Vacuum impregnation for development of new dehydrated products

Pedro Fito
*
, Amparo Chiralt, Jose M. Barat, Ana Andres, Javier Martnez-Monz o,
Nuria Martnez-Navarrete
Abstract
Vacuum impregnation (VI) of structured foods implies the partial release of gas from pores and its substitution by an external
liquid. Therefore, important changes in physicochemical and structural properties take place in the food and these aect its behavior
in drying operations (air-drying (AD) and/or osmotic dehydration (OD)). The adequate control of VI prior to dehydration may be
used as a tool both to improve mass transfer and to develop engineered products. In order to evaluate this alternative, the eec-
tiveness of VI as a tool in porous matrix formulation is analyzed. Likewise, its inuence on some physical and transport properties
of the plant tissue and the relevant changes induced in osmotic and convective drying processes are discussed, since these are
probably the most interesting alternative processes to lengthen the impregnated product shelf-life. Improved yield of some dehy-
dration processes, such as fruit candyin, when VI is applied at the beginning, is also discussed in terms of the cell network relaxation
mechanism, responsible for hydrodynamic tissue impregnation.
Keywords: Dehydrated fruits; Vacuum impregnation; Osmotic processes; Food matrix engineering
1. Introduction
Vacuum impregnation (VI) of a porous product
consists of exchanging the internal gas or liquid oc-
cluded in open pores for an external liquid phase, due to
the action of hydrodynamic mechanisms (HDM) pro-
moted by pressure changes (Fito, 1994; Fito & Pastor,
1994). The operation is carried out in two steps after the
product immersion in the tank containing the liquid
phase. In the rst step, vacuum pressure (p
1
~ 50100
mbar) is imposed on the system for a short time (t
1
) in
the closed tank, thus promoting the expansion and
outow of the product internal gas. The releasing of the
gas takes the product pore native liquid with it. In the
second step the atmospheric pressure (p
2
) is restored in
the tank for a time (t
2
) and compression leads to a great
volume reduction of the remaining gas in the pores and
so to the subsequent in ow of the external liquid in the
porous structure. Compression can also reduce the pore
size depending on the mechanical resistance of the solid
matrix.
The volume fraction of the initial sample (X) im-
pregnated by the external liquid when mechanical
equilibrium was achieved in the sample has been mod-
eled (Eq. (1)) as a function of the compression ratio r
(Eq. (2)), sample eective porosity (e
e
), and sample
volume deformations at the end of the process (c) and
the vacuum step (c
1
), as described in Eq. (2) (Fito,
Andres, Chiralt, & Pardo, 1996). If c = c
1
= 0, Eq. (1)
gives the relationship for VI of non-deformed products
(Fito, 1994). In practical terms, sample deformations in
VI are seen to be negligible for a great number of fruits
(Salvatori, Andres, Chiralt, & Fito, 1998; Chiralt et al.,
1999).
r =
p
2
p
c
p
1
; (1)
e
e
(r 1) = (X c)r c
1
: (2)
The aim of this paper is to discuss how VI may modify
composition of porous food, and therefore its eective-
ness as a tool in porous matrix formulation, its inuence
on some physical and transport properties of the plant
tissue and the relevant changes induced in osmotic and
convective drying processes, which are probably the
most interesting alternative processes to lengthen the
impregnated product shelf-life. Improved yield of some
dehydration processes, such as fruit candy, when VI is
applied at the beginning is also discussed. Special em-
phasis is placed on the behavior of apple samples be-
cause of their high porosity and so their suitability for
VI processes.
2. VI process for the formulation of porous matrices
VI operation can allow us to incorporate any ingre-
dients in a porous product in order to adapt its com-
position to certain stability or quality requirements, in a
quick and simple way. Structured foods such as fruit
and vegetables have a great amount of pores (intercel-
lular spaces) which are occupied by gas, or native liquid
to quite an extent, and which oer the possibility of
being impregnated by a determined solution thereby
improving composition by adding specic/selected sol-
utes: incorporation of acids, preservatives, sugars or
other water activity depressors, special nutrients, etc. In
this sense, VI can be considered as a tool in the devel-
opment of fruit or vegetable products without disrupt-
ing their cellular structure, while conveniently modifying
their original composition (Chiralt et al., 1999). VI also
modies some physical properties of the product and
this will have advantages for other processes (Martnez-
Monz o, Martnez-Navarrete, Fito, & Chiralt, 1998a,
Martnez-Monz o, Barat, Gonzalez-Martnez, Chiralt, &
Fito, 2000).
These aspects may be considered as food matrix
(porous solid) engineering since the original product is
adapted to new requirements. The mass fraction of any
component (i: water or solutes) reached in the impreg-
nated product (x
I
i
) can be estimated by Eq. (3) deduced
from a mass balance in the system, in terms of the
sample initial composition (x
0
i
), the mass ratio of the
impregnating solution in the initial product (x
HDM
) and
the solution composition (y
i
). The value of x
HDM
is easily
deduced from the sample porosity level by applying Eqs.
(1), (2) and (4), if sample deformation is assumed neg-
ligible throughout VI process. From these Equations,
the required solution concentration of a determined
component (water, sugar, acid, additive, etc.) can be
calculated in order to achieve a desired level in the nal
product. In Fig. 1, the predicted values of mass fraction
of any ingredients i reached in a porous sample in a VI
operation was plotted as a function of their mass frac-
tion in the external solution and the sample porosity.
The following assumptions were made to obtain pre-
dicted values: pressure at vacuum and atmospheric
conditions were 50 and 1030 mbar, respectively, the
initial i level in sample was zero and no changes in initial
sample porosity occurred during VI. The limiting factors
for VI are the solubility of component i in the external
liquid and the sample eective porosity.
x
I
i
=
x
0
i
x
HDM
y
i
1 x
HDM
: (3)
x
HDM
= X
q
IS
q
0
: (4)
3. VI eects on physical properties of fruit
The physical property which is most clearly aected
by VI is the product density. Since air in the pores is
replaced by liquid, density increases, thus aecting other
related properties such as thermal conductivity which is
Notation
p
c
capillary pressure
p
1
vacuum pressure in the rst VI process step
p
2
atmospheric pressure in the second VI process step
e
e
sample eective porosity
r compression ratio in the VI process
X sample volume fraction impregnated by the solution at the
end of the VI process
c
1
relative volume deformation of the sample due to pressure
change at the end of the rst VI step
c relative volume deformation of the sample due to pressure
change at the end of the VI process
q
0
density of the initial product
q
IS
density of the impregnating solution
q
0
r
initial real sample density
x
HDM
mass ratio of the impregnated solution in the initial product
y
i
mass fraction of the component i in the impregnating
solution
x
I
i
mass fraction of component i in the impregnated product
x
0
i
mass fraction of component i in the initial product
K thermal conductivity
a thermal diusivity
e
/
; e
//
real and imaginary components of the complex dielectric
permitivity
Fig. 1. Mass fraction of impregnated component i in a porous product
as a function of its mass fraction in the external solution and the
product porosity. Values predicted applying Eqs. (1)(4), assuming:
c = c
1
= 0, x
0
i
= 0, r = p
2
=p
1
, p
1
= 50 mbar, p
2
= 1030 mbar,
q
0
r
(kg=m
3
) = 1056, q
0
(kg=m
3
) = q
0
r
(1 e
e
), q
IS
(kg=m
3
) = 1=
[((1 y
i
)=1000) (y
i
=1500)[.
greatly aected, especially when highly porous. Changes
are dependent on total porosity and pore distribution in
relation with the direction of heat ow and impregnat-
ing solution composition (Martnez-Monz o et al., 2000;
Barat, Martnez-Monz o, Alvarruiz, Chiralt, & Fito,
1994). Fig. 2 shows the values of thermal conductivity
and diusivity of apple (var. Granny Smith ) with and
without VI (p
1
= 50 mbar) with an isotonic solution as a
function of temperature. Determination method of these
properties has been previously described (Martnez-
Monz o et al., 2000). Lesser modications were observed
in thermal diusivity than in conductivity because of the
simultaneous sample density increase during VI (at
25C: q
0
(NI) = 813 kg=m
3
; q
0
(I) = 986 kg=m
3
). Spe-
cic heat (c
p
) does not change if no changes in com-
position are induced in VI, nevertheless the product c
p
q
0
may increase throughout the process. In apple samples
c
p
q
0
varies from 3:12 10
6
to 3:79 10
6
J=m
3
K, in the
range 3060C, due to VI with an isotonic solution. An
increase in the impregnating solution concentration will
promote the expected reduction in all thermal properties
as compared with impregnation without compositional
changes (Fito, Chiralt, Barat, & Martnez-Monz o,
2000).
In microwave drying (MWD) dielectric properties of
a material greatly aect heat generation and drying rate.
Both real (e
/
) and imaginary (e
//
) components of the
complex permitivity decrease when product porosity
increases (Kent & Kress-Rogers, 1987). Gasliquid ex-
change in the product pores promoted by VI could im-
prove microwave-product interactions and so be
advantageous in MWD or combined ADMWD.
Dielectric properties of apple (initial e
e
= 0:23) I and
NI with an isotonic solution have been reported for
samples dried at dierent moisture levels (Martn, Fito,
Martnez-Navarrete, & Chiralt, 1999). The reported
values of e
/
and e
//
reected the inuence of changes in
water content and structure on the capability of the
sample to store and dissipate energy, respectively. Both
components evolve as a function of the moisture content
in a dierent way for NI and I samples. Loss tangent
(e
//
=e
/
) increases in line with sample drying level, this
being faster for impregnated samples. Inuence of im-
pregnation of apple on the complex permittivity mod-
ulus (

e
/2
e
//2
_
) does not seem noticeable, this decreases
when moisture content decreases.
4. Mass transport properties in osmotic and convective
dehydration
Mass transport properties, such as the eective dif-
fusion coecient of the plant tissue in osmotic dehy-
dration (OD) processes are also modied by previous VI
pretreatment. This modication has been analyzed in
apple tissue VI with isotonic solutions in order to avoid
any change in the value of the process driven force
(Martnez-Monz o, Martnez-Navarrete, Chiralt, & Fito,
1998b). The values of the eective diusion coecient
(D
e
) in the product liquid phase (PLP), sugar gain (DM
s
)
and water loss (DM
w
) for NI and I cylindrical samples
(1 cm characteristic dimensions) treated for 3 h, at 30C,
with concentrated grape must (a
w
= 0:789) are given in
Table 1. Impregnation was carried out with low mo-
lecular weight and high molecular weight solutes (HM
pectin) in order to observe the eect of the viscosity of
the liquid in the intercellular spaces. It can be seen that
VI promotes eective diusion in the fruit liquid phase
when impregnated solution has low viscosity, even
considering the corrected D
e
value of NI sample with its
porosity value. Obtained results are in agreement with
the coupling of diusional and osmotic (water selective
diusion through cell membrane) mechanisms to a dif-
ferent extent in each case. Sugar gain occurs through
diusion in the pores, but this mechanism contributes
little to water loss which mainly occurs cell to cell by
osmotic mechanisms. When intercellular spaces are oc-
cupied by gas (NI sample) or by a very viscous solution,
solute diusion through intercellular spaces seems to be
inhibited and the sample reaches the chemical equilib-
rium with the osmotic solution after a greater osmotic
water loss. This aspect also implies greater PLP and
volume losses of the samples.
In practical OD processes of porous fruits, VI pre-
treatments were carried out with the osmotic solution at
the beginning of the process. This is called pulsed vac-
uum OD (PVOD) and has been observed to be very
eective in promoting mass transfer kinetics (Fito &
Chiralt, 1995, 1997; Shi & Fito, 1993; Shi, Fito, &
Chiralt, 1995). VI implies transporting the external sol-
ute and water into the tissue while it modies the ef-
fective diusion coecient in the PLP. The gas liquid
exchange implies a fast change of the sample overall
Fig. 2. Thermal conductivity (circles) and diusivity (rhombus) values
of apple samples impregnated (closed symbols) and non-impregnated
(open symbols) with an isotonic solution (adapted from Martnez-
Monz o et al., 2000).
composition that modies the process driven force at the
very beginning of the process, while pores remain full of
liquid. Fig. 3 shows the comparison of D
e
values in the
PLP, obtained for dierent fruits in mass transfer kinetic
analysis of parallel processes at atmospheric pressure
OD and PVOD. Compositional change promoted by
vacuum pulse was corrected in the analysis to make the
D
e
values comparable, according to a model previously
published (Fito & Chiralt, 1997). Higher values of D
e
in
PVOD processes can be observed in almost all the cases,
the higher the fruit porosity, the greater the D
e
promo-
tion by PVOD.
In addition to promoting diusional mechanism in
the pores, which was commented on the above, VI
brings with it a dierent structural development of the
tissue throughout the osmotic process, thus aecting the
tissue response to mass transport. Dierences in the
structural features observed in vacuum-impregnated and
non-impregnated (NI) samples have been explained in
terms of the dierent pressure drop of uid in the in-
tercellular spaces owing towards the volume generated
by cell water loss, which is very dierent for gas or liquid
phases in the intercellular space (Fito et al., 2000). When
there is a liquid in the pores, the force balance on the
double layer plasmalemma-cell wall leads to layer sep-
aration while plasmalemma shrinks in line with water
loss with scarce deformation of cell wall. In OD pro-
cesses, where a gas phase occupies the intercellular
space, plasmalemma shrinks together with cell wall that
deforms greatly when osmotic the process progresses
(Barat, Chiralt, Albors, & Fito, 1999). Fig. 4 schemati-
cally shows the structure development of the cellular
tissue in OD and PVOD treatments at dierent steps of
the process (Fito et al., 2000).
Air-drying processes (AD) of fruit and vegetables
involve heat and mass transport phenomena in the plant
tissue. Transport rate is greatly aected by the tissue
structure and composition, both dening the eective
values of its transport properties (thermal properties and
water eective diusion coecient). Therefore, VI pre-
treatments may lead to a dierent drying behavior of
fruit and vegetable, as well as to dierent nal properties
of the product. Fig. 5 shows the eect of VI with an
isotonic solution on drying curves of apple slices (7 mm
initial thick). In this case, VI slows down the drying rate
of the product. The increase of the variable c
p
q
0
of the
product as well as the limitation of vapor diusion in the
sample pores are the main factors that made the process
rate slower in I samples. However, when combined AD
MWD is applied, drying rate of I samples overtakes that
of NI samples, starting from the application of a de-
termined MW power, probably due to the induced
changes in dielectric properties (Martn et al., 1998).
5. Impregnation in long-term osmotic processes. Fruit
candying
Impregnation of the fruit pores due to HDMs has
been seen to occur without external pressure changes
when the cellular tissue remains immersed in a liquid
phase for a long time (e.g., syrup canned and candied
fruits). This was explained in terms of the capillary
forces, pressure and temperature uctuations in the
system and relaxation phenomena of the shrunk cellular
matrix when hypertonic solutions were used in the
treatments (Fito et al., 2000; Barat, Chiralt, & Fito,
1998, 1999). It has been observed that HDM contributes
Table 1
Eective diusion coecient, sugar gain and water loss of apple (Granny Smith) osmosed with rectied grape must (a
w
= 0:789) for 3 h at 30C
(adapted from Martnez-Monz o et al., 1998b)
Sample D
e
10
10
(m
2
=s) DM
s
a
DM
w
a
NI 3.96 (5.13)
b
9.0 )40.1
I
c
6.51 16.2 )34.7
I
d
3.07 7.3 )34.7
a
Expressed as g of water or solute gain per 100 g of initial product, for 3 h of treatment.
b
In brackets corrected value taking into account porosity value of apple (D
e
=(1 e
e
)).
c
VI with an isotonic solution containing sugar and 2% (w/w) HM pectin.
d
VI with sugar isotonic solution.
Fig. 3. Comparison of D
e
values obtained in parallel osmotic dehy-
dration processes of dierent fruit at atmospheric pressure (OD) and
pulsed vacuum OD (PVOD). Temperature range: 3050C. Osmotic
solution: sugar solution between 50 and 70 Brix.
to the total mass transfer throughout long-term osmotic
processes due to the internal pressure gradients in the
tissue associated to relaxation of deformed cell network
resulting from cell water losses (Fito, Chiralt, Barat,
Salvatori, & Andres, 1998; Barat et al., 1998). Table 2
summarizes the dierent steps involved in a long-term
osmotic process on the way to equilibrium as well as the
phenomena responsible for the changes in the system
free energy, which occur in each step. Fig. 4 also shows,
in a schematic way, the development of a cellular tissue
throughout the equilibrium pathway in this kind of
process for samples initially vacuum impregnated (I)
with the osmotic solution and for those non-impreg-
nated (NI).
After the chemical equilibrium was reached in the
system, the cell network will have stored a great deal of
mechanical energy in the deformed cell walls and cell
bondings. The amount of stored energy will be depen-
dent on the stiness of the cellular arrangement in the
tissue. Weak cell bonds and soft/thin cell walls will imply
a great dissipation of energy during water loss and de-
formation. On the contrary, strong cell bonds and hard/
thick cell walls will lead to a notable store of free energy
as mechanical tension in the structure. Relaxation of
mechanical energy leads to sample volume recovery and,
if the sample is immersed in a liquid, the subsequent
mass gain due to hydrodynamic ow of the external
liquid.
In apple samples, it has been observed that the vol-
ume was recovered until practically the initial value in a
wide range of process conditions (treatments between
30C and 50C with osmotic solutions from 15 to
65Brix). Volume and mass recovery in PVOD-treated
samples was faster than in those OD treated and the
recovery level was in all cases higher (Barat et al., 1998,
Table 2
Process steps in osmotic dehydration, driven forces and phenomena responsible for changes in the system free energy
Process step Time range Driven force Dissipative free energy
phenomena
Storage free energy
phenomena
Impregnation (capillary, VI) Minutes Pressure gradients Flow of external liquid Volume reduction (gas
phase)
Osmotic dehydration Hours Chemical potential of
components (mainly
water)
Water loss Volume loss of cells
Solute gain
Plasmolysis
a
Deformation of cellular
matrix
Liquid ow through cell
wall
a
Impregnation Days Pressure gradients Relaxation of cellular
network
EQUILIBRIUM
Flow of external uid
a
In osmotic processes where no VI with osmotic solution has been carried out these phenomena occur coupled with the relaxation of shrunk cellular
network in the next impregnation step (Fito et al., 1999a).
Fig. 4. Pathway of the structure changes in the cellular tissue throughout osmotic treatments OD and PVOD. (J
HDM
: hydrodynamic ux of external
liquid, J
w
: water ux, is: intercellular space, ic: intracellular content, isgv: intercellular space generated volume, A and B: cell bonding points).
Fig. 5. Drying curves of apple slices (7 mm thick) impregnated (I) and
non-impregnated (NI) with an isotonic solution (air conditions: 2 m/s,
40C) (adapted from Martn et al., 1998).
1999). This has been explained in terms of a greater
irreversibility of deformations induced in the cell net-
work by OD, associated with the greater cell wall de-
formation (Fig. 4).
Mass and volume gains in long-term osmotic pro-
cesses have great practical interest in fruit candy pro-
cesses. These are improved in PVOD processes as shown
in Table 3 for some candied fruits with 6Brix in their
liquid phase.
Acknowledgements
We thank the Comision Interministerial de Ciencia y
Tecnolog

ia, the UE (STD3 programme) and the CY-

TED Program for their nancial support.
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Table 3
Mass (DM) and volume (DV ) change (referred to the sample initial values) of dierent 65Brix candied fruits obtained by OD or PVOD (at 40C)
with osmotic solutions of increasing concentration (24 h in 45 Brix OS and 24 h in 65 Brix OS)
Treatment OD PVOD
Candied fruit DM (%) DV (%) DM (%) DV (%)
Pineapple )28 )45.8 2 )21.4
Apple )55 )71.3 )20 )38.3