (lower
graph).
continued at a fairly constant rate to about 15 h. The shape
of the two curves indicates a different number of consecu-
tive steps. In evaporative freezing at least three periods can
be identiŽ ed: a Ž rst period of rapid weight loss correspond-
ing to the initial freezing and vaporization of water, an
intermediate period and Ž nally a period of progressive
slowing down of water sublimation, as the process
approached its end. On the contrary, the conventional
process achieved over 80% of the weight loss at an almost
constant drying rate, followed by a Ž nal step in which the
water release was progressively slowing down. If the drying
rate as a function of the residual water is considered, in the
case of evaporative freezing the drying rate is higher until
about 60% of the water has been removed, then the drying
rate is slightly higher in the conventional process. Also, the
Ž nal moisture content for the conventional drying is lower,
even if the difference is very small. An explanation of the
more difŽ cult drying at the end of the process can be found
in the product aspect: the apple chips produced by the
evaporative drying were characterized by a stickiness, as a
clear indication of expulsion of constitutive liquids (mainly
water and sugar). In comparison, conventional freeze-
drying, via diffusive transport of water vapour only, left
the outer apple chip surface very dry.
CONCLUSIONS
The evaporative freezing of fruits and vegetables has been
investigated in detail: the use of this freezing technique in
Trans IChemE, Vol 78, Part C, December 2000
191
substitution for the traditional freezing step reduces the
duration of the freeze-drying process and consequently the
process costs. It was shown that the freezing step is very fast
and the amount of water that leaves the product during it
(from 20 to 40% of the total) reduces not only the drying
period but also the energy consumption.
The freezing rate affects, generally, the size of the ice
crystals and therefore the Ž nal porosity of the dried product.
In accordance with other  uid-particle phenomena, it can be
deduced that the larger the pores, the easier the water
removal from the porous product. Only a slow freezing
rate allows the growth of large ice crystals at the beginning
of the freeze-drying process; this fact should consequently
lead to larger pores and thus to shorter freeze-drying time. In
the case of evaporative freezing, the freezing rate is excep-
tionally rapid; but the Ž nal size of the pores in this case can
be in uenced by water vapour generation in the bulk of the
product. Evaporative freezing is a difŽ cult method to control
because the shape and the size of the ice crystals are affected
by the rate of cooling which, in turn, depends on the velocity
at which the pressure is reduced and is affected by product
structure. Both fruits and vegetables are deŽ ned capillary-
porous materials; the matrix has interstitial spaces, capil-
laries and gas-Ž lled cavities. Different transport mechanisms
can play a role during the freezing step, according to the
suggestions of many workers: liquid diffusion due to
concentration gradients, liquid transport due to capillary
forces, vapour diffusion due to vapour pressure gradients
and liquid transport due to the difference in total pressure
caused by the low external pressure, condensation effects
and surface diffusion.
Also, the drying rates differ because of product structure,
water and sugar content. Different water release mechanisms
were identiŽ ed by simultaneously monitoring the product
temperature and mass.
REFERENCES
1. Mumenthaler, M. and Leuenberger, H., 1988, Atmospheric spray
freeze-drying of pharmaceutical solutions, Proc Int Symp Control Rel
Bioact Mater, 15: 432–433.
2. Mumenthaler, M. and Leuenberger, H., 1991, Atmospheric spray
freeze-drying: a suitable alternative in freeze-drying technology, Int J
Pharm, 72: 97–110.
3. Mellor, J. D., 1978, Fundamentals of Freeze-Drying (Academic Press,
London).
4. Dalgleish, J. McN., 1990, Freeze-Drying for the Food Industries
(Elsevier Applied Science, London).
5. Elia, A. M. and Barresi, A. A., 1998, IntensiŽ cation of transfer  uxes
and control of product properties in freeze-drying, Chem Eng Process,
37(5): 347–358.
6. Rey, L., 1975, Freezing and freeze-drying, Proc R Soc (London), B 191:
9–19.
7. Mellor, J. D., 1964 Vacuum cooling of mushrooms, Mushroom
Growers’ Bulletin, no. 177, 396 (quoted from Reference 3).
8. Ghio, S., 1999, Freeze-drying. Experimental and Theoretical Analysis,
PhD Dissertation (Politecnico di Torino, Italy).
9. Rovero, G., Ghio, S. and Barresi, A. A., 2001, Development of a
prototype capacitive balance for freeze-drying studies, Chem Eng Sci,
in press.
10. Elia, A. M., 1996, Problematiche di Lio®lizzazione per Alimenti
e Farmaceutici: Cinetiche del Processo e Modellazione, PhD Disserta-
tion (Politecnico di Torino, Italy).
11. Bruttini, R., Rovero, G. and Baldi, G., 1991, Experimentation and
modelling of pharmaceutical lyophilization using a pilot plant, Chem
Eng J (Lausanne), 45: 67–77.
192 GHIO et al.

ACKNOWLEDGEMENTS Chimica, Politecnico di Torino, Corso Duca degli Abruzzi 24, 10129
Torino, Italy. E-mail: barresi@athena.polito.it
Financial support by the Italian National Research Council (CNR) is
gratefully acknowledged. The manuscript was received 11 August 2000 and accepted for publica-
tion after revision 21 December 2000.
ADDRESS
Correspondence concerning this paper should be addressed to
Dr A. Barresi, Dipartimento di Scienza dei Materiali ed Ingegneria

Trans IChemE, Vol 78, Part C, December 2000