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J. Snchez, Y. Ruiz, J.M. Auleda, E. Hernndez and M. Ravents
Review. Freeze Concentration in the Fruit Juices Industry

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Review. Freeze Concentration in the Fruit Juices Industry
J. Sa nchez,
1
Y. Ruiz,
2
J.M. Auleda,
1
E. Herna ndez
1
and M. Ravento s
1,
*
1
Agri-Food Engineering and Biotechnology Department, Technical University of Catalonia (UPC)
Avda, Canal Olmpic, 15, 08860 Castelldefels, Barcelona, Spain
2
Chemical Engineering Department, Faculty of Engineering, National University of Colombia
Ciudad Universitaria Cra, 30 No 45 26, Bogota, Colombia
In conventional processes, such as evaporation, higher levels of concentration can be reached compared
with freeze concentration or membrane techniques. However, the advantage of the freeze concentration
technique is based on the quality of the product obtained due to the low temperatures used in the
process, which makes it a very suitable technology for the processing of fruit juices. There are two basic
methods for concentrating solutions by freezing: suspension and film freeze concentration. Suspension
freeze concentration systems (FCS) already have operating equipment in the food industry, while film
FCSs, also called layer crystallization, is still at an experimental stage. This review summarizes the most
important studies relating to the suspension and film freeze concentration in fruit juices and sugar
solutions, illustrating the different possibilities that freeze concentration has in the fruit juices industry;
it also presents trends and suggests improvements for the future development of this technology. It is noted
that most recent publications refer to the film FCS. The technology used to design, build and maintain
layer crystallization equipment is simple and it can be available to any operator in the food industry, layer
systems will be used in the future if their results can be improved in terms of ice purity and degree of fluid
concentration.
Key Words: freeze concentration, suspension system, layer concentrators, fruit juices, sugar solutions
INTRODUCTION
The growing demand for fruit juices of high sensory
and nutritional quality has led to the search for new or
improved food processing technologies. Among the
techniques for concentration of liquid foodstuffs,
freeze concentration is of particular interest due to the
low temperatures used in the process.
Freeze concentration is a technology that can be used
in the food processing industry to concentrate fruit
juices (Rahman et al., 2006). This process allows
removal of water from a solution by cooling or freezing
it until high-purity ice crystals are formed and separated
to leave a concentrated fluid. The nutritional and sen-
sory quality of freeze-concentrated fruit juices is higher
than those concentrated conventionally by means of
evaporation due to the low processing temperatures,
which avoid undesirable chemical and biochemical
changes, and minimize the loss of sensory properties.
Some authors have summarized the studies referring to
the concentration of fruit juices as cryoconcentration,
however the subject is treated in general, making com-
parisons with other methods for the concentration of
juice (Ramteke et al., 1993) and with emphasis on the
description and operation of equipment involved in the
process (Deshpande et al., 1984).
The objectives of this paper are to summarize the
most important studies relating to the suspension and
film freeze concentration in fruit juices and sugar solu-
tions, present trends and suggest improvements for the
future development of this technology.
FREEZE CONCENTRATION
METHODS
According to various researchers (Mu ller and
Sekoulov, 1992; Flesland, 1995; Chen et al., 1998;
Miyawaki, 2001; Wakisaka et al., 2001), there are two
basic methods for ice crystal formation in solutions. The
first is known as suspension crystallization (Huige and
Thijssen, 1972; Hartel and Espinel, 1993), consisting of
an initial phase of ice nuclei formation (nucleation), also
called crystallization, followed by a second phase which
involves the growth of ice nuclei in the solution
(Figure 1(a)). The second method is the crystallization
*To whom correspondence should be sent
(e-mail: merce.raventos@upc.edu).
Received 23 March 2009; revised 3 June 2009.
Food Sci Tech Int 2009;15(4):0303315
SAGE Publications 2009
Los Angeles, London, New Delhi and Singapore
ISSN: 1082-0132
DOI: 10.1177/1082013209344267
303
of water present in the solution in formof an ice layer on a
cold surface (Mu ller and Sekoulov, 1992; Flesland, 1995;
Figure 1(b)).
In the industry, suspension freeze concentration con-
sists of three stages: crystallization, growth and separa-
tion of ice crystals, performed with specially designed
equipment for each purpose. The system comprises the
following equipment (Lemmer et al., 2001; Jansen
et al., 2001; Verschuur et al., 2002; van Nistelrooij,
2005): a scraped-surface heat exchanger (SSHE;
Figure 2) and a recrystallizer. The SSHE forms ice
nuclei at high supercooling and low residence times,
where ice nuclei are formed on the inner surface of the
heat exchanger and then are scraped off by rotating
blades. The ice nuclei go to the recrystallizer (Figure 2)
for ice crystal growth based on the Gibbs Thomson
effect and then a separation of ice crystals from the con-
centrate occurs normally in a pressurized wash column
(Figure 2). In this system, ice crystals of high purity can
be attained (Thijssen, 1986).
The second system, film freeze concentration,
consists of formation of a single crystal, which grows
layer by layer from the solution to be concentrated.
The crystal growth (dendrites) tends to be parallel
and opposite to the direction of heat transfer
(Flesland, 1995) The crystal adheres to the cold surface
during the process, facilitating separation of the two
phases (Figure 3).
This concentration system is based on directional
freezing, and the most important crystal form is the
dendrite (Flesland, 1995; Chen et al., 1998; Chen
and Chen, 2000; Pardo et al., 2002; Gu et al., 2005;
Caretta et al., 2006). Heat transfer rates are normally
greater than mass transfer rates, due to the high ther-
mal conductivity of ice and low mass diffusion coeffi-
cients. Therefore solute diffusion will be the limiting
factor for ice growth, and supercooling (constitutional
supercooling) in the tip region will be observed (Rutter
and Chalmers, 1953; Ozu m and Kirwan, 1976; Teraoka
et al., 2002; Hindmarsh et al., 2005; Ayel et al., 2006).
Ice crystal
Ice nuclei
Concentrate
Concentrate
Ice layer
Cold surface
(a) (b)
Figure 1. Two methods for concentration by freezing.
Feeding tank
Nucleation (crystallization)
scraped-surface heat exchanger (SSHE)
Concentrate
Growth
recrystallizer
Heater
Water
Separation
wash column
Figure 2. Schematic suspension freeze concentration system (courtesy of Niro Process Technology).
304 J. SA

NCHEZ ET AL.
Solute inclusion in ice is difficult to avoid in practical
applications, especially for solute concentrations of
commercial interest for freeze concentration, which
means between 20% and 50% of dissolved solids
(Flesland, 1995). The two methods described for the for-
mation of ice in solutions differ in terms of heat extrac-
tion, ice growth rate, ice purity, equipment, industrial
process, solidliquid contact surface, and necessary
investment (Table 1).
SUSPENSION FREEZE
CONCENTRATION
Research in suspension freeze concentration has
focused on two issues: control of nucleation and
growth of ice crystals to obtain large ice crystals, pref-
erably of uniform size, and to separate ice crystals selec-
tively from the concentrate. According to Thijssen
(1986) and Hartel and Espinel (1993) this system
requires separate stages for nucleation and growth of
ice crystals since the optimal operating condition
requirements for these distinct crystallization phenom-
ena can be significantly different.
The studies using juices have a wide range of aims,
including examination of the basis of the process
(Omran and King, 1974; Stocking and King, 1976;
Thijssen, 1986; Chiampo and Conti, 2002) and determi-
nation of the sensory quality of the juices obtained (Van
Weelden, 1994; Lee and Lee, 1998). Those studies show
that the final concentrations attained by this method
vary between 45

Bx and 55

Bx.
Crystallization
The study of suspension freeze concentration has
shown that in fruit juices and sucrose solutions the
most important category of nucleation is secondary
rather than primary nucleation (Omran and King,
1974). For that reason, some researchers have studied
that aspect in greater depth to understand the mechan-
isms that give rise to secondary nucleation and many
models have been generated to represent its kinetics.
That is the case with the studies performed by
Stocking and King (1976), who found that the velocity
of nucleation and rate of growth depend on the super-
cooling of the system and established that a model based
on a power law can be used to represent the relationship
between those variables for sucrose solutions, orange
juice and apple juice. They also found that crystal
growth at high supercooling occurs dendritically or
with a needle shape, which gives rise to a larger surface
area and greater difficulty of separation from the con-
centrated solution. In highly concentrated sucrose solu-
tions the nucleation rate is independent of the
concentration of the solution and as the concentration
of a sucrose solution increase the rate of crystal growth
declines due to greater viscosity. In studies using sugars
such as dextrose or fruit juices, Thijssen (1975) found
that the rate of nucleation increases with the concentra-
tion of dissolved solids and is proportional to the square
of the supercooling of the sine of the solution, and also
that the presence of localized supercooling in the crystal-
lizer due to nonuniform mixture gives rise to an increase
in the rate of nucleation, so that the presence of such
Refrigerant
Expansion valve
Distribution juice duct
Ice layer
Liquid food falling film
Evaporator
Refrigerant
By-pass
Pump
Tank
Figure 3. Schematic film freeze concentration
system (Raventos et al., 2007).
Table 1. Indicative data of film and suspension
crystallization systems.
Film
crystallization
Suspension
crystallization
Heat extraction Through ice layer Through solution
Ice growth rate 10
6
10
7
(m/s)
a
10
7
10
8
(m/s)
b
Ice purity Low High
Equipment No moving parts
except pumping
equipment
Moving parts
in all the
equipment
are needed
Industrial process Discontinuous Continuous
Solidliquid
contact surface
Low High
Percentage of needed
investment
c
100 150250
a
Olowofoyeku et al. (1980); Flesland (1995); Chen et al. (1999); Miyawaki
et al. (1998).
b
Huige and Thijssen (1972); Hartel and Espinel (1993); Chiampo and Conti
(2002).
c
Flesland (1995).
Review. Freeze Concentration in the Fruit Juices Industry 305
points should be avoided in the interest of controlling
the average size of the crystals formed.
Huige and Thijssen (1972) developed the basic
knowledge of the suspension freeze concentration
process (Table 2) involving supersaturation in a crystal-
lizer with continuous seeding of small crystals that dis-
solved and promoted the growth of larger crystals
already present in the crystallizer (Ostwald ripening
mechanism).
Another method of increasing the size of ice crystals
has been presented by Shirai et al. (1987) and
Kobayashi et al. (1996). The authors have used agglom-
eration to increase the ice crystal size in order to
improve the solidliquid separation. Kobayashi et al.
(1996) concluded from storage experiments (Table 2)
that agglomeration of ice crystals mainly depends on
the seed crystals, the initial crystal size distribution
and the concentration of solute. Extensive agglomera-
tion of ice crystals was observed in glucose solutions
with concentrations of 10% and lower, but not in solu-
tions with concentrations of 20 and 30%.
More recently, Pronk et al. (2002) confirms that the
Ostwald ripening mechanism in ice suspensions is the
most important for crystal size. Agglomeration is
observed in some cases but this mechanism plays a
minor role. A computer-based dynamic model of
Ostwald ripening in ice suspensions has been conducted
to simulate the development of ice crystal size distribu-
tions during adiabatic ice slurry storage (Pronk et al.,
2005). Validation with experimental results for different
types and concentration of solutes (sucrose solutions),
different ice fractions and different mixing rates showed
that the model is able to predict the development of the
average crystal size in time.
Bayindirli et al. (1993) carried out studies for formu-
lation of a mathematical model to describe the freeze
concentration of apple juice (Table 3), concluding that
the kinetic of the cryoconcentration process fits to a
sigmoidal curve. A similar behavior of the concentration
kinetics can be found in the work of Nonthanum and
Tansakul (2008) during the process of cryoconcentration
with lime juice. Chiampo and Conti (2002) presented the
results obtained in a freeze concentration pilot plant of
Niro Process Technology (Table 3), using strawberry
juice and other kinds of sugar solutions (sucrose solu-
tions at different initial concentrations). It was found
that for an optimal functioning of the equipment, the
maximum amount of ice in the re-crystallizer must not
exceed 40% and secondly that the average speed of ice
growth is lower in the strawberry juice than in the sugar
solutions. The ice productivity of the equipment is lower
with strawberry juice than with the sugar solutions, with
a maximum of 150 kg /h/m
3
.
Separation of Ice Crystals
The separation of ice crystals from concentrated fruit
juices can be performed using presses, centrifuges, and
wash columns, operating either in batch or in continu-
ous mode. Both presses and centrifuges present pro-
blems with carry-over of the product, whereas wash
columns have been developed to the point where the
solute inclusions have been reduced to less than
100 ppm. Several types of wash columns have been
Table 2. Some studies including suspension freeze concentration of sugars.
Fluid, author and
year of publication Aim of study Equipment Results
Sucrose solutions
(Huige and
Thijssen, 1972)
To describe (by means of a
mathematical model) a new
bulk crystallization process
studied experimentally for the
growth of ice crystals from
aqueous sucrose solutions.
Crystallizer (SSHE) The model predicts an increase of the mean
size of the product crystals with a decrease
of feed crystal size for small feed crystals.
The size of the product crystals also
increases with an increase in crystal con-
centration in the crystalliser.
Glucose solution
(Kobayashi
et al., 1996)
To develop an easier method
to produce large ice crystals
agglomerated in a common
batch crystallizer with an
inner heat exchanger.
Experimental apparatus
based on that proposed
by Shirai et al. (1987)
To make large agglomerated ice crystals: Keep
the initial supercooling, i.e., the temperature
difference between the lowest temperature
initially attained and the freezing point of the
solution less than 0.2 K and introduce seed
ice crystals greater than 6% of the solution
weight to trigger the ice crystallization.
Sugar solutions
(Qin et al., 2006)
To measure the heat transfer
coefficient and the power
consumption of a laboratory
SSHE used for freezing
a sugar solution.
SSHE Heat transfer coefficient with phase change (ice
formation) is about three to five times greater
than that without phase change.
Power consumption increased synchro-
nously with the ice fraction in the process
fluid mainly due to the fluidity reduction
(or the apparent viscosity increase) of ice
slurry.
306 J. SA

NCHEZ ET AL.
developed and put into industrial application and they
differ in the various crystal bed transport mechanisms
(Verdoes et al., 1997), where the crystal can be trans-
ported by either gravity, mechanically (piston/screw), or
hydraulic pressure. The last two are known as wash
columns with forced transport. For more than two dec-
ades the gravity-type units were the only commercially
available ones, since problems with scale-up and the
effect of back mixing on product purities have limited
their commercial application. Forced transport wash
columns are smaller and operate with short residence
times; crystals obtained are relatively pure and strong
enough so that a wash column with forced transport
will be preferred over a gravity wash column. (Scholz
et al., 2002).
The most commonly used wash column for freeze
concentration systems (FCS) in the fruit juices industry
is the piston-type wash column in countercurrent wash-
ing (van Nistelrooij, 2005; Morison and Hartel, 2006).
Quality
Studies performed in the 1980s and early 1990s focused
on assessment of the quality of the products obtained,
such as in the studies with pineapple and orange
juice carried out by Braddock and Marcy (1985; 1987).
Table 3. Studies that include suspension freeze concentration of fruit juices.
Fluid, author and
year of publication Aim of study Equipment Results
Apple juice, orange juice,
sucrose solution, glucose
solution, fructose solution
(Omran and King, 1974)
To study secondary nucleation
kinetics with fruit juices and
sugar solutions.
Crystallizer with
cooling bath and
glass stirrer.
The nucleation order is independent of sugar
concentration, type of sugar, and stirring rate.
The nucleation rate order is a strong function of
the sugar concentration.
Apple juice, orange juice,
sucrose solution, glucose
solution, fructose solution
(Stocking and King, 1976)
To study ice nucleation rates in
fruit juices, sugar solutions,
and distilled water.
Crystallizer cell with
cooling bath and
glass stirrer.
Nucleation rate in sugar solutions and fruit juices
increases with approximately the second
power of subcooling.
Pineapple juice (Braddock
and Marcy, 1985)
To examine pilot scale
processing parameters and
product quality aspects of
freeze concentration applied
to fresh pineapple juice.
Suspension pilot
equipment (Model
W-8, Grenco
Process
Technology).
Flavor of reconstituted freeze concentrated juice
was comparable to single strength juice and
preferable to evaporator concentrated juice.
Orange juice
(Braddock and
Marcy, 1987)
To determine the effects of
heat inactivation of enzymes
and pulp content on quality of
freeze concentrated orange
juice.
Suspension pilot
equipment (Model
W-8, Grenco
Process
Technology B.V).
Except for considerable pulp reduction of feed
stream juices, there were few differences
from normal citrus juice recovery procedures
for freeze concentration (the product retained
most of the aroma constituents of fresh juice).
Orange juice
(Thijssen, 1986)
Grenco freeze concentration is
compared with evaporation
and hyperfiltration.
Grenco Process
Technology B.V.
cryoconcentrator.
Freeze concentration appears an attractive
method: Conservation of nutritional and
organoleptic characteristics of fresh product,
the net added value must be based on the
packaged product (production costs makes a
relatively small contribution of the processing
costs to the total costs of the packaged
product).
Apple juice
(Bayindirli et al., 1993)
To study apple juice cryocon-
centration in a single-stage
process and a multi-stage
process.
Hemispherical por-
celain containers.
At the end of the single-stage experiments only
a double concentration could be achieved.
With multi-stage experiments higher concen-
tration levels could be achieved.
Sugar cane juice, sucrose
solution (Patil, 1993)
To examine freezing points, visc-
osities, and changes with
concentration of raw and clear
cane juices.
Crystallizer cell with a
cooling jacket.
The freezing points of raw juices are lower than
those of sucrose solutions.
The maximum juice concentration was limited to
about 54

Bx.
The decrease in crystal size with increasing
concentration and the high viscosities
observed would make it impractical to use
freezing to increase the Brix value beyond
about 50

Bx.
Strawberry juice and
sugar solutions
(Chiampo and
Conti, 2002)
To present the results obtained in
freeze concentration of fruit
juices at a pilot plant.
Pilot plan implemen-
ted for Niro
Process
Technology B.V.
Speed of ice growth in strawberry juice is
lower than the speed obtained for sucrose-
water solutions.
Maximum specific yield, dependent on the con-
centrated product (150 kg/h/m
3
)
Review. Freeze Concentration in the Fruit Juices Industry 307
They compared the aroma and flavor of fresh juice
with those of freeze concentrated juice and vacuum
evaporation concentrated juice (Table 3), finding that
the freeze concentrated juice preserved its sensory quali-
ties better in comparison with the juice concentrated by
evaporation.
During the 1990s and the early years of the new cen-
tury, there were references using fruit juices, some aimed
at studying the sensory qualities of juices obtained
through suspension freeze concentration (Van
Weelden, 1994; Lee and Lee, 1998). Lee and Lee
(1998) examined changes in quality during the refriger-
ated storage of clarified pear juice at 10

Bx obtained by
vacuum evaporation, reverse osmosis and cryoconcen-
tration. The results indicated that after 10 days of stor-
age there are no significant differences in browning and
turbidity. Juices obtained by reverse osmosis and cryo-
concentration show a similar sensory quality and it is
superior to that obtained by evaporation.
RECENT DEVELOPMENTS AND
POTENTIALS TRENDS
More recent studies have aimed at improving the
stages in commercial equipment of suspension
freeze concentration (Niro Process Technology,
The Netherlands; Figure 2).
Very little information is available regarding the ice
crystallization process in scraped surface ice generators
(SSHE) and most theories of ice crystallization mechan-
isms largely depend on anecdotal evidence and are
somewhat speculative (Hartel, 1992; Stamatiou et al.,
2005). Schwartzberg (1990) proposed that dendrites
grow out from the wall into the bulk solution due to
the large temperature gradient present at the wall sur-
face by some heterogeneous mechanism and are subse-
quently scraped off by the rotating blades. It is possible
that ice crystal fragments that remain on the wall after
the scraper blade passes are the source of new crystals
that form along the wall between scrapes (Drewett and
Hartel, 2007). Ice fragments that break off provide sec-
ondary nuclei and can result in formation of new crys-
tals through a contact mechanism.
In a recent work, Qin et al. (2009) studied and mod-
eled ice nucleation from aqueous solutions on a sub-
cooled solid surface. The most important applications
in suspension FCSs of the modelling studies are that
the induction time of ice fouling is correlated with the
degree of supercooling in the cooling wall, and this can
be used to estimate the critical time interval between two
scraping actions in the SSHE in order to optimize the
process and save energy.
Botsaris and Qian (1999) replaced the SSHE by one
with ultrasonic radiation for ice nucleation. The use of
ultrasound permits nucleation at low levels of
supercooling (0.40.5

C) and consequently an inexpen-
sive plain heat exchanger can be used for minimizing ice
scaling in the heat exchanger, higher coolant tempera-
tures lead to savings of capital and operation costs of
refrigeration. Moreover, better quality crystals are
obtained due to the use of lower supercooling, and for
this reason the use of ultrasound in scraped surface
exchangers should be considered, as suggested in the
work of Zheng and Sun (2006). Also worth noting is
the work of Verschuur et al. (2002) who replaced the
SSHE with a vacuum crystallization system which oper-
ated below the triple point pressure of an aqueous mix-
ture (<6 mbar). Vacuum crystallization would require
semi-continuous (cyclic) operation, and offer only a lim-
ited cost reduction potential, moreover the process is not
suitable for food liquids, since aromas and other volatile
flavors may be lost in the process. Slurry crystallization
(Verschuur et al., 2002; van Nistelrooij, 2005) is per-
ceived as a well-established crystallization process, and
provides significant cost reductions in crystallizers and
recrystallizers. The average achievable crystal size in a
slurry crystallizer is smaller than in a conventional pro-
cess, for certain applications these smaller crystals can
still be perfectly treated in a wash column. Additionally
the specific energy consumption is less, which results in a
much lower overall production cost for the final user.
More recent noteworthy studies are those of Habib
and Farid (2006) on the crystallization process in a flui-
dized-bed heat exchanger (FBHE), which is a less costly
alternative in comparison with the SSHE. Those studies
involved the design and construction of a vertical flui-
dized-bed heat exchanger to test the viability of the pro-
cess, which uses particles of stainless steel to remove ice
from the cooling surface. Experiments of Nazir and
Farid (2008) show that it is possible to carry out freeze
concentration of apple juice in a fluidized-bed heat
exchanger. Operation remains stable as long as the ero-
sion rate caused by the fluidized particles is equal or
greater than the ice growth rate.
The application of high-pressure freezing during the
nucleation stage might also give worthwhile results. This
is effective for very fine control of the ice structure size
(Miyawaki, 2001). Freezing by change of pressure pre-
sents a number of advantages over conventional sys-
tems. The main advantage is that a large amount of
the water in the product is frozen instantaneously and
uniformly throughout the volume at the same time
(immediately after expansion) unlike what happens in
the traditional systems where nucleation only takes
place at the surface of the sample in contact with the
cooler (Cheftel et al., 2000; Otero and Sanz, 2000, Otero
and Sanz, 2006; Norton et al., 2009). An important col-
lateral effect of the treatment is the microbial and/or
enzymatic inactivation that can be produced in the pro-
cessed food due to the effect of the high pressure pro-
moted by the low temperature.
308 J. SA

NCHEZ ET AL.
FILM FREEZE CONCENTRATION
A wide variety of liquid foods have been studied in
film freeze concentration. In the case of juices, the max-
imum concentrations attained are around 30

Bx and
with sugar solutions 54

Bx. There are no references in
the papers examined in the use of this sort of equipment
in the food industry. There are two film freeze concen-
tration techniques that have been studied in the papers
examined: Layer freeze concentration and progressive
freeze concentration. The difference between these two
techniques lies in the equipment used for the formation
of ice layers.
Progressive freeze concentration involves the crystal-
lization at the bottom or sides of a vessel or in a pipe.
In film FCSs the crystallization occurs on a plate.
Layer Freeze Concentration
In layer freeze concentration, the solution to be con-
centrated is in contact with a cold surface which consists
of a cooled vertical plate on which the fluid descends; ice
forms a single layer on the cold surface and the solution
is concentrated continuously throughout the whole pro-
cedure. Mu ller and Sekoulov (1992) suggested that the
layer freezing process is easier to manage, but when the
crystal grows on a cooled surface this induces a rapid
rate of crystallization and under these conditions impure
ice crystals can be produced. In spite of this moderate ice
purity, the disadvantages are compensated by the sim-
plicity of the operation, because there are no moving
parts in the equipment and no slurry handling.
Flesland (1995) has been studying the layer crystalli-
zation in laminar falling film (50 <Re <600) for freeze
concentration applications, using sucrose solutions
(Table 4). Ice growth rates and impurities in the ice or
loss of solute are measured for varying conditions.
Experimental results show that one-step layer crystalli-
zation has a lower separation effect than suspension
crystallizers with wash columns. The solute inclusions
could be reduced by increasing turbulent conditions,
by adding more steps and re-circulating melt water
with high sucrose concentration.
Chen et al. (1998) and Chen and Chen (2000) studied
(experimentally) the solute inclusion in an ice layer on a
smooth stainless steel surface under subcooled flow con-
ditions in sucrose (Table 4) and fructose solutions as
well as in orange juice. The average ice growth rate,
the solution velocity, the bulk solute/solid concentration
and type of solute have been shown to be the four key
factors in determining average distribution coefficient
(solute distribution between the ice and the liquid
phase). It was concluded that the ice obtained is more
pure at low concentrations of soluble solids, low growth
rates of ice and high speeds of the solution on the plate.
In solutions with a single component, heavier solutes
(higher molecular weight) are less likely to be trapped
in the ice and thus, produce a more pure ice. No data are
provided in the behavior of solutes in solutions with
various components, such as fruit juices.
An application at pilot scale of that type of process
was presented by Ravento s et al. (2007) and Herna ndez
et al. (2009), to study the process of concentration of
aqueous solutions of sugars (glucose, fructose, and
sucrose) and apple as well as pear juice in a layer
freeze concentrator. In general, a higher degree of con-
centration was attained in the sucrose solutions in a
shorter time, in comparison with the results for the glu-
cose and fructose solutions. The best results, in terms of
purity of the ice, were found at low initial concentrations
of the sucrose, glucose and fructose solutions. The kinet-
ics of the cryoconcentration process fitted to a linear
function in all cases.
Previous works have focused on ice growth rate,
solution velocity, concentration and type of solute,
being the dominant factors in the efficiency of removing
impurities in ice. However, it was found that the crystal
orientation is another very important factor to eliminate
impurities in ice (Kramer et al., 1971; Okawa et al.,
2009). In the study of Okawa et al. (2009) the mecha-
nism of the difference in trap between kinds of crystal
orientations was discussed with the existence of a con-
stitutional supercooling.
Progressive Freeze Concentration
Progressive freeze concentration has been carried out
using vertical equipment and tubular equipment.
Vertical Progressive Freeze Concentration
A vertical progressive FCS consists of a cylindrical
receptacle, a cooling bath, a system for immersing the
receptacle in the bath, an agitator for the solution in the
ice-solution interface and an external heating blanket to
control the level of ice formed in the receptacle and reg-
ulate the growth of the crystal (Figure 4).
The variables of the process studied while using this
type of equipment are: the type of solution, rate of
immersion or rate of ice growth, rate of agitation and
mechanisms to reduce supercooling. In progressive
freeze concentration, the distribution coefficient of
solute between the ice and the liquid phase is most
important. This is strongly dependent on the advance
rate of the ice front and the mass transfer at the ice-
liquid interface determined by stirring rate (Liu et al.,
1997) (Table 4). The effect of these operating conditions
on the partition constant in the progressive freeze con-
centration was theoretically analyzed by using a concen-
tration polarization model (Burton et al., 1953).
Progressive freeze concentration has been applied
to solutions of glucose, tomato juice, raspberry
(Rubus glaucus) pulp and aqueous solutions of sucrose.
Review. Freeze Concentration in the Fruit Juices Industry 309
Table 4. Studies that include film freeze concentration and other techniques with sugars solutions.
Fluid, author and
year of publication Aim of study Equipment Results
Mixture of water and
sucrose
(Flesland, 1995)
To study layer crystallization in a
falling film of aqueous solutions.
Cooled plate and glass
vessel.
Ice removed in each experiment is less than 0.2 (kg)
It is difficult to separate pure ice in a step process for
concentrations from 20% to 40%.
Glucose solutions,
glucose, and
blue dextran
solutions (Liu
et al., 1997)
To investigate the effect of the
moving speed of the freezing
front, the stirring speed at the ice
solution interface and kind of
solute in freeze concentration
ratio.
Progressive freeze
concentrator
(cylindrical sample
vessel of stainless
steel).
A lower moving speed and a higher stirring speed
produced a better freeze concentration ratio.
The kind of solute affects the concentration ratio.
Glucose solutions
(Liu et al., 1998)
To avoid solution accumulation in
the solid phase.
Progressive freeze
concentrator
(bottom plate with a
large number of
holes).
The plate with holes turned out to be an effective
mechanism to avoid subcooling.
Use of the plate allowed a 54% purer solid phase to
be obtained.
Sucrose solutions
(Chen et al.,
1998)
To study solute inclusion levels in
ice layers formed on a smooth
stainless steel plate under
subcooled flow conditions.
Test section with two
fluid channels sepa-
rated by a 1(mm)
thick stainless steel
plate.
Distribution of solid inclusion of ice layer for 20wt%
sucrose solution: solute inclusion values along the
horizontal directions are approximately the same
(width 14 cm)
Aqueous solutions
of: L-phenyl and
sucrose
(Matsuda et al.,
1999)
Freeze concentration of three
aqueous solutions with/without
supersonic radiation under a
constant freezing rate
(40mm/h).
Stainless steel freezing
column.
Stainless steel bottom
plate.
Freezing without supersonic radiation could greatly
concentrate solutes and decreased the average
distribution factor under 0.4.
The solutes of large molecular weight are more easily
separated and concentrated than those of small
molecular weight.
Sucrose solution
(Chen et al.,
1999)
To investigate effect of potato
starch particles on sucrose
inclusion in ice and effect of
solute (sucrose) on starch
particle inclusion in ice.
Experimental appara-
tus (two fluid
channels).
Sucrose in ice layer formed from sucrose solution is
not affected by the addition of potato starch and
potato starch in ice layer formed from suspension
is influenced by sucrose concentration quite
significantly.
Glucose solutions
(Wakisaka
et al., 2001)
To examine ice productivity and the
effect of operating on ice
crystallization.
Ice maker unit for
freezing wastewater.
Ice production: 578.6 kg/m
2
h
99% of glucose was rejected during ice growth with
ice seeding.
A higher purity of the ice layer was found at a flow
velocity of 1 m/s, with initial solution concentration
from 2600 to 5800 V of glucose.
Sucrose solutions
and three-com-
ponent solution
(Kawasaki et al.,
2006)
To examine the performance of
freeze concentration at constant
freezing rate (40mm/ h) with or
without ultrasonic irradiation.
Referring to Miyawakis
apparatus.
The solutes of smaller molecular weight were sepa-
rated and concentrated more effectively than
solutes of larger molecular weight.
The concentration efficiency increased with increasing
intensity of ultrasonic irradiation.
Glucose, fructose,
and sucrose
solutions
(Raventos et al.,
2007)
To examine the concentration of
aqueous solutions of glucose,
fructose and sucrose using a
multi-plate cryoconcentrator.
Pilot plant: (multi-plate
cryoconcentrator).
Maximum concentration was attained with sucrose,
taking the shortest process time (32.2

Bx in
16.6h).
The concentration limits attained with glucose and
fructose were similar and it increases linearly over
the process time.
As the solution becomes more concentrated, the
amount of water removed in the form of ice grad-
ually increases.
Sugar solution
(Qin et al., 2006)
To measure the heat transfer coef-
ficient and power consumption
of a laboratory scraped-surface
heat exchanger.
Cylindrical vessel. Heat transfer coefficient was found having a step-
function jump at the onset time of phase change.
Glucosewater and
sucrosewater
(Chudotvortsev
and Yatsenko,
2007)
To determine the concentration
and temperature of eutectic
points in aqueous systems with
glucose and sucrose.
Cylindrical plastic
vessel in a freezer.
An anomalous behavior near the eutectic point was
observed in the sucrose water system: solutions
with concentrations of 5562% behave identically
both in fractional melting of ice and in cooling of a
solution until the onset of crystallization.
The component distribution in the sucrosewater
system at other concentrations is similar to that for
the rest of the systems studied.
310 J. SA

NCHEZ ET AL.
The results of the studies show that the performance of
freeze concentration is strongly influenced by the type of
compound present in the solution. Liu et al. (1999) and
Halde (1979) found that small solutes are retained in the
ice more easily than the larger ones. Moreover Kawasaki
et al. (2006) noted that the solutes of small molecular
weight were separated and concentrated more effectively
than solutes of larger molecular weight, and this corre-
sponded well to the magnitude of the diffusion coeffi-
cient of each solute.
On the subject of rate of growth of the ice, Liu et al.
(1997) found that a slower rate, on the order of 0.5 cm/h
gave lower values for the distribution coefficient
between the ice and liquid phase K (00.1) in solutions
of sucrose. Likewise, Ramos et al. (2005), using similar
equipment to that described by Liu et al. (1997)
obtained lower purity in the solid phase with an increase
in the rate of growth of ice.
Vigorous agitation of the ice-solution interface pre-
vents the retention of solutes in the ice due to the elim-
ination of the concentration and temperature gradient
on the interface. Halde (1979) found that a faster rate of
agitation in the interface resulted in a greater purity of
the ice formed with aqueous solutions of glucose. This is
similar to the results obtained by Liu et al. (1997) with
solutions of glucose, where a faster rate of agitation in
the interface (1400 rpm) gave lower values for the
distribution coefficient K (00.1) and by Liu et al.
(1999) with tomato juice, which showed that a faster
rate of agitation gave lower concentrations of solids in
the ice phase, with the corresponding increase of con-
centration in the solution. Matsuda et al. (1999) inves-
tigated the effects of supersonic radiation on the
efficiency (distribution coefficient) of separation and
concentration of glucose solutions under various freez-
ing rates. They found that for equal mass concentration,
efficiency was greatly improved using supersonic radia-
tion because of the effect of turbulence in the liquid
phase by supersonic cavitation. The most recent research
by Kawasaki et al. (2006) concluded that concentration
efficiency improved with increasing intensity of super-
sonic irradiation (Table 4).
With the aim of reducing the likelihood of dendritic
growth from the outset of the formation of the solid
phase, Liu et al. (1998) proposed a plate with small
holes at the bottom of the receptacle for a faster nuclea-
tion of the solution trapped in the holes (Table 4). The
result obtained was that in the freeze concentration of a
5% solution of glucose, use of the plate with holes made
it possible to obtain ice with a glucose retention of 57%
lower than in the ice obtained without use of the plate.
Regarding the effect of progressive freeze concentra-
tion on the characteristics of the fruit juices, Liu et al.
(1999) showed that freeze concentrated and reconsti-
tuted tomato juice showed no material difference in
acidity, vitamin C content or color in comparison with
non concentrated tomato juice. An examination of the
effect of progressive freeze concentration on the reten-
tion of compounds in the flavor of raspberry (Rubus
glaucus) pulp revealed a 20% loss of volatiles during
the freeze concentration process (Ramos et al., 2005;
Table 5). The sensory analysis, performed by a panel
of trained tasters, found that untreated pulp, enzyme-
clarified pulp and freeze concentrated and reconstituted
pulp did not show any material difference in appear-
ance, color, taste, aroma, or overall quality.
Tubular Progressive Freeze Concentration
To increase the productivity of progressive freeze con-
centration, a tube ice system was proposed by Shirai
et al. (1999). In this method, ice crystal grows on the
inside surface of a pipe cooled by a coolant. In this
work, an ice tube was produced in a bubble-flow circu-
lator and the effect of seed ice crystals on tube ice for-
mation with a high purity was investigated. Without
seed ice crystals, substantial supercooling occurs and
dendritic ice crystals are formed, the solutes are trapped
between dendritic ice crystals, thus resulting in poor
quality. Use of seed ice crystals is effective because it
generates other ice crystals, resulting in no supercooling.
The productivity was easily increased simply by increas-
ing the surface area of the cooling plate. Numbers of
Stirrer
Stainless tube
Unfrozen
fraction
Power supply
Frozen
fraction
Cooling bath
Hot wire
Motor
Figure 4. Apparatus for progressive freeze concen-
tration (Miyawaki et al., 1998).
Review. Freeze Concentration in the Fruit Juices Industry 311
pipes can be bundled together and interconnected to
increase the cooling surface area.
Atubular ice systemwith a large cooling surface area is
an effective method for freeze concentration of tomato
juice and sucrose solutions; increased productivity and
high yield (Miyawaki et al., 2005; Table 5) showed that.
The system comprises two connected sleeved tubes, the
solution circulates inside the tube while the coolant cir-
culates outside (Figure 5). The solid phase is generated on
the inner walls of the tubes and the concentrated solution
is re-circulated, it flows through the annulus that has not
yet frozen. In this systemthe slower growth rate of ice and
the higher circulation rate gave a lower effective partition
constant (distribution coefficient).
Table 5. Studies that include film freeze concentration and other techniques with juices.
Fluid, author and year
of publication Aim of study Equipment Results
Apple juice (Nazir and
Farid, 2008)
To estimate the erosion rate at
different operating conditions
with an empirical model based
on an analogy between ero-
sion and heat-transfer
phenomenon.
4 and 5 mm equilateral
cylindrical particles
made of stainless steel
(SS304) fluidized in the
inside pipe of a vertical
double pipe heat
exchanger.
It is possible to carry out freeze
concentration of fruit juices in fluidized-
bed heat exchanger.
The erosion model predicts stable
operating limits for the fluidized bed
at different bed porosities, particle
sizes, and concentrations of
apple juice.
Andes berry pulp
(Rubus glaucus
Benth) (Ramos et
al., 2005)
To apply progressive freeze con-
centration to Andes berry
(Rubus glaucus Benth) pulp to
study its effects on free vola-
tiles composition and
concentration.
Progressive freeze con-
centrator (Halde, 1979;
Liu et al., 1998).
The color of Andes berry (Rubus glaucus
Benth) pulp is preserved during the
concentration process.
This treatment does not change the flavor
compounds and even intensifies aroma.
Tomato juice, sucrose
solution, coffee
extract (Miyawaki et
al., 2005)
To apply a tubular ice system to
concentrate liquid food. To
explore the concentration limit
by this method.
Tubular ice system (two
straight pipes).
Tubular ice system gave extremely high
concentrations with good yields.
Sugarcane juice (Rane
and Jabade, 2005)
To propose a heat pump-based
freeze concentration system
(FCS) to concentrate sugar-
cane juice from 20 to 40

Bx.
Heat pump-based FCS
(uses layer freezing
process).
Use of heat pump facilitates rejection of a
major part of the condenser heat at
about 10

C while melting the ice.
Bagasse saving of 1338 kg per day or for
1000 kg jaggery can be achieved.
Tomato juice (Liu et al.,
1999)
To apply progressive freeze con-
centration to tomato juice and
evaluate its effect on juice
quality.
Progressive freeze
concentrator.
No substantial differences in acidity, vitamin
C content, and color quality after recon-
stitution of freeze-concentrated tomato
juice compared with unconcentrated
juice.
Kiwifruit juice (Maltini
and Mastrocola,
1999)
To propose the use of freeze
concentration to produce a
concentrated juice to be
stored in the frozen state ready
for use by simple addition of
water.
Separation solidliquid
(ice-concentrated solu-
tion) by means of
centrifugation.
The quality of the re-constituted juice is
ideal.
Slight fading of the green color of the frozen
juice is observed after storage for 90
days.
Actinidia (kiwi) juice
(Maltini et al., 1998)
To propose the use of freeze
concentration to produce a
concentrated juice to be
stored in the frozen state ready
for use by simple addition of
water.
Separation solidliquid
(ice-concentrated solu-
tion) by means of
centrifugation.
The concentrated juice shows a
slightly non-Newtonian (pseudo plastic)
behavior.
It is not necessary to surpass a content of
30% solids in the cryoconcentration
phase to prepare juice of sugary kiwi.
The quality of the reconstituted juice is ideal
after 4 months storage at 18

C.
Carrot juice
(Mahmutoglu
and Esin, 1996)
A phase distribution coefficient
for the concentration of liquid
foods at the solidliquid inter-
face is defined and estimated
for freezing of carrot juice.
Cylindrical container (insu-
lated with polystyrene
foam).
At four freezing temperatures:
range 6.5

C to 14.2

C, the distri-
bution coefficient was found to be prac-
tically independent of the freezing
temperature and is about 0.38.
Apple juice
(Olowofoyeku
et al., 1980)
Freeze concentration of apple
juice using a new rotational
freeze concentrator.
Rotational freeze
concentrator.
The higher initial feed stream concentration
resulted in higher occluded solids in the
ice melt.
The difference in temperature effects at
10

C and 20

C was not significant.

312 J. SA

NCHEZ ET AL.
ASPECTS TO CONSIDER IN THE
FUTURE DEVELOPMENT OF
FREEZE CONCENTRATION
The future development of freeze concentration will
be centered on overcoming its drawbacks, for that
reason, it might involve the following points:
(a) Suspension crystallization attains levels of ice
purity that are clearly superior to those attained
with film crystallization. For this reason, the
future of film crystallization technology will
depend on the reduction of levels of occlusion in
the solid phase.
(b) The degree of concentration obtained with film crys-
tallization is still lower than that obtained with the
suspension system; an increase in final concentration
will need to be attained.
(c) Reduction of the level of ice impurity and an
increase in the degree of concentration of the fluid
with the film crystallization system requires progress
in the following aspects:
Transport of the fluid to be concentrated in a hydra-
ulic regime with the greatest possible turbulence
(on a plate, Re >2500 is recommended, and inside
circular conduits Miyawaki et al. (2005) recom-
mends working with velocities of over 1 m/s).
Application of the characteristic techniques of melt
crystallization: Controlled seeding, nucleation
mechanically induced by shock waves, ultrasonic
vibration, supersonic radiation or partial melting
(sweating) to drain impurities trapped in the ice.
(d) One advantage of the film crystallization system is
its simplicity, in terms of both the construction and
operation of its equipment, nevertheless, in order to
optimize operation, a continuous operation system
will have to be devised.
(e) The design of equipment with the minimum number
of moving parts in the suspension crystallization
system would simplify its operation and it would
make it more competitive.
FINAL REMARKS
Although industrial equipment exists for suspension
freeze concentration, a layer system will be used in the
future if its results can be improved in terms of ice purity
and degree of fluid concentration.
Film crystallization technology may be an emerging
technology with the potential to overcome the obstacles
of its industrial feasibility due to the simplicity of this
system in terms of the construction and operation of its
equipment.
ACKNOWLEDGMENTS
The author J. Sa nchez thanks the Ministry of Popular
Power for Science and Technology for the fellowship
granted through FONACIT (National Fund for
Science and Technology) from Bolivarian Republic of
Venezuela. The author Y. Ruiz thanks Instituto para
el Avance de la Ciencia y Tecnolog a
COLCIENCIAS for its condonable loan for doctoral
studies, national 2004.
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