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1
C
C
0
dt (1)
where Q is the column feed ow rate (mg min
1
), C is the outlet
concentration (mg L
1
), C
0
is the inlet concentration (mg L
1
) and
t
sat
is the time required for the bed to become saturated (min).
The bed capacity (q
bed
, mg g
1
) is a parameter that determines
the amount of avor recovered by the xed bed per gram of
adsorbent present in the bed and is calculated from Equation (2),
where m is the mass of activated carbon present in the bed (g)
(Calero et al., 2009; Chen et al., 2012; Salman et al., 2011):
q
bed
q
total
m
(2)
The total amount of benzaldehyde fed into the column until full
bed saturation (W, g) can be calculated using Equation (3) (Aksu &
G onen, 2004; Calero et al., 2009):
W
QC
0
t
sat
10
6
(3)
The bed performance (P) relates the amount of aroma retained
in the bed (q
total
) with the amount of aroma fed in the same run (W)
(Aksu & G onen, 2004; Calero et al., 2009; Chen et al., 2012). A high
performance indicates a good operational set up, and the perfor-
mance can be calculated using Equation (4):
P%
q
total
W
100 (4)
The adsorbent utilization (h) relates the total capacity obtained
in the xed bed (q
total
) with the total capacity obtained in a batch
experiment (q
batch
) and therefore represents the amount of active
sites that are not utilized in the xed bed. This parameter is
calculated from Equation (5):
h
q
bed
q
batch
(5)
The residence time, which affects the shape of the breakthrough
curve and the breakthrough time (Singh et al., 2009), is the time
required for the uid to ll the empty column (Ko et al., 2000). This
parameter is the most important in the design of a xed bed
(McKay & Bino, 1990), and effects in the residence time may be
easily observed as a result of changes in the bed depth and feed
ow rate. The true residence time (TRV) can be calculated from
Equation (6):
TRV
V
L
Q
(6)
Where is the bed porosity and V
L
is the volume occupied by the
adsorbent inside the bed (mL). The bed porosity can be estimated
by the fraction of empty spaces (volume of distilled water present
in the xed bed after packing (mL) divided by the xed bed volume
(mL)).
1.2. Scale-up study
The bed depth service time (BDST) model predicts the rela-
tionship between the bed depth, Z (cm), and the operation time, t
(min). This model assumes that the adsorption rate is controlled by
the surface reaction between the adsorbate and the unused ca-
pacity of the adsorbent (Srivastava et al., 2008; Zou, Zhao, & Zhu,
2013). Equation (7) expresses a linear relationship between the
bed depth and the service time:
t
N
0
C
0
v
Z
1
K
BDST
C
0
ln
C
0
C
t
1
(7)
where N
0
is the adsorption capacity (mg mL
1
), v is the uid ve-
locity (cmmin
1
), C
t
is the outlet concentration at time t (mg mL
1
)
and K
BDST
is the mass transfer coefcient (mL (mg min
1
)). K
BDST
and N
0
can be calculated from the linear and angular coefcient,
respectively, from the graph of t as a function of Z at a given C
t
/C
0
ratio (iso-concentration line).
At 50% breakthrough (C
t
/C
0
0.50 and t t
0.50
), the linear term
of Equation (7) becomes indeterminate (ln(1)), and the equation is
thus reduced to Equation (8):
t
0;50
N
0
C
0
v
Z (8)
Thus, the graph of t
0.50
at 50% breakthrough as a function of Z
forms a line passing through the origin, and N
0
can be calculated by
the angular coefcient (Srivastava et al., 2008). A simplied form of
the BDST model is expressed by Equation (9) (Goel et al., 2005):
t aZ b (9)
a
N
0
C
0
v
(10)
b
1
K
BDST
C
0
ln
C
0
C
t
1
(11)
where a is the angular coefcient (min cm
1
) and b is the linear
coefcient (min) of the straight line obtained with Equation (7).
A.M.D. Canteli et al. / LWT - Food Science and Technology xxx (2014) 1e8 2
Please cite this article in press as: Canteli, A. M. D., et al., Fixed-bed column adsorption of the coffee aroma compound benzaldehyde from
aqueous solution onto granular activated carbon from coconut husk, LWT - Food Science and Technology (2014), http://dx.doi.org/10.1016/
j.lwt.2014.06.015
The slope of Equation (9) at velocity v can be used to obtain the
angular coefcient for a different velocity v
0
using Equation (12):
a
0
a
v
v
0
(12)
where a is the angular coefcient for the new velocity, v
0
(cm min
1
). The model assumes that the linear coefcient does not
change as the velocity is varied.
2. Materials and methods
2.1. Adsorbent
Granular activated carbon derived from coconut husks (CAR-
BOMAFRA
t
exp
t
cal
t
exp
100 (14)
3. Results and discussion
3.1. Column study
In a previous study, the total capacity of the adsorbent obtained
from batch studies (q
batch
) was 251.2 2.3 mg g
1
, and this value
was used to obtain the values of h. The average estimated porosity
was 0.56 0.013, and this value was used to obtain the TRV for each
run.
3.1.1. Effect of the inlet concentration
Fig. 2a shows the effect of changing the inlet concentration in
the range of 91.9e440.0 mg L
1
while keeping the other parameters
constant. These results are presented in Table 2 (runs 1, 2 and 3).
The change in the concentration gradient signicantly affects the
carbon saturation rate. At lower values of the aroma inlet concen-
tration, the shape of the curve is less pronounced, indicating that
Fig. 2. Comparison of experimental breakthrough curves for benzaldehyde adsorption onto an activated carbon packed column at T 293 K and D 9.2 mm. (a) Curves obtained
with varied inlet concentrations (C
0
): 91.9 mg L
1
, B 272.6 mg L
1
and , 440.0 mg L
1
. In these runs, Z 60 mm, Q 11.8 mL min
1
, M 2 g and v 17.7 cm min
1
. (b)
Curves obtained with varied feed ow rates (Q): 3.9 mL min
1
, 7.8 mL min
1
and 11.8 mL min
1
. In these runs, Z 30 mm, M 1 g, and v 5.9e17.7 cm min
1
. (c)
Curves obtained with varied bed depths (Z): ; 30 mm, A 60 mm and 90 mm. In these runs, Q 11.8 mL min
1
, M 1e3 g and v 17.7 cm min
1
.
Table 2
Comparison of activated carbon xed-bed performance for benzaldehyde adsorp-
tion under different experimental conditions.
TRV (min) q
bed
(mg g
1
) q
total
(mg) h W (g) P (%) t
sat
(min)
Run 1 0.18 142.0 284.1 0.56 0.552 51.4 510
Run 2 0.18 165.6 331.3 0.66 0.658 50.3 205
Run 3 0.18 165.3 330.6 0.65 0.777 53.1 120
Run 4 0.26 217.5 217.5 0.86 1.05 20.6 626
Run 5 0.13 206.6 206.6 0.82 1.25 16.4 330
Run 6 0.09 184.5 184.5 0.73 0.86 21.3 165
Run 7 0.18 187.5 375.1 0.74 1.400 26.8 270
Run 8 0.27 239.4 718.3 0.95 3.654 19.6 740
Run 9 0.35 214.7 429.4 0.85 1.817 23.6 780
Run 10 0.16 181.7 363.4 0.72 1.572 23.1 300
Run 11 0.15 192.8 385.7 0.77 1.562 24.7 300
Run 12 0.09 170.7 341.4 0.68 1.884 18.1 210
A.M.D. Canteli et al. / LWT - Food Science and Technology xxx (2014) 1e8 4
Please cite this article in press as: Canteli, A. M. D., et al., Fixed-bed column adsorption of the coffee aroma compound benzaldehyde from
aqueous solution onto granular activated carbon from coconut husk, LWT - Food Science and Technology (2014), http://dx.doi.org/10.1016/
j.lwt.2014.06.015
adsorption occurs slowly, whereas an increase in the inlet con-
centration increases the steepness of the slope, causing the adsor-
bent to saturate in less time. In addition, lower concentration
gradients cause the transport within the pores to occur slowly due
to reductions in the coefcients of diffusion and/or mass transfer
(Aksu & G onen, 2004), which results in an increase in the satura-
tion time. P (%) does not change signicantly as C
0
increases. The
values of q
bed
, q
total
and h were very similar at higher C
0
(272.6 and
440.0 mg L
1
). At the lowest C
0
(91.9 mg L
1
), all of these param-
eters were lower. These results indicate that changes in the con-
centration gradient between 91.9 and 272.6 or 440.0 mg L
1
affect
the adsorbent saturation rate (as C
0
increases, the driving force also
increases, which implies a reduction in the size of the mass transfer
zone (Goel et al., 2005)). Similar trends have been described in the
literature (Chen et al., 2012; Salman et al., 2011; Tan et al., 2008).
However, the similar q
bed
values obtained at high C
0
were not an
expected result because increasing the inlet concentration from
272.6 to 440.0 should increase q
bed
, a trend that was not observed.
Therefore, there is a limit to the concentration difference be the
driving force for adsorption.
3.1.2. Effect of the ow rate
The effect of the feed ow rate on the adsorption of benzalde-
hyde onto activated carbon was investigated by varying Q from 3.9
to 11.8 mL min
1
while holding the other parameters constant.
Fig. 2b shows the breakthrough curves for different values of Q, and
Table 2 presents these results (runs 4, 5 and 6).
The data shown in Table 2 illustrate that t
sat
, q
bed
, q
total
and h
decrease as Q increases. This result occurs because the time
required for equilibrium between benzaldehyde and activated
carbon is much higher than the retention time (6 h, Zuim et al.,
2011). Therefore, as Q increases, TRV is reduced, which causes a
negative effect on the mass transfer efciency and thus results in a
decrease in t
sat
(Aksu & G onen, 2004; Ko et al., 2000; Singh et al.,
2009). Similar trends have been noted by other investigators in
the literature (Aksu & G onen, 2004; Carpin e et al., 2013; Ko et al.,
2000; Singh et al., 2009).
According to Ko, Porter, and McKay (2001), an increase in the
feed ow changes the diffusion of the lm without changing the
intra-particle diffusion. The movement of the adsorbate from the
solution to the region surrounding the adsorbent causes a con-
centration gradient to develop at this interface, which allows the
adsorbate to cross over the lmand be adsorbed. An increase in the
solution velocity reduces the adhesion of the adsorbate to the
adsorbent and consequently reduces the efciency of the process
(Kundu & Gupta, 2007; Singh & Pant, 2006). The P (%) values ob-
tained for ow rates equal to 3.9 and 11.8 mL min
1
were similar;
however, the P (%) value for the intermediate ow rate was only
16.4%. This result may be explained by the larger amount of
adsorbate fed into the bed (W) to reach bed saturation.
3.1.3. Effect of the bed depth
Fig. 2c shows the effect of changing the bed depth Z between 30
and 90 mm, and the data are shown in Table 2 as sets 6, 7 and 8; the
other parameters remained constant.
As Z increases, t
sat
and q
total
also increase as a result of the higher
number of active sites that are available due to the increase in the
total surface area (increasing the adsorbent mass) as the bed depth
increases (Singh et al., 2009).
At lowers depths (30 and 60 mm), the obtained values for q
bed
and h were similar; however, at a depth of 90 mm, these values
were higher. The shape of the mass transfer zone resembles the
characteristic S of the breakthrough curves, as illustrated in Fig. 2c,
and offers an explanation for these increased values. Another
possible explanation is that the residence time increases as Z
increases and thus results in improvements in the column param-
eters. Similar trends have been previously described in the litera-
ture (Han et al., 2007; Salman et al., 2011; Tan et al., 2008).
As Z increases, P decreases; this result may have occurred as a
result of the tail formed at higher bed depths. The increase in the
tail implies a higher benzaldehyde loss, which reduces the column
performance. An inverse relationship between h and P was
observed. As the adsorbent becomes saturated, more adsorbate is
consumed.
According to Cooney (1991), the gradual approach of C/C
0
to 1
(called the tail) in the breakthrough curves occurs when intra-
particle diffusion is the rate-limiting step.
3.1.4. Effect of the inner diameter
i) DQM
Fig. 3a shows the effect of changing the inner diameter from 6.2
to 12.2 mm, and the data are shown in Table 2 as runs 10, 7 and 11.
The shape of the mass transfer zone does not change signicantly
when the column inner diameter is altered. As D increases, q
bed
,
q
total
and h increase due to the longer contact time between the
adsorbate particle and the adsorbent particle caused by the
reduction in uid velocity, which favors aroma adsorption.
ii) DQZ
The effect of changing the inner diameter from9.2 to 12.2 mmis
shown in Fig. 3b, and the data are shown in Table 2 as runs 6 and 11.
The values of q
bed
and h increase as D increases. This effect may be
due to the lower velocity required to maintain a constant Q, which
would result in a longer contact time for benzaldehyde with the
adsorbent and thereby promote adsorption. The values of q
total
and
t
sat
also increase as D increases because the larger diameter ac-
commodates more adsorbent and increases the number of active
sites present in the bed. P also increases as D increases, and this
effect may be due to the more complete mass transfer zone of the
larger-diameter column. This result agrees with similar trends that
were previously reported in the literature (Singh et al., 2009;
Srivastava et al., 2008).
iii) DVM
Fig. 3c shows the effect of changing the inner diameter from 6.2
to 12.2 mm, and the results are shown in Table 2 as runs 9, 7 and 12.
The other parameters were maintained constant. The data in
Table 2 illustrate that an increase in D results in decreases in q
bed
, h
and t
sat
. The reduction of these parameters is due to the decrease in
TRV as D increases and the bed depth decreases. Thus, at lower
diameters, benzaldehyde has a longer contact time with the acti-
vated carbon, which promotes higher adsorption. This effect, in
addition to the increase in turbulence, weakens the solideliquid
interaction, which disfavors adsorption (Goshadrou & Moheb,
2011).
iv) DVZ
The effect of changing the internal diameter from9.2 to 12.2 mm
is shown in Fig. 3d, and the results are shown in Table 2 as runs 6
and 12. Increasing the inner diameter changes the tendency of the
breakthrough curve. The breakthrough curve for higher D saturates
faster until C/C
0
is approximately 0.8. After this value, the saturation
rate decreases, and the curve for the lower D saturates before the
higher D. Table 2 indicates that the values of q
bed
, P and h decrease
as D increases. This result may be due to the difculties associated
A.M.D. Canteli et al. / LWT - Food Science and Technology xxx (2014) 1e8 5
Please cite this article in press as: Canteli, A. M. D., et al., Fixed-bed column adsorption of the coffee aroma compound benzaldehyde from
aqueous solution onto granular activated carbon from coconut husk, LWT - Food Science and Technology (2014), http://dx.doi.org/10.1016/
j.lwt.2014.06.015
with packing a larger diameter bed. As expected, t
sat
and q
total
in-
crease as D increases due to the increased number of active sites
present in the xed bed.
3.2. Scale up
Fig. 4 shows the iso-concentration lines for benzaldehyde re-
covery in a xed bed at 20, 40, 50 and 60% breakthrough. The
angular coefcient values do not vary signicantly, as shown in
Table 3. The line obtained for 50% saturation does not pass through
the origin (b s 0). Sharma and Forster (1995) and Zulfadhly,
Mashitah, and Bhatia (2001) obtained the same behavior and
developed a complex adsorption mechanism, which involves more
than one rate-limiting step. The equation obtained using a owrate
of 11.8 mL min
1
was used to predict the performance for the other
Fig. 3. Comparison of experimental breakthrough curves with different inner diameters at T 293 K. (a) Curves obtained with varied inner diameters (DQM): 12.2 mm,
B 9.2 mm and , 6.2 mm. In these runs, Z 30e120 mm, Q 11.8 mL min
1
, M 2 g and v 10.1e39.0 cm min
1
. (b) Curves obtained with varied inner diameters
(DQZ): 12.2 mm and < 9.2 mm. In these runs, Z 30 mm, Q 11.8 mL min
1
, M 1e2 g and v 10.1e17.7 cm min
1
. (c) Curves obtained with varied inner diameters (DVZ):
12.2 mm, A 9.2 mm and ; 6.2 mm. In these runs, Z 30 mm, Q 11.8e20.7 mL min
1
, M 1e2 g and v 17.7 cm min
1
. (d) Curves obtained with varied inner diameters
(DVZ): 12.2 mm, and 9.2 mm. In these runs, Z 30 mm, Q 11.8e20.7 mL min
1
, M 1e2 g and v 17.7 cm min
1
.
Fig. 4. Iso-recovery lines for breakthroughs of , 0.20, B 0.40, 0.50 and
0.60 for different bed depths. T 293 K; C
0
440.0 mg L
1
; v 17.7 cm min
1
;
D 9.2 mm; and Z 30e90 mm.
Table 3
Predicted parameters for the BDST model at 11.8 mL min
1
.
C
t
/C
0
a (min cm
1
) b (min) K
BDST
(mL
(mg min)
1
)
N
0
(mg mL
1
)
R
2
ERRSQ
0.20 10.7 0.7 24.0 4.7 0.130 82.23 0.9910 9.375
0.40 10.8 0.8 9.0 5.6 0.101 82.87 0.9873 13.500
0.50 11.0 0.9 2.6 6.2 e 84.1 0.9848 16.666
0.60 11.2 1.4 6.3 9.1 0.144 86.06 0.9697 35.042
A.M.D. Canteli et al. / LWT - Food Science and Technology xxx (2014) 1e8 6
Please cite this article in press as: Canteli, A. M. D., et al., Fixed-bed column adsorption of the coffee aroma compound benzaldehyde from
aqueous solution onto granular activated carbon from coconut husk, LWT - Food Science and Technology (2014), http://dx.doi.org/10.1016/
j.lwt.2014.06.015
feeding ow rates (7.8 and 3.9 mL min
1
), and these results are
presented in Table 4.
The data shown in Table 4 indicate that the errors (E) were low
and that good predictions were obtained with ow rates of 7.8 and
3.9 mL min
1
. Therefore, the constants obtained using the BDST
model could be used to predict the times at which the ratio C
t
/C
0
equals 0.20, 0.40, 0.50 and 0.60 for other ow rates.
4. Conclusions
The adsorption of benzaldehyde from an aqueous solution onto
activated carbon was investigated in a xed bed column at 293 K.
The effects of the inlet concentration, feed ow rate, bed depth and
inner diameter on adsorption were investigated. In general, the
evaluated parameters improved as a result of increases in Z and
decreases in Q. These performance metrics also improved as C
0
was
increased; however, this improvement in performance exhibited a
limit at higher concentrations.
An increase in the inner diameter without changing Q resulted
in an improvement in the column parameters. However, when V
was held constant, increasing D reduced the aroma adsorption. The
effect of the inner diameter was studied in four different ways, and
the results showed that a decrease in the inner diameter while
maintaining the contact time between the adsorbate and adsorbent
constant resulted in improvements in most of the response vari-
ables. However, the low surface area when V and Z were held
constant (DVZ) resulted in a lower total adsorption at small inner
diameters.
The shape of the breakthrough curve was different in almost all
of the runs with the exception of the run in which D was changed
and the feed owrate and the amount of adsorbent in the xed bed
were held constant. Additionally, there is likely more than one rate-
limiting step in the adsorption of benzaldehyde onto activated
carbon because the formation of a tail was observed in most of the
runs. The scale-up study also indicated that there is more than one
limiting rate. The BDST model was applied to the experimental data
and used for the scale-up study, demonstrating that this model is
suitable for scaling up the system.
Zuim et al. (2011) proposed the use of the batch adsorption
process for the recovery of benzaldehyde and achieved good re-
sults, although the process is usually not applicable to industry. The
results obtained in this work are very promising, as demonstrated
by the high aroma recovery rate achieved with the continuous
system, and should be useful for further applications involving
coffee aroma adsorption.
Acknowledgments
The authors are grateful for the scholarship and the research
grant provided by Coordena~ ao de Aperfeioamento de Pessoal de
Nvel Superior and the support provided by the Graduation Pro-
gram of Food Engineering (Federal University of Paran a, Curitiba,
Brazil).
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Table 4
Predicted breakthrough times based on the BDST parameters for new ow rates of
7.8 and 3.9 mL min
1
.
C
t
/C
0
a' (min cm
1
) b' (min) t
cal
(min) t
exp
(min) E (%)
Q 7.8 mL min
1
0.20 16.1 24.0 24.3 22 10.8
0.40 16.3 9.0 39.7 36 10.4
0.50 16.5 2.6 46.8 43 8.9
0.60 16.8 6.3 56.9 51 11.7
Q 3.9 mL min
1
0.20 32.2 24.0 72.7 66 8.5
0.40 32.4 9.0 88.4 91 2.8
0.50 32.9 2.6 92.3 102 5.6
0.60 33.7 6.3 107.5 111 3.1
A.M.D. Canteli et al. / LWT - Food Science and Technology xxx (2014) 1e8 7
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Please cite this article in press as: Canteli, A. M. D., et al., Fixed-bed column adsorption of the coffee aroma compound benzaldehyde from
aqueous solution onto granular activated carbon from coconut husk, LWT - Food Science and Technology (2014), http://dx.doi.org/10.1016/
j.lwt.2014.06.015