Chemical Engineering and Processing 41 (2002) 223– 230

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Adsorption equilibrium and breakthrough analysis for sulfur

dioxide adsorption on silica gel
Türkan Kopaç *, Sefa Kocabaş
Department of Chemistry, Zonguldak Karaelmas Uni6ersity, 67100 Zonguldak, Turkey

Received 14 November 2000; received in revised form 4 April 2001; accepted 4 April 2001

Abstract

In this work, the adsorption equilibrium and adsorption rate of sulfur dioxide were investigated on silica gel. A packed bed
adsorber 0.1 m in length and 0.0095 m in diameter was used for the adsorption experiments. The adsorption equilibrium
experiments were carried out at 473 K constant temperature with an initial sulfur dioxide concentration in the range 430–3400
p.p.m. in nitrogen carrier gas. The experimental adsorption isotherms were compared with the Freundlich, Langmuir, and the
linearized form of the Brunauer–Emmett–Teller and the Dubinin– Radushkevitch– Kaganer models by the nonlinear least-
squares estimate method. The Freundlich model gave the best fit with a correlation coefficient greater than 0.98, suggesting a
surface adsorption mechanism for sulfur dioxide adsorption on silica gel. The deactivation model was applied to the adsorption
rate data. It was found that the adsorption rate data fitted well with the deactivation model. Observed adsorption rate constants
and the first-order deactivation rate constants were obtained from the model. The nonlinear least-squares analysis technique was
used to estimate the parameters appearing in the deactivation model. The breakthrough experiments were repeated at 1610 p.p.m.
constant initial sulfur dioxide concentration in a temperature range of 323– 473 K, and the effect of initial sulfur dioxide
concentration and the effect of temperature were investigated on the model results. © 2002 Elsevier Science B.V. All rights
reserved.

Keywords: Sulfur dioxide adsorption; Silica gel; Adsorption isotherms; Deactivation model

1. Introduction Among the dry processes, adsorption has many advan-

Adsorption is used in many fields related to separa-
tion and purification processes, including hazardous
pollutants from flue gases. Sulfur dioxide is believed to
be the major precursor of acid rain so the control of
sulfur dioxide emissions is a significant concern of
research and development, as well as industrial imple-
mentation. There have been various processes devel-
oped or proposed to remove sulfur dioxide from flue
gases. These processes generally fall into two categories
such as wet scrubbing and dry sorption processes.
Because of their simplicity and relatively low cost, dry
sorption technologies for removing sulfur dioxide emis-
sions are increasingly employed by industrial sectors.
* Corresponding author. Tel.: + 90-372-2574010; Fax: +90-372-
2574181.
E-mail address: kopact@karaelmas.edu.tr (T. Kopac).
tages over the others.
Physical adsorption processes offer an alternative
and promising way for the emission control of sulfur
dioxide from combustion gases since they are dry,
self-contained and energy saving. Adsorption processes
could be used to concentrate SO2 in the flue gas (2000 –
3000 p.p.m.) before they are fed in the flue gas desulfu-
rization processes. This solution offers a potential to
significantly reduce the volumetric flow rate of flue gas
treated and, therefore, to greatly increase the efficiency
of the flue gas desulfurization processes. The key to the
success of this adsorption process for SO2 concentra-
tion is mainly dependent on the search or development
of an appropriate adsorbent that possesses the ideal
properties for the selective adsorption of SO2. Among
those commonly used commercial adsorbents, activated
carbon and polymer resin adsorbents were extensively
studied for their SO2 adsorptive properties.

0255-2701/01/$ - see front matter © 2002 Elsevier Science B.V. All rights reserved.
PII: S 0 2 5 5 - 2 7 0 1 ( 0 1 ) 0 0 1 3 7 - 4
224 T. Kopaç, S. Kocabaş / Chemical Engineering and Processing 41 (2002) 223–230
Extensive research work has already been carried out
for sulfur dioxide adsorption on either carbonaceous
adsorbents [1–4] or on metallic oxide sorbents of tran-
sition metals either pure or mixed based on the ele-
ments Fe, Zn, Mo, Mn, V, Ca, Sr, Ba, Co, Cu and W
[1,5].
Kopaç et al. [6] investigated the adsorption proper-
ties of SO2 on 5A, 4A and AW300 type molecular sieve
zeolites in a temperature range of 523–718 K. It was
found out that the adsorption of SO2 on the adsorbents
investigated were found to decrease in the order of
AW300\4A\ 5A. Kopaç [7] used, in another study,
nonisobaric pulse chromatography for the investigation
of the adsorption properties of sulfur dioxide on molec-
ular sieve 13X and activated carbon. Adsorption equi-
librium constants were calculated using the moment
analysis of the chromatographic peaks. They investi-
gated the adsorption of sulfur dioxide in a temperature
range of 353–453 K with the activated carbon, which is
a typical temperature range of desulfurization of flue
gas, and in a temperature range of 523– 673 K with
molecular sieve 13X. Adsorption equilibrium constants
of sulfur dioxide were found to decrease considerably
with increasing temperature. The heat of adsorption of
sulfur dioxide on molecular sieve 13X and the activated
carbon was determined as − 12.4 and − 8.99 kcal/mol,
respectively.
1.1. Adsorption equilibrium and breakthrough analysis
for SO2 adsorption on silica gel
In this work, the adsorption equilibrium and break-
through analysis of sulfur dioxide were investigated on
silica gel.
Equilibrium studies on adsorption have provided in-
formation on the capacity of the adsorbent or the
amount required to remove a unit mass of pollutant.
An adsorption isotherm is characterized by certain
constants, the values of which express the surface prop-
erties and affinity of the adsorbent and can also be used
to compare the adsorptive capacities of the adsorbent
for different pollutants. The adsorption isotherm mod-
els used in this study are Langmuir, Freundlich,
Brunauer– Emmett –Teller (BET) and Dubinin–
Radushkevitch –Kaganer (DRK) models as shown in
Table 2. The Langmuir and Freundlich equation mod-
els are the widely used models because of their simplic-
ity and having the ability to describe experimental
results in wide range of concentrations. The Langmuir
model is valid for monolayer sorption to a surface with
a finite number of identical sites [8,9]. The Freundlich
model does not describe the saturation behavior of the
sorbent, and it is an empirical equation based on sorp-
tion on a heterogeneous surface suggesting that binding
sites are not equivalent and/or independent [8,9]. The
BET isotherm is valid mainly for physical adsorption.
Langmuir considered only monolayer adsorption,
which must be the maximum for chemisorption. How-
ever, physical adsorption is never single-layer adsorp-
tion, except at very low coverages. At these low
coverages, the Langmuir equation might thus hold true,
but for higher coverages there is multilayer adsorption.
The BET isotherm treats this by performing, essen-
tially, a series of Langmuir isotherms. This equation is
used to determine the surface area of porous catalysts
and other materials [8,9].
Dubinin and Radushkevich (DR) put forward an
equation for the estimation of the micro-pore volume
from the low and medium pressure parts of the adsorp-
tion isotherm, and their treatment represents an adop-
tion of the earlier Polanyi theory of adsorption. The
fractional filling of the DR equation was replaced by
the surface coverage, but the new equation (often
termed the DRK equation) has the same form as the
original DR equation [9].
There have been various models in literature for
breakthrough analysis of gas–solid systems. The impor-
tant factors that should be considered in the modelling
of gas–solid reactions are pore and product layer diffu-
sion resistances, changes in pore structure and variation
in surface area during the reaction. The models pro-
posed for gas– solid reactions related with sulfur diox-
ide generally classified into two groups. The models
listed in the first group do not consider pore diffusion
resistance. First group models are extensions of the
unreacted core model and they are limited to small
particle sizes in the order of magnitude of a few mi-
crons. Pore diffusion resistance becomes important es-
pecially at high temperatures and at the initial stages of
the reaction for larger particles. In the second group of
models, pore diffusion resistance is considered together
with product layer diffusion. These models are also
grouped from a different point of view as grain models,
pore models, volume reaction models and deactivation
models. In number of these models, changes in pore
structure during the reaction and variations in diffusion
and reaction parameters are considered [10].
Orbey et al [11] used a model that accounts for
structural changes for the breakthrough analysis of
solid– gas noncatalytic reactions taking place in a
packed-bed reactor. Analytic expressions derived for
the breakthrough curves were successfully used to ana-
lyze the kinetics of the reaction between precalcined
limestone and sulfur dioxide. Effect of film mass trans-
fer, pore diffusion and structural changes on the ob-
served rate were investigated and it has been shown
that the experimental results and the predictions from
the model agree well. Yaşyerli et al. [12] applied the
deactivation model for char gasification with CO2 suc-
cessfully, and indicated that the deactivation model
describes gas–solid noncatalytic reactions more accu-
rately than the unreacted core and volume reaction
 T. Kopaç, S. Kocabaş / Chemical Engineering and Processing 41 (2002) 223–230 225

models. Suyadal et al. [13] applied deactivation model unimodal distribution [8]. Properties of commercial sil-
for the adsorption of trichloroethylene vapor on an ica gels given by Ruthven [8] are presented in Table 1.
activated carbon bed, and found that the deactivation The large-pore material is used in many liquid-phase
model described the experimental breakthrough curves applications, while the small-pore material is widely
more accurately compared with the adsorption used as a desiccant in vapor-phase systems [8].
isotherms given in literature. Kopaç et al. [14] proposed
1.3. Aim of the study
a unit cell model for the reaction of SO2 with activated
soda considering the changes in pore length and radius
A wide variety of sorbents and reactor types are
with reaction extent and variations in product layer
being developed for sulfur dioxide adsorption [15]. The
diffusion resistance, which was shown to be successfully
problem is whether it is possible to obtain reasonable
used in the analysis of experimental observations.
adsorption capacity with these materials. The aim of
In the present study, the deactivation model pro-
this study is to investigate the sulfur dioxide adsorption
posed by Suyadal et al. [13] for the adsorption of
characteristics on silica gel and to obtain the experi-
trichloroethylene vapor on activated carbon was used
mental adsorption isotherms of sulfur dioxide on silica
for the adsorption of SO2 on silica gel as presented in
gel, and to compare these isotherms with various exist-
Table 3. In this model, it was assumed that the packed-
ing isotherm models in literature. The adsorption equi-
bed adsorber could be approximated to a batch-solids
librium data of sulfur dioxide on silica gel was analysed
reactor with a plug constant flow of fluid. The deactiva-
using various adsorption isotherm models such as
tion of the adsorbent was assumed to be first order with
Langmuir, Freundlich, BET and DRK using nonlinear
respect to the solid surface, and an exponential decrease
regression analysis. The other aim of this study is to
was assumed with time in its available surface. The
investigate the sulfur dioxide adsorption breakthrough
other assumptions made were negligible external mass-
curves, to apply the deactivation model proposed by
transfer limitations, isothermal system and the pseudo-
Suyadal et al. [13], and to determine adsorption rate
steady-state assumptions throughout the adsorption
and deactivation rate constants. To investigate the ef-
column.
fect of initial sulfur dioxide concentration and tempera-
ture on sulfur dioxide adsorption rate on silica gel are
1.2. Silica gel the other aims of this study.

Silica gel is a partially dehydrated form of polymeric 2. Experimental

colloidal silicic acid. The chemical composition can be
expressed as SiO2·nH2O. The water content, which is In this work, SO2 adsorption on silica gel was investi-
present mainly in the form of chemically bound hy- gated. Silica gel samples, in the form of 0.1–0.3 mm
droxyl groups, amounts typically to about 5 wt.% [8]. size granules, were packed in stainless steel columns of
On drying, the particles agglomerate to form a microp- 0.1 m length and 0.0095 m I.D. Before packing, silica
orous structure in which the pore size is determined gels were dried at 373 K under vacuum for 2 h, and
mainly by the size of the original microparticles. Bond then weighed and packed to columns. In each adsorp-
formation between adjacent particles occurs with the tion experimental run, about 4.22 g silica gel granules
elimination of water between neighboring hydroxyl was used. The columns were then placed in a tube
groups and the final structure is therefore physically furnace. Nitrogen was the carrier gas used. The experi-
robust. The size of the original microparticles and mental system is shown in Fig. 1. The experimental
consequently the size of the micropores in the final conditions are summarized in Table 2. The packed
dried gel is sensitive to pH and to the presence of other columns were purged with nitrogen for 2 h at the
cations in the solution during precipitation. By careful temperature at which the adsorption experiments would
control of the synthesis conditions, it is therefore possi- be performed. The experimental procedure consisted of
ble to control the pore size, which generally shows a introducing sulfur dioxide containing carrier gas on the
inlet of the adsorbent packed column and measuring
Table 1 the concentration change with time leaving the other
Properties of commercial silica gels [8]
end of the column by a sulfur dioxide gas analyzer.
High area Low area Physical properties of the silica gel samples were
determined using a Quantachrome Autoscan 60000
Specific pore volume (cm3/g) 0.43 1.15 mercury intrusion porosimeter and a Micromeritics He-
Average pore diameter (A, ) 22 140 pycnometer. Apparent densities and total porosity of
Specific surface area (m2/g) 800 340
Pore size distribution Unimodal Unimodal
the samples are 1.59 g/cm3 and 0.26, respectively. The
Particle density (g/cm3) 1.09 0.62 total surface area determined by a Quantachrome Sorp-
tometre is 239 m2/g.
226 T. Kopaç, S. Kocabaş / Chemical Engineering and Processing 41 (2002) 223–230

Fig. 1. Figure of the experimental system.

Experimental runs were carried out at variable inlet
SO2 concentration at a constant temperature of 473 K
and at variable temperatures at constant feed gas
concentration.
2.1. Constant bed temperature
peated for different sulfur dioxide concentrations. The
breakthrough curves were obtained for each different
sulfur dioxide inlet concentration. These concentration
versus time curves were analysed for adsorption
isotherm models and adsorption rates.

These runs were carried out at 473 K constant tem-

perature. At six to ten different sulfur dioxide inlet 3. Results and discussion
concentrations in the range of 430– 3400 p.p.m. in inert
carrier gas, the experiments were performed and break- In the present study, sulfur dioxide adsorption equi-
through curves were obtained for each different sulfur librium and rate on silica gel have been investigated.
dioxide inlet concentration. These concentration versus The experimental adsorption isotherms have been ob-
time curves were analysed for adsorption rates and tained for a temperature of473 K and the experimental
adsorption isotherm models. adsorption isotherms were compared with the adsorp-
tion isotherm models existing in literature as shown in
Table 3.
2.2. Constant inlet gas composition
It was found by the adsorption experiments per-
formed in this work that the adsorption of nitrogen on
These runs were carried out keeping the sulfur diox-
silica gel is negligible as compared with the adsorption
ide inlet concentration at a value of 1610 p.p.m. for
of SO2 on this sorbent. So it is reasonable to consider
temperatures of 373 and 473 K, and of 1500 p.p.m. at
323 K. Concentration versus time curves obtained for
these runs were analysed to investigate the effect of Table 2
temperature on the shape of the breakthrough curves Experimental conditions
and the adsorption rate.
The gas mixture containing a given concentration of Adsorbent Silica gel (0.1–0.3 mm granules)
SO2 was introduced into the system after the constant mads (g.) 4.22
temperature for adsorption was reached. Once the equi- C0,SO2 (p.p.m.) 430–3400
librium uptake of the sorbent was reached, the inlet gas Temperature (K) 473
mixture was switched to pure nitrogen at the same flow Carrier gas N2
rate and desorption was performed subsequently by Carrier gas flow rate (cm3/s) 5.58
Tracer gas SO2
flowing nitrogen through the adsorption column at the Column length (m) 0.10
same temperature as adsorption to check the reversibil- Column diameter (m) 0.0095
ity of adsorption isotherm. This procedure was re-
 T. Kopaç, S. Kocabaş / Chemical Engineering and Processing 41 (2002) 223–230 227

Table 3 orption is seen to be about 10 min at 980 p.p.m. inlet

Adsorption isotherm model results
sulfur dioxide concentration. The experimental adsorp-
Adsorbent Silica gel tion isotherms obtained were compared with the ad-
sorption isotherm models shown in Table 3, and the
Freundlich isotherm, qe = KF C 1/n
e KF = 0.000051 constants appearing in Freundlich, Langmuir and
n= 0.61160 DRK models were determined by the nonlinear least-
r 2 = 0.9818
Langmuir isotherm, qe =(Q obCe)/(1+bCe) Q o = 73.2198
squares estimate method. A quasi-Newton method was
b=0.000127 used to converge the experimental data. As regression
r 2 = 0.7998 did not converge with the original form of the BET
Ce 1 C−1 equation, it was used in linearized form. The results of
BET isotherm, = + Ce qO = −2.8297349
qe(1−Ce) q0C q0C C= 0.999688 these analyses are shown in Table 3. The values of the
r 2 = 0.490 constants of each model with the square of the correla-
tion coefficients (r 2) are tabulated in Table 3. The
DRK isotherm, qe =a exp[−b ln2(Ce)] a= 0.026724
b= −0.010651 goodness of the fit for both linear and nonlinear regres-
r 2 = 0.9857 sion is commonly described by r 2. If the value of r 2 =1,
then the goodness of fit is perfect, but r 2 is always less
then unity. As far as the r 2 values are concerned, it is
seen that the equilibrium data can be better represented
nitrogen as an inert component in the SO2 adsorption. by Freundlich and DRK isotherms with a reasonable
SO2 concentration change in the gaseous phase with accuracy over the concentration range studied in this
respect to time for sulfur dioxide adsorption at 473 K work. Freundlich and DRK isotherms fitted the data
for different SO2 inlet concentrations is shown in Fig. 2. with almost the same correlation coefficient of values
The estimates of the maximum standard errors associ- greater than 0.98 for sulfur dioxide adsorption on silica
ated with the measurements in the experimental data gel at 473 K. Although the agreement of the experimen-
have been determined as 93.4%. It is seen that adsorp- tal data with the predictions of the DRK model (which
tion rate is high in the first 20 min and then decreases. suggests a pore filling mechanism for adsorption) were
In Fig. 3, variation of adsorption percentage of sulfur quite good, numerical values of the adjustable parame-
dioxide on the solid for different sulfur dioxide initial ters came out as negative, which is an unexpected
concentrations is shown. The desorption experimental result. The linearized forms of the BET equation with a
studies in this work showed that the adsorption is correlation coefficient of 0.49 did not give good fit to
reversible in all cases. The desorption curves for sulfur the adsorption data as shown in Table 3, yielding also
dioxide on silica gel are shown in Fig. 4 for two a negative parameter. The Langmuir isotherm did not
different initial sulfur dioxide concentrations of 980 and give a good fit with the experimental data with a
1450 p.p.m. The time required for sulfur dioxide des- correlation coefficient of around 0.79. Langmuir

Fig. 2. Variation of sulfur dioxide concentration in the gas phase with time for adsorption on silica gel at 473 K for different initial sulfur dioxide
concentrations in nitrogen carrier.
228 T. Kopaç, S. Kocabaş / Chemical Engineering and Processing 41 (2002) 223–230

Fig. 3. Variation of adsorption percentage of sulfur dioxide on silica gel with time at 473 K for different initial sulfur dioxide concentrations in
nitrogen carrier.

isotherm is the simplest theoretical model for mono- rate data at these concentrations. The squares of the
layer adsorption that assumes the molecules are ad- correlation coefficients are also shown in this table, the
sorbed at a fixed number of well-defined localized sites values of which are all greater than 0.89, 0.92 and 0.98.
and that each site can hold one adsorbate molecule. It Fig. 7 shows the experimental and model results for
is also assumed that all sites are energetically equivalent three different temperatures of 473, 373 and 323 K. The
and there is no interaction between molecules adsorbed initial sulfur dioxide concentration was 1610 p.p.m. at
on neighboring sites. The predictions of this model 373 and 473 K temperatures, and 1500 p.p.m. for 323
showed that these assumptions did not hold for sulfur K. Model parameters for these temperatures with the
dioxide adsorption on silica gel at 473 K temperature. square of correlation coefficients are also tabulated in
Fig. 5 shows the comparison of the experimental ad- Table 4. From Fig. 7 and the results presented in Table
sorption isotherms of sulfur dioxide with adsorption 4, it can again be concluded that the model gives an
isotherm models. The Freundlich model takes surface
heterogeneities and activity variations into account, and
the good fit of the model predictions with the experi-
mental data suggests a selective surface adsorption
mechanism for adsorption of sulfur dioxide on silica
gel.
For the breakthrough analysis, in this study, the
deactivation model proposed by Suyadal et al. [13] for
the adsorption of trichloroethylene vapor on an acti-
vated carbon bed was applied for the sulfur dioxide
adsorption rate data on silica gel. Fig. 6 shows the
experimental and model results for different initial sul-
fur dioxide concentrations of 600, 850, 1610 and 3400
p.p.m. at 473 K temperature. The dimensionless ad-
sorption rate constant and first-order deactivation con-
stants were calculated by the nonlinear least-squares
estimate method for each initial sulfur dioxide concen-
tration and the results are tabulated in Table 4. As seen Fig. 4. Desorption curves of sulfur dioxide on silica gel at 473 K
from the results, it can be concluded that the model temperature at 980 and 1450 p.p.m. inlet sulfur dioxide concentra-
gives an adequate representation of the sulfur dioxide tions.
 T. Kopaç, S. Kocabaş / Chemical Engineering and Processing 41 (2002) 223–230 229

Fig. 5. Comparison of experimental adsorption isotherms of sulfur dioxide with adsorption isotherm models on silica gel at 473 K.

Fig. 6. Comparison of deactivation model predictions with experimental results at different initial sulfur dioxide concentrations at 473 K.

adequate representation of the experimental break- Acknowledgements

through curves of sulfur dioxide at different tempera-
tures. The good fit of the experimental data with the
deactivation model predictions suggests a significant
decrease of activity of the sorbent with time with
respect to probable changes in pore structure, in the
active surface area and active site distribution of the
sorbent.
This work was funded by Research Fund AFP99-13-
02-08 of Zonguldak Karaelmas University. The authors
would like to acknowledge Professor Dr Gülşen Doğu
of Gazi University and Professor Dr Timur Doğu of
Middle East Technical University for the characteriza-
tion of adsorbent samples.
230 T. Kopaç, S. Kocabaş / Chemical Engineering and Processing 41 (2002) 223–230

Fig. 7. Comparison of deactivation model predictions with experimental results for different temperatures (C0,SO2 =1610 p.p.m.).

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