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ABSTRACT
305
INTRODUCTION
with a model food gel with no membrane. This result showed that a semipermeable
cell membrane is not a necessary condition for osmotic processes.[17,18]
Differences in chemical potentials of water and solutes in a solid – solution system
result in fluxes of several components of the material and solution. The osmotic
pressure gradient is imposed by a concentrated external solution (sugar, salt, etc.).
Through control of the main variables of the process, mass transfer behavior will
cause either osmotic dehydration (dewatering) or impregnation soaking (swelling).
By using a highly concentrated osmotic solution (usually 50– 80 g solute per 100 g
solution), water flow (water mixed with low concentration of some natural solutes
from food material) out of the solid product into the osmotic solution occurs.
The transport of natural solutes in the food always accompany water transfer and
solutes also transfer from the osmotic solution into the food product. However,
water removal is much greater than osmotic solute uptake (Fig. 1).
In osmotic dehydration, the chemical potential gradient of water drives water
removal, which also promotes transport of the natural solutes of the food material
into the osmotic solution. The flow of water and solutes out of the solid foodstuff
mainly occurs in the first 2 – 3 hr of immersion. After this, the difference in water
content between solid product and osmotic solution tends to zero, until eventually
the system reaches a state of dynamic equilibrium of molecule transfer (Fig. 2).
During the later period of immersion, solute gain continues to increase steadily
because the gradient of solute concentration is still high (Fig. 2).
If the food material is immersed in a low concentration osmotic solution,
osmotic solution uptake by the food is greater than water removal from the food.
This process is called impregnation soaking (swelling or rehydration). During this
process, the gradient of moisture concentration drives osmotic solution into the
food product. The solute concentration gradient between solid food product and
osmotic solution causes the osmotic solute to transfer into the food material.
However, some pigments, flavors, and nutrients may transfer from the food into
Figure 1. Mass transfer pattern when a cellular material is immersed in osmotic solution.
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Figure 2. Water removal and osmotic solute gain in cellular material immersed in osmotic
solution.
of the final products. Soluble solids present in the osmotic solution are taken up
by the food material. Also, there may be gas flow out of the intercellular space.
There have been numerous studies to describe the kinetics of the two
counter-current flows in osmotic dehydration. Variables such as temperature, time
of treatment, and concentration and composition of solutes influence the mass
transfer kinetics. The kinetics of mass transfer is usually described through the
terms: water loss, solids or solutes gain, and weight reduction. Water loss and
solute gain may be measured through rate of water and solute flow, respectively,
over time or through the amount of water lost or solute gained after a certain
period of time per amount of initial material. Solids gain can also be studied
through solute penetration techniques, where the amount of solute uptake by the
material is determined with time.
A mixture of various transport mechanisms occur and the contributions of
the different mechanisms to the total transport varies from place to place and
changes as drying progresses.[19] Recently, rapid progress has been made on the
theoretical modeling of osmotic processes for food materials. Water transfer in
food materials immersed in osmotic solutions may be described by several
different transport mechanisms, depending on the nature of the material, the type
of moisture bonding, the moisture content, temperature, and the pressure in the
capillary pores.[20] In general, liquid diffusion occurs in nonporous solids, whereas
capillary movement occurs in porous solids. In liquid solutions and gels, transport
of water takes place only by molecular diffusion, a relatively simple phenomenon.
In porous biological materials, gas-filled cavities, capillaries, cell walls, and
intercellular and extracellular spaces all can influence the mass transfer properties.
Water can be transported by several mechanisms simultaneously: molecular
diffusion, liquid diffusion, vapor diffusion (through gas flow), hydrodynamic flow,
capillary transport, and surface diffusion. Most frequently, a combination of these
mechanisms occurs due to the complex structures found in foods.
Mass transfer kinetics depend on both process parameters and the structural
properties of the product. In biological materials such as fruit, vegetable, fish and
meat, the water content, cell maturity, tissue structure, porosity, as well as the
geometry of pieces immersed in the osmotic solution influence water removal,
product solute loss, and osmotic solute uptake. The transfer process of
water þ solute out of the food material and uptake of osmotic solutes into the
food material are usually based on the following mechanisms.
Figure 3. Schematic cellular material tissue representation and mass transfer pattern.[33]
the same layer can be considered in the same physical condition. As shown in
the section AI in Fig. 3, cellular structure is not changed. The water is being driven
out of the material from cell to cell only through the plasmodesmata by a turgor
pressure difference. In section A, water loss, osmotic solute uptake, and structure
change occur simultaneously. Osmotic solute is accumulated in the extracellular
space. Water is transferred from cells into the extracellular space through
membranes due to the concentration difference between extracellular space and
cellular solution. In section B, primarily water flow and osmotic solute flow
occurs. Section BI is considered as a reservoir of osmotic solution.
Figure 4. A schematic diagram of the changes of concentration of water and osmotic solute during
process.[33]
Most mass transfer models for osmotic dehydration process are based on the
assumption of independent diffusion of water and osmotic solutes in the solid
phase, and that the solid material is isotropic and does not shrink. Using these
assumptions, the mass transfer models apply the fundamental differential
equations for diffusion in solid material such as the first law of Fick.[34] Initially,
the moisture concentration in the food material is constant and no chemical
reaction occurs in the system; thus, the system may be treated as a one-
dimensional isothermal diffusion problem. In the isothermal transport process,
Fick’s law is the commonly used to theoretically predict the diffusion coefficients
of water and solutes in food materials, whether under continuous flow or
nonsteady state conditions. The process of osmotic dehydration can be
characterized by the rates of water loss and solute uptake of food material. For
a constant external condition (constant concentration) in osmotic solution and
negligible resistance at the solid– liquid contacting surface (sufficient agitation),
the internal resistance of the material to diffusion controls water and solute
transport. Fick’s first law provides the basic definition for mass transfer as shown
in Eq. (1).
›C
J¼D ð1Þ
›X
where J is mass flux induced by diffusion in the X direction, ›C/›X is the solute
concentration C gradient in that direction X.
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Bird et al.[35] gave a general form of Fick’s second law that can be used to
analyze unsteady-state diffusion in symmetric porous material.
›C 1 › n21 ›C
¼ n21 X D ð2Þ
›t X ›X ›X
where t is time; n ¼ 1 for an infinite slab, 2 for an infinite cylinder, and 3 for a
sphere; and X is the distance measured from the center of the solid material.
Crank[34] provided solutions to Eq. (2) for a wide variety of initial and
boundary conditions. Assuming that individual molecular transport is
unidirectional and independent, the unsteady-state diffusion in symmetric porous
materials can be analyzed using a general form of the second Fickian equation.
The diffusion equations assuming an infinite slab geometry describe the transport
of one of the solutes (natural solute loss and osmotic solute uptake) into a food
material Eq. (3), and water transfer out of the solid material Eq. (4).
X1 2
Cs 2 C se 2að1 þ aÞ 2qn Dt
¼ exp ð3Þ
C so 2 Cse n¼1 1 þ a þ a qn 2 2 L2
2
Cw 2 C we X
1
22ð1 þ aÞcos qnLX 2qn Dt
¼ exp ð4Þ
C wo 2 Cwe n¼1 ð1 þ a þ a qn Þcos qn
2 2 L2
X ¼ X0 C w ¼ Cwe ; Ci ¼ C ie for t . 0
Based on the assumption that mass transfer is the rate limiting step, and the
rate of mass transfer can be approximately predicted by appropriate mathematical
solutions of the simplified unsteady-state Fickian equation, mass transfer in
osmotic dehydration is controlled by internal resistance of the material.[36 – 38]
Fick’s law of diffusion in solids[34] was applied by Beristain et al.,[36] Favetto
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The main source of water inside biological material tissue is the cells. The
transfer of water from within the cell to the extracellular region involves migration
through the cells, its enveloping structure, through the porous tissue structure, and
then through the outside boundary layers. Philip[48 – 50] presented a quantitative
theory of water transport through plant tissue. Nonequilibrium thermodynamics
theory was used to develop a quantitative description of water transport through an
aggregation of plant cells containing both permeating and nonpermeating solutes
in aqueous solution. It is now generally accepted that there are three main potential
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pathways that water can follow while traversing plant tissue: (a) the apoplastic
transport pathway (cell wall pathway), which occurs outside the cell membranes
(plasmalemma) and can be defined as water diffusion through cell walls and
intercellular space between cells; (b) the symplastic transport pathway (symplasm
pathway), which is inside the plasmalemma and characterized by a fluid transport
from one cell directly into another cell through small channels (plasmodesmata);
and (c) the transmembrane transport pathway (vacuolar pathway), which is
defined as a water exchange route between the cell interior (cytoplasm and
vacuole) and the cell exterior (cell wall and intercellular space) across the cell
membrane.[51 – 54] There are also some sub-pathways possible for water to be
exchanged between the vacuole and cell wall.
Philip’s analysis assumed a tissue composed of cells with ideal semiperme-
able cell membranes and resulted in a linear diffusion equation with either water
potential, osmotic potential, turgor potential, or cell volume as the dependent
variable. The cell wall plays an important role in water transport. In the cell-to-cell
pathway, it is assumed that only the cell membranes have resistance to water
transport. The relevant conservation equations can be written by assuming that the
water fluxes in both the cells and cell walls are proportional to a potential gradient.
The potential for driving water along the cell-to-cell pathway can be given by
Eq. (5).
c ¼ PT þ Pos ð5Þ
where c is cell water chemical potential (bar), PT is cell turgor pressure (bar), and
Pos is cell osmotic pressure (bar).
Philip’s theory has been extended to describe water transport in cell walls
and plasmodesmata using the formalism of nonequilibrium thermodynamics to
allow for the simultaneous movement of water and diffusible solutes.[51 – 56] The
basic transport equations are expressed by Eqs. (6) and (7)[51] for the external
diffusion process.
2
›c ›c c2t
¼ D2 2 ð6Þ
›t ›X 2 Rf2
2
›t ›t c2t
¼ D1 þ ð7Þ
›t ›X 2 Rf1
where t is time (sec), t is wall water potential (bar), f1 is per cell water capacity of
cell wall pathway (cm3 bar21), f2 is per cell capacity of cell-to-cell pathway for
water (cm3 bar21), and R is per cell water flow resistance between pathways
(bar sec cm23).
The leakage of some natural solutes from food material into solution (such as
sugar, organic acids, mineral substances, and other chemical components) is
quantitatively negligible, but it may be essential as far as organoleptic or
nutritional qualities are concerned. From an osmotic point of view, the pathways
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of osmotic solution from the external into the intercellular space, or vice versa are
readily accomplished by diffusion during the passage of substance from the
outside of the plant cell to its interior or vice versa.[57]
where Ji is mass (water and solute) flux, Yj is the thermodynamic driving force, and
Lij are the phenomenological coefficients.
One of the first applications of irreversible thermodynamics to osmotic
dehydration was that of Toupin et al.,[58] who developed a model of the mass
transport phenomena in plant material based on an earlier model of Molz et al.[54]
Later, Biswal and Bozorgmehr[59] calculated mass transfer rate parameters from
osmotic dehydration of green beans in aqueous solution of sodium chloride
through thermodynamics of irreversible process. The model indicated that mass
fluxes and driving forces were nonlinearly related. The general theory of
irreversible thermodynamics is based on the assumption that the flux, Ji, is a linear
function of all the factors operative in the system assuming the system is defined as
a mass transfer operation in three components, i.e. (1) osmotic solute, (2) water,
and (3) total solid. Applying the idea of irreversible thermodynamics,
multicomponent mass transfer is a coupling phenomenon between mass transfer
of components, where the driving force is the chemical potential gradient. In
modeling diffusion mass transfer through thermodynamics of irreversible
processes, a linear flux and force relation is developed.
J 1 ¼ L11 Y 1 þ L12 Y 2 ð9Þ
where the diffusion coefficients Dij, are assumed constant. Equation (15) is valid
for radial coordinates, with r # cylinder radius, a, and 2L # X # L (L, half
height of cylinder).
Many experiments have revealed that the osmotic solute that penetrates
the material tissue is found mostly in a superficial layer or zone at the interface
of the osmotic fluid with the solid material, even after long periods of immersion in
the solution.[17 – 19,74 – 79] The bi-compartmental model proposed by Raoult-Wack
et al.[17] assumed average concentrations in both zones (solid phase and liquid
phase) (Fig. 4),[33] and described their variation in time combining two
exponential equations. Salvatori[77 – 79] extensively studied this zone. The zone
grows deeper with time, creating a variable set of conditions for mass transfer both
in space and time. This zone is characterized by the depth of penetration of the
solute from the interface. The penetration depth of the osmotic solute was found to
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be proportional to the square root of time. The effort to include the complex
characteristics of the cellular tissues in the modeling of osmotic dehydration has
led to the development of models from a cellular level approach.
Spiazzi and Mascheroni[80] developed a model for apple tissues using finite
volumes to represent the cells, and derived effective diffusivities from literature
data. A second method used averaged tissue properties, instead of dealing with
arrays of single cells. The fundamental feature of this method is to assume the
properties of the tissue at any given depth as equal to their average at that point.[81]
The averaging can even be extended to the overall active zone.[82] The principles
of diffusion are applied through the extended Fick’s law including bulk flow, for
the continuum in the extracellular space, combined with irreversible
thermodynamics for the membrane transport. The conceptual model, as proposed
by Yao and Le Maguer,[25 – 28] is schematically presented in Fig. 5.[82]
A generalized concentration profile for either water or osmotic solute is shown
along the path of a conceptual capillary.
The tissue consists of intracellular and extracellular volumes separated by a
semipermeable membrane. The individual cell membranes in the tissue are
combined into one single equivalent membrane.[81] The extracellular volume is
considered continuous, filled with water and in contact with the membranes. The
extracellular volume is partitioned into free volume (includes the volume of
capillaries and the volume between the fibers within the cell walls) and volume of
the cell wall fibers. The ratio of the free volume to the total volume of the tissue
gives the porosity. Properly averaged values for the cell dimensions and porosity
of the tissue allow the model to keep the proportions existing in the real tissue.
A value of tortuosity establishes the equivalence in length between the path
through the extracellular free volume, and the distance measured from the surface
of the slab. This graphic depiction of the tissue allows for an easier formulation of
the equations describing the phenomena involved in osmotic dehydration. Finite
element methods were used to solve these equations in space and time. It was
concluded that the osmotic flow of water is accountable for 90% of the water loss,
and that the solute would diffuse 60% less into the tissue compared to a pure
diffusion mechanism. The advance of the front of penetration is related to the
shrinkage of the tissue. By making a mass balance and a volume balance, the
following Eqs. (16) and (17) were developed for free volume along the X
direction.[25 – 28]
›ðCi AÞ › ›C i ›ðC i vAÞ
¼ ADi 2 þ J iE i ¼ 1; 2: ð16Þ
›t ›X ›X ›X
›ðvAÞ X k
›A
¼ ðJ i vi ÞE 2 i ¼ 1; 2: ð17Þ
›X i¼1
›t
The equilibrium is reached when mass flows stop.[86,87] From the irreversible
thermodynamics point of view, this happens for the cells when the difference in
chemical potential of water and solutes is zero. This is consistent with the
consideration of Lenart and Flink[6] that at equilibrium the water activity of the
osmotic solution and the potato tissue are equal. Biswal and Le Maguer[88] and
Biswal and Bozorgmehr[89 – 91] mentioned that the equilibrium is reached when the
aqueous phase activity of the product and the osmotic solution are equal. Other
authors refer only to the soluble substances concentration in the plant and osmotic
solution, considering them equal at equilibrium.[6,91 – 93]
Azuara et al.[41,42] used the concepts of water loss and solids gain in
equilibrium as asymptotes for the model in Eqs. (18) and (19). The water loss, WL,
per unit mass of initial tissue at equilibrium, WL1, was defined as the asymptote
for a hyperbolic expression to compute WL as function of a time constant, s1, and
time, t. The same concept is used for the solids gain, SG.
WL s1 t
¼ ð18Þ
WL1 1 þ s1 t
SG s2 t
¼ ð19Þ
SG1 1 þ s2 t
Long-time osmotic treatment (several days) revealed that the biological
cellular material product tends to gain weight, and the result is a product rich in
solutes.[17,18,94,95] Monsalve-González et al.[96] studied fruit cylinders and slabs,
and observed that the slabs lost less water than the cylinders, and the slab sugar
gain was also significantly less than the cylinders. In addition, a phase in which the
samples began to gain weight was observed. Barat et al.[97] explained these long-
term phenomena as relaxation responses of the tissue matrix. After the chemical
potential equilibrium with the cells is reached, the collapsed tissue matrix expands
slowly, recovering like a sponge while absorbing osmotic solution.
within the cell walls) between 2 and 10%. Some fruits, like apples, have up to 25%
free volume.[77 – 79] This space can be filled with water or solution during the
osmotic treatment, providing the pathway necessary for mass transfer inside the
tissue. Some water from the surface goes directly into the solution, but most of it
has to go through the network of capillaries and porous cell walls. This main
pathway for the movement of water in the tissue is called the apoplast. As time
progresses after cellular biological material is immersed in osmotic solution, the
solute penetrates further into these extracellular spaces of the tissue, creating the
zone where the cells are losing water through their membranes. This is considered
the active zone. Beyond that depth of penetration lays, the tissue remains
essentially unaltered.
Although readily observed under the microscope, the quantitative changes
that occur during osmotic dehydration are not easily measurable. Light
microscopy only works well on very thin sections of tissues. The actual physical
cutting of the material causes disruption of the tissues, thus limiting the area
available for observation and for measurement. Using scanning electron
microscopy (SEM) would require material to be frozen and embedded. These
processes also destroy the tissue. Therefore, a method that allows the observation
of thick sections of fresh or “minimally processed” tissue is necessary. Using red
beet tissue cells as materials, a three-dimensional true-color optical microscopy
system was developed.[65] This system allows the observation of the mass transfer
phenomenon in situ. This is a new technique to study cell volumetric changes in a
tissue matrix during osmotic dehydration in three-dimensions. The three-
dimensional imaging technique provides a means to visualize the cells in a tissue
in a more complete setting, although a time correction is required to take the “dead
time” for image preparation into consideration. Many modeling parameters are
estimated based on averaged data due to lack of proper data or based on
assumptions, due to lack of proper experimental techniques to measure them. With
experimental data obtained from imaging, the soundness of a diffusion model
could then be tested.
Another method for visualizing cell structures is confocal laser scanning
microscopy (CLSM) a form of light microscopy in which white or a narrow range
of wavelengths of laser light excites a specific fluorescent material.[100] The
microscope can image very clean, thin optical sections (or slices) from thick
fluorescent specimens.[101] CLSM also has the capability to obtain three-
dimensional images of biological and other microscopic structures.[102 – 104] The
microscope works very well with fresh tissues as well as with embedded samples.
To quantify changes in cell structure during osmotic dehydration, an
algorithm called the “spider” can explore the boundaries within the edge of the
selected cell (Fig. 7).[99] This procedure can be conducted on each selected and
labeled cell through a stack of images. The spider can also detect the missing
boundaries or gaps in the cell’s edge based on surrounding points in all dimensions
(X, Y, and Z ). The spider then interpolates all the points it has detected in the cell
and uses this to reconstruct a three-dimensional view of the cells (Fig. 8).[99]
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The reconstruction may be viewed as sample points or as a wire frame, and may be
moved and rotated in different axes and dimensions. These methods are able to
improve the kind of images acquired on osmotically-dehydrated plant materials.
Such imaging techniques provide a new dimension to studying the phenomenon of
osmotic dehydration at a cellular level in both qualitative and quantitative aspects.
FUTURE DEVELOPMENT
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