Discoloration Kinetics of Clarified Apple

Juice Treated with Lewatit S 4528

Adsorbent Resin During Processing
Ibarz Albert, Falguera Vctor, Garza
Salvador & Garvn Alfonso

Food and Bioprocess Technology

An International Journal
ISSN 1935-5130
Volume 5
Number 6
Food Bioprocess Technol (2012)
5:2132-2139
DOI 10.1007/s11947-011-0649-9

1 23

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Food Bioprocess Technol (2012) 5:21322139
DOI 10.1007/s11947-011-0649-9

ORIGINAL PAPER

Discoloration Kinetics of Clarified Apple Juice Treated

with Lewatit S 4528 Adsorbent Resin During Processing
Ibarz Albert & Falguera Vctor & Garza Salvador &
Garvn Alfonso

Received: 6 September 2010 / Accepted: 29 June 2011 / Published online: 13 July 2011
# Springer Science+Business Media, LLC 2011

Abstract The present work studies the adsorption of

colored compounds in apple juice with a Lewatit resin S
4528. The sorption equilibrium through the adsorption
isotherms for 20, 35, and 50 C was studied. The
absorbance at 420 nm was used to measure the concentration of colored compounds, which permits correlating the
residual concentration with the adsorbed concentration,
proving that the data matched reasonably well according
to the Langmuir and Freundlich models. Also, the efficiency of the adsorption process was studied for different resin/
juice mass ratios at different temperatures, from which it
was observed that there was an improvement in efficiency
as the resin content increased, while the increase in
temperature was not so important in the process. The
adsorption kinetics at 35 C for different resin/juice mass
ratios was also studied. The kinetic model developed by
Ibarz was used, concluding that the data matched this model
reasonably well. The adsorption kinetic constant was always
higher than the desorption kinetic constant, which indicates
that the adsorption stage predominates the desorption stage.
The adsorption kinetic constant shows a decreasing tendency
with the raise in the resin/juice ratio, and the desorption kinetic
constant shows an increasing tendency. The variation of the
I. Albert : F. Vctor : G. Salvador : G. Alfonso (*)
Food Technology Department, Universitat de Lleida,
Av. Rovira Roure 191,
25198 Lleida, Spain
e-mail: garvin@tecal.udl.cat
I. Albert
e-mail: aibarz@tecal.udl.cat
F. Vctor
e-mail: vfalguera@tecal.udl.cat
G. Salvador
e-mail: garza@tecal.udl.cat

CIELab color parameters (L*, a*, and b*) with the adsorption
time was studied, obtaining results that match the kinetic
adsorption model proposed.
Keywords Adsorption . Kinetics model . Discoloration .
Resin . Apple juice . Browning
Notation
A
Absorbance (dimensionless)
A0
Initial absorbance (dimensionless)
C
Resin concentration in the juice (grams resin/gram
juice)
Z
Adsorption efficiency (%)
m
Adsorbate concentration on resin surface (grams
melanoidins/gram resin)
S
Adsorbate concentration in the juice
(grams melanoidins/gram juice)
m0
Maximum concentration of adsorbate retained in the
juice (grams melanoidins/gram resin)
Kads Equilibrium adsorption constant (Langmuir model,
grams juice/gram resin)
KF
Equilibrium adsorption constant (Freundlich model,
grams juice/gram resin)
n
Constant of adsorption equilibrium (Freundlich
model, dimensionless)
t
Adsorption time (hours)
Kinetic constant of the adsorption stage (grams
ka
juice/gram resin second)
kd
Kinetic constant of the desorption stage (per second)
K
Equilibrium constant of dynamic adsorption
desorption process (grams juice/gram resin)
m
Adsorbate concentration on resin surface in equilibrium
conditions (grams melanoidins/gram resin)
L*
CIELab color parameter (dimensionless)
a*
CIELab color parameter (dimensionless)

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Food Bioprocess Technol (2012) 5:21322139

b*

L0

L1
a

CIELab color parameter (dimensionless)

Initial value of CIELab L* parameter
(dimensionless)
Value of CIELab L* parameter when equilibrium is
reached (dimensionless)
Parameter associated to the discoloration speed
(per hour)

Introduction
Two of the most important stability problems during the
processing of fruit juices are browning and turbid appearance.
In the case of apple juices, the main reason for these changes is
the oxidation of polyphenolic substances (Constenla and
Lozano 1995; Fernndez de Simn et al. 1992; Falguera et
al. 2011).
Browning is one of the most important processes of
deterioration that occurs in fruit juices during processing
and storage (Toribio and Lozano 1984), and consists of the
appearance of colored reaction products. There are two
kinds of browning: enzymatic browning and non-enzymatic
browning (Shahidi and Naczk 1995). Enzymatic browning
is caused by the action of polyphenol oxidase over phenolic
substrates, resulting in melanins. Non-enzymatic browning
is caused by the reaction between the reducing sugars and
the free amino acids that result in melanoidins. Both
melanins and melanoidins are colored products that confer
the juice a dark color.
Different methods are currently used to reduce browning
and the possible turbidity. Turbidity treatment usually takes
place prior to the pasteurization process, and its utility is not to
avoid browning but to allow the reduction of colored
compounds (melanins and/or melanoidins) once they have
been undesirably produced during storage and/or thermal
treatment. One of the methods used to remove the color of
juices is flocculation and later sedimentation through the use
of gelatine and bentonite (Gkmen et al. 2001). This method
has the disadvantage of obstructing the pores of the
membranes used in the clarification stage. A method also
used in the clarification of apple juices by ultrafiltration
is adsorption through polyvinylpolypyrrolidone (PVPP;
Gkmen et al. 2001; Hums et al. 1980), but PVPP has the
inconvenience of being expensive and hard to recover.
Another method that can be used is the photochemical
destruction of these compounds (Ibarz et al. 2005), although
it is expensive and the products of the reaction are not known
and could be toxic. The adsorption method with cheaper and
easier-to-recover adsorbents is an alternative to remove the
colored compounds causing the turbidity that appears in
juices (Carabasa et al. 1998; Fisher and Hofsommer 1992;
Qiu et al. 2007). The adsorbent that meets these requirements
is activated carbon, and it is widely used with good results. If

2133

its particle size is very small, it makes it hard to remove and

able to contaminate the juice. If the size is bigger, the price is
much higher. There are other adsorbent materials such as
zeolites (natural and synthetic), clays, silica gel, exchange
resins, activated alumina, and some synthetic polymers.
Lewatit S 4528 (Lanxess Energizing Chemistry, Edition
2009-11-19; www.lewatit.com) is a food grade resin and
weak basic macroporous anion exchange resin (tertiary and
very low level of quaternary amino groups) based on
polystyrene. According to the manufacturers specifications,
it is suitable in the free base form for the decolorization of
organic products (colorants) such as fruit concentrates. The
manufacturer proposed this research because this resin has
not been studied before as an adsorption resin for decoloring.
Although the adsorption of dark-colored compounds in
apple juice has been studied by several authors (i.e., Gkmen
and Serpen 2002; Ata and Gkmen 2011), the aim of this
research was to study the elimination of color compounds
(melanoidins) when they have been undesirably produced
during the browning reaction of apple juice with a new
adsorbent Lewatit S 4528. For that purpose, isotherms of
the adsorption equilibrium at different temperatures were
obtained and adjusted to the Langmuir and Freundlich
models. The adsorption efficacy according to the resin
concentration, the adsorption kinetics, and the evolution of
color parameters (L*, a*, and b*) with time for different
resin/juice ratios were also evaluated.

Material and Methods

The sample of concentrated apple juice used in this study
was provided by an industry near Lleida (Spain) from the
most prevalent apple varieties (Starking Delicious, Golden
Delicious, and Granny Smith) processed in the Lleida
region. This sample was obtained from apples after the
processes of selection, cleaning, massing, pressing, depectinization, clarification, and concentration up to 65Bx
through evaporation in a Unipektin industrial evaporator
(Unipektin AG, Eschenz, Czech Republic). The soluble
solid content was determined using a digital refractometer
Atago RX-1000 (Atago Co. Ltd., Tokyo, Japan).
The adsorbent resin used was the Lewatit S 4528
(Bayer Chemicals AG, Leverkusen, Germany). Its physical
data are: beige opaque ball-shaped grains with a specific
surface (BET) of 25 m2/g, bead size between 0.4 and
1.25 mm, pore volume of 0.35 cm3/g, pore diameter
between 10 and 70 nm, bulk density of 0.62 g/mL, and
grain density of 1.02 g/mL. The resin was dried by storing in a
vacuum oven at 60 C until constant weight prior to use.
First of all, the samples of the concentrated juice were
thermally treated at 70 C in a laboratory stove for 24 h.
This thermal treatment produced non-enzymatic (Maillard)

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browning reactions (melanoidins) in the juice that, after

being treated, was stored in a fridge at 4 C for further
usage. This thermal treatment also produced the conversion
of polyphenols to colorless forms (Brouillard 1982;
Beveridge et al. 1986). In this way, melanoidin concentration was directly proportional to the absorbance at 420 nm,
as was prior studied by Martins and Van Boekel (2003). The
melanoidin content was obtained as the absorbance variation, as Falguera et al. (2010) did with melanins.
Absorbance measures were taken in a Helios gamma
spectrophotometer (Thermo Fisher Scientific Inc., Waltham,
USA) at 420 nm.
Equilibrium Model
Adsorption consists of the separation of a substance from a
phase through its accumulation or concentration on the
surface of the adsorbing phase. This transference process
takes place until the conditions of dynamic equilibrium are
reached, being then when the solution concentration
remains constant, although the adsorption and desorption
with equal rates still take place. The adsorption isotherms
describe the relations between the equilibrium concentrations of the adsorbate in the adsorbing phase (m) and in the
fluid phase (S) at a fixed temperature. The Langmuir and
Freundlich models are the most widely used to describe the
relation between both concentrations.
If a single adsorbate is only retained on a molecular
surface, the Langmuir model can be described as follows
(Langmuir 1918):
m
Kads S

m0 1 Kads S

where m0 is the maximum concentration of adsorption

retained by the adsorbent, Kads is the constant of adsorption
equilibrium, and S is the concentration of the adsorbate in
the fluid phase. Both parameters depend on the temperature
and the adsorbateadsorbent system; thus, for a specific
application at a fixed temperature, both remain constant.
The Freundlich model is empirical and can be described
with the following power equation (Freundlich 1906):
m kF S n

where kF and n are adsorption parameters that depend on

the temperature and the adsorbateadsorbent system.
To evaluate the adsorption efficiency of the colored
compounds contained in a browned juice through resins,
the following equation can be used:
Z %

A0  A
 100
A0

where A0 is the initial absorbance value and A is the final

absorbance value corresponding to the equilibrium conditions.

The colored compounds retained concentration in the

resin can be obtained from the following equation:
m

A0  A
C

where A0 is the initial absorbance value, A is the concentration

measure of colored compounds (melanins and melanoidins) in
the juice, and C is the resin concentration per juice unit,
defined as grams resin/gram juice.
From the equilibrium constant, thermodynamic parameters such as Gibbs free energy (G), enthalpy change
(H), and entropy change (S) for the adsorption process
can be obtained using the following equations (Gkmen
and Serpen 2002):
G RT ln Kads
ln Kads

S H

Van0 t Hoff 0 s equation
R
RT

5
6

where Kads is the adsorption equilibrium constant, T is the

absolute temperature, and R is the universal gas constant.
From the concentrated and thermally treated juice, 12Bx
samples were obtained by dilution with distilled water.
The absorbance measure prior to the addition of resin
provides information on the initial content of melanoidins
in the juice.
A preliminary study was carried out to determine the
necessary time to reach the dynamic equilibrium between
the fluid phase (juice) and the adsorbent (resin). For that
purpose, the absorbance was measured during 24 h for each
of the resinjuice relation studied.
A known quantity of resin in the range of 0.53.5 g was
added to 50 g of juice. In this way, several samples were
obtained with a resin concentration in the juice between 0.01
and 0.07 g resin/gram juice. The recipients containing the juice
and resin were placed for 24 h in a Bunsen BTG 1620
thermostatic shaking bath (Bunsen, Madrid, Spain) with a fixed
working temperature, with the aim of reaching the equilibrium
conditions at that temperature. Once the equilibrium conditions
were reached, the samples were filtered using porous cellulose
nitrate membranes (Whatman International Ltd., Maidstone,
England) with a pore diameter of 0.45 m. Finally, the
absorbance at 420 nm was measured to obtain the content of
melanins and melanoidins in the juice (S). This process was
carried out at temperatures of 20, 35, and 50 C. All the
experiments were done in triplicate.
Kinetic Model
To carry out a kinetic study of the adsorption process, it is
necessary to define a mechanism that allows obtaining a
kinetic equation that properly describes the adsorption
process. One of these models is based on considering the

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2135

For each resin/juice ratio, seven samples were prepared,

one for each time: 0.5, 1, 2, 3, 4, 5, and 6 h. After the
corresponding time of adsorption, these samples were
filtered through a 0.45-m membrane filter prior to the
measurement of absorbance values at 420 nm and
measuring the CIELab color parameters (L*, a*, and
b*). In the CIELab color space, L* stands for luminance,
a* is the redgreen axis, and b* corresponds to the blue
yellow axis. In this way, small values of a* and b* mean
that the sample is less colored. The color parameters L*,
a*, and b* were obtained with a Macbeth Color Eye 3000
spectrophotometer (Macbeth-Kollmorgen Int. Corp.,

Fig. 1 Evolution of adsorption efficiency (Z) with resin/juice ratios at

different temperatures

process as two-staged, one of adsorption and another of

desorption, both of them being first-order kinetic stages
(Langmuir 1918). This model has the disadvantages that it
is necessary to know the equilibrium constant in order to
calculate the equation parameters and the desorption
constant cannot be measured independently. To work out
this inconvenience, an approximate geometric model has
been developed (Kuan et al. 2000; Qiu et al. 2007) to
calculate the two constants.
Ibarz et al. (2008) developed an equation to describe the
variation with time of the adsorbate contents (colored
solute) in the resin:
dm
k a  kd m
dt

where m is the adsorbate concentration on resin surface, t is

the time, ka is the kinetic constant of the adsorption stage,
and kd is the kinetic constant of the desorption stage.
This equation can be integrated with the boundary
condition that the initial concentration of colored compounds
in the resin is zero, obtaining the following equation:
m K1  ekd t

For high values of t, in which the equilibrium has been

reached:
m1 K

ka
; ka m 1 kd
kd

which shows that the rates of the two stages of color compound
liberation and retention are in dynamic equilibrium.
A fixed quantity of resin (0.5, 1.0, or 1.5 g) was
placed in an empty recipient. Subsequently, 50 g of
browned juice was added and the recipient was placed in
a thermostatic bath with a constant temperature of 35 C.

Fig. 2 a Colored compounds adsorption isotherms on adsorbent resin

at different temperatures. b Adsorption isotherms compared with the
linearized Langmuir model. c Adsorption isotherms compared with
the linearized Freundlich model

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Table 1 Parameters for Langmuir

and Freundlich isotherms

Langmuir model
m
m0

Freundlich model

Kads S
1K
ads S

m kF S n

T (C)

m0

Kads

R2

KF

R2

20

23.752.32

7.951.84

0.9834

27.653.93

0.430.08

0.9593

35
50

37.261.09
81.988.82

8.700.61
3.790.48

0.9988
0.9836

46.495.04
86.2510.01

0.460.06
0.610.15

0.9826
0.9470

Neuburgh, NY, USA) and the Macbeth Optiview software,

which uses the curve corresponding to the light source D75 and observer of 10. All absorbance measurements for the
adsorption process were corrected with those of the control
sample for each corresponding time interval in order to
exclude thermal effect on the measured absorbances.
Color Evolution
A consequence of melanoidin adsorption is the discoloration
of the juice. Thus, to know the adsorption kinetics, the
evolution of the L*, a*, and b* CIELab parameters can be
studied. The following equation is used for L* (Carabasa and
Ibarz 2000; Ibarz et al. 1999):

L L0 L1  L0 1eat

10

where L0 is the L* parameter at time 0, L1 is the L*

parameter once the equilibrium is reached, and a is a
parameter associated with the discoloration rate.
Statistical Analysis
The experimental results obtained were fitted to the
mathematical models by using the Statgraphics (version
Plus 5.1, STCSC Inc. Rockville, Md, USA) software for
data processing. All the fittings and the estimates were
calculated at a 95% significant level. All experiments and
analysis were carried out in triplicate.

a 24-h time frame; thus, the 24-h period is adequate for this
experiment.
Adsorption Efficiency
Figure 1 shows the variation in the adsorption efficiency
(z) for resin concentrations (C) at different temperatures. It
can be observed that the efficiency of the adsorption
increases with temperature between 20 and 35 C. When
temperature rises, the motion of the pigments in the juice
increases. This behavior favors the different adsorption
stages (external transference and diffusion inside the
resin), making the adsorption of the colored compounds
on the surface and inside the resin favored. It was also
observed that the adsorption efficiency asymptotically
increases with the resin concentration, which is evident
since a rise in the resin concentration entails a rise in the
adsorption surface. Minimal temperature influence on
adsorption efficiency was observed with higher resin
concentration in the juice; thus, at a low resin concentration, the adsorption efficiency was temperature-dependent.
These results are consistent with the studies on vinegar
presented by Achaerandio et al. (2002), on clarified peach
juice by Carabasa et al. (1998), on peach juice by Ibarz et
al. (2008), and on detergent by Leyva-Ramos (1989).
Between 35 and 50 C, the adsorption efficiency is

Results and Discussion

The preliminary experiment conducted has shown that a
dynamic equilibrium between phases can be obtained with
Table 2 Thermodynamic parameters
T (C)
20
35
50
S (kJ/(molK))
H (kJ/mol)

Kads

G (kJ/mol)

7.95
8.70
3.79
0.046
19.02

5.052
5.540
3.578
Fig. 3 Resin adsorption dynamic curves, at 35 C, for three different
ratios resin/juice

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Table 3 Kinetic constants
values in an adsorption process
for different resin/juice ratios
at 35 C

dm
dt

2137

ka  kd m $ m K 1  ekd t

Ratio (g resin/
g juice

k (a.u. g juice/
g resin h)

kd (h1)

m1 K ka =kd
(g juice/g resin)

R2

0.01

7.811.44

0.450.13

17.351.81

0.9868

0.02
0.03

7.371.22
7.150.38

0.580.13
0.690.05

12.710.74
10.360.20

0.9894
0.9987

temperature-independent, as was found by Fischer and

Hofsommer (1992) and Kim et al. (1992).
The fact that temperature has little effect on adsorption efficiency, along with the inconveniences related to
raising the temperature and the resin concentration
(favoring the non-enzymatic browning, warming overcost, and higher resin consumption over-cost), suggests
working with the lower temperature and the lower resin
concentration that allow obtaining a juice according to a
colorimetric level prior defined. If a low color level was
desired, the process should use temperatures between 35
and 50 C.
Adsorption Isotherms
Figure 2 shows that for a fixed absorbance value, the m
variable rises with temperature. The reason is that, as it is
known, the temperature rise causes a viscosity reduction
(Augusto et al. 2011) and, therefore, a diffusion acceleration
of the colored compounds in the juice is produced,
improving the global adsorption process.
Equilibrium data were adjusted according to the
Langmuir and Freundlich models, which are the most
widely used in the case of mono-compound systems in
which the solute is kept in an only molecular surface.
Table 1 shows the parameters of the adjustments of the
experimental data to the Langmuir and Freundlich models,

Fig. 4 Evolution of lightness with time of adsorption

and Fig. 2 shows the fits. Figure 2 and the coefficients of

determination of the adjustments of the data with the two
adsorption isotherms reveal that the two models permit
properly describing the behavior of the adsorption isotherms.
In Table 1, it can be observed that the adsorption
equilibrium constant of the Langmuir model, K ads ,
decreases with the temperature increase. A value of Kads
higher than the unit shows that the process is a favorable
type adsorption (McCabe et al. 1993). It can also be
observed that the maximum concentration of the adsorbed
solute per adsorbent weight unit, m0, increases with
temperature. With regard to the Freundlich model, the KF
constant increases with temperature; the n exponent also
increases with temperature, being <1 in all cases. The main
difference between the Langmuir and Freundlich models is
that the Langmuir model is obtained as a theoretical process
with simultaneous adsorption and desorption stages, both of
them with first-order kinetics, while the Freundlich model
is totally empirical.
Thermodynamic Parameters
Table 2 shows the thermodynamic parameters obtained
for the adsorption process. The negative values of G for
all the temperatures tested indicate the spontaneous
nature of the adsorption process, as was obtained by

Fig. 5 Correlation between lightness and adsorption (m)

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Table 4 Adjustment parameters
of L* evolution for different
resin/juice ratios at 35 C

Food Bioprocess Technol (2012) 5:21322139

Ratio resin/juice (g resin/g juice)




L L0 L1  L0 1eat

R2

L0

L1

0.01
0.02

89.690.42
89.370.66

94.240.60
94.680.43

0.480.18
0.920.32

0.9901
0.9860

0.03

90.350.76

95.140.43

1.120.48

0.9778

Gkmen and Serpen (2002). The increment in the G

values with temperature indicates that the adsorption
process is not favored by an increase in temperature. The
fact that the value of H is negative indicates the
exothermic nature of the adsorption process. The slightly
negative value of S shows the slightly decreased
randomness at the solid/solution interface during the
adsorption process.
Adsorption Kinetics
Figure 3 shows the evolution of the concentration of the
colored compounds that are retained by the resin at a
temperature of 35 C for different resin/juice ratios. It can
be observed that the pigment concentration in the solid
phase (m) rises with resin/juice contact time, reaching an
asymptote that corresponds to the equilibrium achievement,
as occurs in mass transfer when the driving force depends
on the difference between the concentration and the
equilibrium concentration. After 6 h, the variation of the
parameters was meaningless. The experimental data fitted
Eq. 8. Table 3 shows the values obtained in the adjustments.
In all cases, it can be observed that the value of the kinetic
constant of the adsorption stage (ka) is higher than the
kinetic constant of the desorption stage (kd). This fact
allows the adsorption of the colored compounds in the solid
structure of the resin.
Figure 4 shows the evolution of the L* parameter. It can
be observed that this evolution follows asymptotic kinetics
with adsorption time, which is consistent with the evolution
of the m concentration in Fig. 3, in accordance with the fact
that the adsorption kinetics consists of two stages (adsorption
and desorption).
Figure 5 shows the correlation between L* and m,
showing that the greater the adsorption, the lighter the juice
becomes.
Table 4 shows the adjustment parameters of the L*

parameter with Eq. 10. The initial parameter, L0 , is almost

the same in all cases; the equilibrium value, L1 , is also

very similar. Thus, the total discoloration does not depend
on the resin/juice relation in the ratio of the studied
concentrations. The value of the a* parameter increases
with the resin/juice mass ratio. This can be caused by the
fact that when raising the resin/juice ratio, the interphase

surface also rises, and therefore the material transference

rate behaves in the same way.
Figure 6 shows the evolution of the a* and b*
parameters, proving a loss of color because of the decrease
of both parameters. Initially, both values decrease, but
from a certain time (lower as the resin concentration gets
higher), the a* parameter almost does not change and only
the b* parameter continues its decrease. A higher resin/
juice ratio entails a higher reduction of both parameters,
especially for b*. The global process is a reduction of the
reddish colors.

Conclusion
The adsorption efficacy does not clearly rise when
temperature increases and rises when the amount of resin
used increases. Considering the technical and economic
disadvantages associated with these optimal conditions, the
most reasonable option is to work with the lowest
parameters for both of them that allow obtaining the desired
characteristics of juice coloring.
The adsorption process is spontaneous, exothermic, and
not favored by an increase in temperature.
The values of the kinetic constant of the adsorption stage
are higher than the ones of the desorption stage. Thus, the

Fig. 6 Evolution of color parameters a* and b* with time of

adsorption

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Food Bioprocess Technol (2012) 5:21322139

concentrations of adsorbed colored compounds in the

steady state are high.
The evolution of the adsorbed concentration values (m) and
the L* parameter values follows an increasing exponential
function, in accordance with the observed adsorption kinetics.
The greater the adsorption, the lighter the juice becomes.
The evolution of the a* and b* parameters shows a color
reduction, which continued for the b* parameter but limited
for the a* parameter, which is globally appreciated as a
reduction of the reddish colors.

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