Journal of Cleaner Production 182 (2018) 372e378

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Journal of Cleaner Production

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Liquid and vapor phase adsorption of BTX in lignin derived activated

carbon: Equilibrium and kinetics study
Dipendu Saha a, *, Nathan Mirando a, Andre Levchenko b
a
Department of Chemical Engineering, Widener University, One University Place, Chester, PA 19013, USA
b
TA Instruments, 159 Lukens Dr, New Castle, DE 19720, USA

a r t i c l e i n f o a b s t r a c t

Article history: Benzene, toluene and xylene (BTX) are few of the chemicals that cause environmental pollution in both
Received 26 June 2017 liquid and vapor phase. In vapor phase, they are classified as volatile organic compounds (VOCs) and
Received in revised form cause both indoor and outdoor air pollution. Although different kinds of activated carbons have been
21 January 2018
used for the adsorptive removal of BTX, the fundamental equilibrium and kinetic data of VOC adsorption
Accepted 7 February 2018
Available online 9 February 2018
in porous carbon are very rare in literature. It order to focus on such fundamental data, in this work,
activated carbon was synthesized from de-alkaline lignin precursor by one-step chemical activation with
KOH. The resultant carbon has the BET surface area of 2250 m2/g and total pore volume 1.1 cm3/g.
Keywords:
Adsorption
Equilibrium and kinetics of liquid phase BTX adsorption were measured upto 100 ppm concentration of
BTX each the component in water. In vapor phase adsorption, automated VTI-SA þ sorption analyzer was
VOC employed with nitrogen as carrier gas and equilibrium and kinetic data were recorded as a function of
Activated carbon varying relative pressure or dew point (p/p0) of BTX. For adsorption isotherms, Henry's law, Langmuir,
Freundlich and Sips models were successfully employed, whereas for adsorption kinetics, pseudofirst
order, pseudosecond order and micropore diffusion model were used to calculate the necessary
adsorption parameters.
© 2018 Elsevier Ltd. All rights reserved.

1. Introduction
Benzene, toluene and xylene (BTX) are the key contributors of
volatile organic compounds (VOCs) and cause environmental
pollution. Besides their vapor form, the liquid forms of BTX are also
released from several industrial or household wastes and causes
aquatic pollution. Indoor air quality is an important aspect of hu-
man health (Jones, 1999). These pollutants can create moderate to
severe health related issues to the person who is exposed to them
for a long period of time. These health hazards include eye, skin or
throat irritation, headache, nausea, fatigue, dizziness, respiratory
disease, weakening of mucus, damage to liver and central nervous
system, cancer and immature mortality (Das et al., 2004; Ehrlich
et al., 1977; Spengler et al., 2001). These VOCs can serve as the
potential precursors for the formation of photochemical smog and
a number of toxic byproducts (Dobre et al., 2014), which are
extremely hazardous to the health and environment, even in very
low concentrations (Dwivedi et al., 2004; Gupta and Verma, 2002).
* Corresponding author.
E-mail address: dsaha@widener.edu (D. Saha).
Among different methods that can remove BTX are absorption,
adsorption, condensation, thermal oxidation and catalytic oxida-

denas et al., 2005). Within these processes, adsorption
tion (Lillo-Ro
in porous materials is considered to be most benign, inexpensive
and regenerable process. Porous or activated carbon has been
widely studied for their adsorption capacity of BTX molecules.
Different types of activated carbons, including activated carbon fi-
bers (ACF) (Foster et al., 1992; Huang et al., 2002; Yun et al., 1998)
granular activated carbons (GAC) (Chiang et al., 1999, 2002; Ryu
et al., 2002; Yun et al., 1999), activated carbon cloth (ACC)
(Dimotakis et al., 1995), biological activated carbon (BAC) (Noll
et al., 1989), or activated carbon pellets (Benkhedda et al., 2000)
have been employed to remove small amounts of different com-
ponents of BTX through adsorption process. Different types of
precursors, like mesophase pitch (Silvestre-Albero et al., 2010),
coconut shell (Kim et al., 2006), wood and different varieties of coal
(Lillo-Ro
denas et al., 2005) are activated by acid or alkali treatment
to synthesize the activated carbons for BTX adsorption. It has been
suggested that high surface area and micropore volume of the
porous carbon is essential for the efficient adsorption of BTX

denas et al., 2005). In a recent
(Silvestre-Albero et al., 2010; Lillo-Ro

https://doi.org/10.1016/j.jclepro.2018.02.076
0959-6526/© 2018 Elsevier Ltd. All rights reserved.
 D. Saha et al. / Journal of Cleaner Production 182 (2018) 372e378
simulation study on benzene adsorption onto porous carbon at
303 K, researchers (Huang et al., 2016) demonstrated that benzene
molecules were adsorbed in the micropores of 14e18 Å diameters
while mesopores provided easy access to the transport of benzene
molecules. It was also demonstrated that the favorable sorption
energy for benzene adsorption was 37.45 kJ/mol while the separa-
tion distance was 5.75 Å from the benzene center of mass to the
carbon surface. In recent times, metal-organic frameworks (MOFs)
(Wang et al 2011, 2013), silica (Kosuge et al., 2007) or zeolite
(Monneyron et al., 2003) based materials were also employed for
the adsorption of different types of VOCs.
Despite porous carbon was most commonly used for the
adsorption of BTX or similar VOCs, the fundamental equilibrium and
kinetics of adsorption data and their model fitting parameters were
rarely or only partially reported (Chiang et al., 2002; Shao et al.,
2006; Cloirec, 2012). In majority of cases, the reported data were
either the maximum adsorption capacity, experimental or simu-
lated breakthrough behavior or thermodynamic aspects of adsorp-
tion. In this work, we have synthesized high surface area powdered
activated carbon (PAC) from lignin and employed them for the
systematic investigation of adsorption isotherms and kinetics of BTX
in both liquid and vapor forms. Finally, we employed the necessary
model fittings to characterize the adsorption behavior.
2. Experimental
2.1. Synthesis and characterization of lignin-derived activated
carbon
The activated carbon was synthesized by one-step synthesis
method from lignin with similar methodology that was used for
other lignin-derived carbons that were synthesized in our lab (Saha
et al., 2017a, 2017b). Typically, 3 g solid de-alkaline lignin (TCI
America) and 3 g of KOH pellets (Alfa Aesar) are mixed together in a
coffee grinder and put them in a porcelain boat. We have employed
1:1 ratio of lignin to KOH as it provided best surface area of the
resultant carbon. The boat is inserted in the alumina tube within
the Lindberg-Blue tube furnace and carbonized in the N2 atmo-
sphere. In a typical fashion, the temperature was ramped to 800  C
at a ramp rate of 10  C/min and dwelled in the final temperature of
2 min. After that, it is cooled down to room temperature in the
same N2 flow. Then, the porcelain boat is taken out and the carbon
is washed in copious amounts of deionized water several times and
then filtered out and dried.
In order to investigate the surface area and pore size distribu-
tion, the carbon is analyzed volumetrically with N2 adsorption-
desorption at 77 K and CO2 adsorption at 273 K in Quantach-
rome's Autosorb-iQ any gas instrument. The activated carbon is
outgassed in the same instrument at 300  C for 3 h before any
adsorption experiment. The temperature of 77 K is obtained by
liquid nitrogen whereas 273 K is maintained by an external tem-
perature (Julabo) with 1:1 mixture of water and propylene glycol as
chilling fluid. The BET surface area is calculated within the p/p0
values of 0.05e0.3. The pore size distribution and total pore volume
is calculated by non-local density function theory (NLDFT) method
and all the calculations are performed in the instrument's built-in
software. The scanning electron microscopic (SEM) images were
obtained in Evex mini SEM II HR 3000 instrument. Thermogravi-
metric analysis (TGA) data were obtained in TA instruments' SDT
Q600 TGA-DSC analyzer.
2.2. Liquid and vapor phase adsorption of BTX
The liquid phase adsorption of benzene, toluene and xylene
(BTX) is carried out in deionized water with benzene, toluene and
373
xylene concentration of 20e100 ppm each. For equilibrium run,
typically, 25 mL of each of the solution is stirred with 0.025 g
activated carbon in a 100 mL round bottom flask by a magnetic stir
bar. After 3 h, the stirring is stopped and the carbon was separated
from the solution by filtration. For kinetic runs, the concentration of
each of the materials is set to 100 ppm only and the run is ceased
after the time intervals of 2 min, 15 min, 30 min, 1 h, 2 h and 3 h. The
concentrations of benzene, toluene and xylene were measured in
UVeVis spectroscopy (Thermo Fisher Genesis UVeVis spectro-
scope). A known linear calibration plot was made for each of the
components and the unknown concentration was measured
against this calibration plot. Each of the analysis was performed
thrice and the average value was reported along with the standard
deviation.
The vapor phase adsorption of BTX was performed gravimetri-
cally in TA instruments' VTI-SA þ automated vapor sorption
analyzer with ultrahigh purity N2 as carrier gas. Typically, a pre-
outgassed activated carbon is inserted in the quartz pan of the in-
strument, whereas the benzene, toluene or xylene is introduced,
each at a time, in the solvent container of the instrument. The
activated carbon is further regenerated within the instrument upto
the temperature of 150  C in nitrogen flow. Then, it is cooled down
to room temperature and exposed to the vapor of each of the
component with controlled relative saturation pressure or hu-
midity (p/p0) by the heating the solvent container. Both adsorption
and desorption of vapors are performed by increasing the relative
saturation pressure from 0.01 to 0.9 and then decreasing it in the
same fashion. Both adsorption equilibrium and kinetics data are
automatically recorded in the instrument by registering the change
in weight of activated carbon. The total time to complete
adsorption-desorption cycle for each of the vapors was in the range
of 10 h.
3. Results and discussions
3.1. Characteristics of lignin derived nanoporous carbons
The N2 adsorption-desorption plot at 77 K is shown in Fig. 1.
According to IUPAC nomenclature, this is type I isotherm with
negligible hysteresis loop. This type of isotherm is the indicator of
primarily microporous structure with negligible mesopore
contribution. (IUPAC classification: micropore, pore width<20 Å;
mesopore: pore width 20e500 Å; macropore: pore width>500 Å).
Fig. 1. Nitrogen adsorption-desorption on lignin-derived activated carbon at 77 K
(closed symbol for adsorption, open symbols for desorption).
374 D. Saha et al. / Journal of Cleaner Production 182 (2018) 372e378

Fig. 2. Pore size distribution of activated carbon obtained from N2 adsorption at 77 K Fig. 4. TGA studies of the activated carbons in N2.
and CO2 adsorption at 273 K.

differential and cumulative pore size distributions are shown in the

The Brunauer-Emmett-Teller (BET) surface area of the carbon is
pore size distribution data. It is observed all the pore widths are
calculated to be 2250 m2/g with total pore volume 1.1 cm3/g. The
narrower than 20 Å and the key pore widths are within the range of
complete range of pore size distribution is obtained by NLDFT
3.5, 4.8, 5.7, 8.2, 15.4 and 18.4 Å.
technique through combining the N2 adsorption isotherm at 77 K
Scanning electron microscopic (SEM) images (Fig. 3) revealed
and CO2 adsorption at 273 K (Saha et al., 2016, 2017c) (Fig. 2). CO2
that the particles are quite irregular in shape and size. The size of
adsorption is used for the pore widths narrower than 14 Å, whereas
the particles varies within 2e100 mm. Such irregular shapes of the
N2 adsorption was used for the pore widths greater than that. Both
particles are common for other activated and porous carbons re-
ported in literature. Thermogravimetric analysis (TGA) revealed
that the carbon is stable in inert (N2) atmosphere in the tempera-
ture upto 400  C and then slowly loose its weight (Fig. 4).

3.2. Liquid and vapor phase adsorption of BTX

The liquid phase adsorption isotherms are shown in Fig. 5. It is

observed that all the isotherms are linear in nature upto the
100 ppm concentration of benzene, toluene or xylene. Such a lin-
early increasing profile and absence of a flat plateau may also be the
indication of micropore filling mechanism and clearly adsorption
would increase more if higher concentration of the components
were used. It is also interesting to note that the adsorption amount
of each of the components is almost similar, where toluene
demonstrated the highest adsorption followed by benzene and

Fig. 3. Scanning electron microscopic (SEM) images of lignin derived activated carbon. Fig. 5. Adsorption isotherms of liquid phase BTX in water in activated carbon.
 D. Saha et al. / Journal of Cleaner Production 182 (2018) 372e378 375

total uptake amount for BTX was 600 mg/g with only marginally
higher toluene uptake compared to the rest of the components. It is
interesting to observe that the vapor phase adsorption uptake of
BTX is over double that of liquid phase adsorption. The underlying
reason may be attributed to the competitive adsorption of BTX with
water and nitrogen in ambient temperature. It is obvious that the
adsorption capacity of liquid phase water in activated type of car-
bon is much higher compared to that of nitrogen at ambient

Fig. 6. Kinetics of liquid-phase BTX adsorption in water.

xylene. Similar adsorption behavior may be associated with the

similar chemical structure or molecular weight and toluene may
have provided the better molecular orientation within the nano-
pores of carbons resulting in slightly elevated uptake.
The kinetics of liquid phase BTX adsorption is shown in Fig. 6. In
the figure, the adsorption amount is normalized with respect to
saturation (maximum) uptake, and hence mt denotes the adsorp-
tion uptake at any time t and m∞ is the saturation uptake. It is
observed that adsorption kinetics is very fast, 80% to over 90% of the
saturation uptake already occurred in less 2 min. Toluene and
xylene demonstrated similar kinetics, each of them completed
about 95% of saturation uptake in 2 min and reached the saturation
uptake in 30 min. Benzene kinetics was only slightly sluggish, it
completed about 82% in 2 min but completed the saturation level in
the same time of 30 min.
The vapor phase equilibrium adsorption of BTX is measured at
different relative pressure or dew point (p/p0) of benzene, toluene
and xylene in the carrier gas (N2). Clearly, the vapor phase
adsorption (Fig. 7) demonstrated a completely different isotherm
behavior compared to liquid phase adsorption. The nature of
adsorption isotherms is similar to type I isotherm according to
IUPAC classification, with a sharp uptake in lower relative pressure
region and then a flat plateau in the higher relative pressure. The

Fig. 8. Kinetics of vapor-phase benzene (a), toluene (b) and xylene (c) adsorption with
Fig. 7. Adsorption isotherms of vapor phase BTX with N2 as carrier gas. N2 as carrier gas.
376 D. Saha et al. / Journal of Cleaner Production 182 (2018) 372e378

Table 1 Freundlich isotherm model is given by

Equilibrium model fitting parameters for vapor-phase BTX adsorption.

Model Parameters Benzene RMSE- Toluene RMSE- Xylene RMSE- 1

Type (B) Benzene (T) Toluene (X) Xylene qe ¼ kCen (3)
Langmuir am 555.55 18.31 588.23 22.40 588.23 29.96
b 257.14 340.0 188.88 where k and n are the model constants and can be calculated by
Freundlich K 581.43 5.81 622.03 4.51 609.35 30.93 linear regression of ln (qe) versus ln (Ce) plot.
n 20.32 26.95 27.70 Sips isotherm model is the combined form of Langmuir and
Sips am’ 1161.38 5.60 1224.58 4.42 599.82 13.44 Freundlich model and given by the equation,
B0 1.01 1.04 469.22
n’ 10.33 12.36 0.075

temperature. Therefore, the less competition in vapor phase

resulted in higher equilibrium uptake of BTX. It is noticeable that
the adsorption and desorption of BTX in vapor phase follows the
similar trend with no visible hysteresis. It also needs to be
mentioned that, in both liquid and vapor phase, there is no sig-
nificant difference between adsorption amounts of benzene,
toluene or xylene. Therefore, current adsorbent cannot be used to
separate those components from each other.
The kinetics of vapor phase BTX adsorption was measured at
the same time of equilibrium adsorption. For convenience, the
normalized kinetics plots are shown for p/p0 values of 0.1, 0.4 and
0.9 for each of the components of benzene, toluene and xylene
(Fig. 8). In the low relative pressure (p/p0) region, kinetic of vapor
phase adsorption appeared to be very fast similar to liquid phase
adsorption; over 90% of saturated adsorption took place in
1e2 min only. However, the kinetics gets significantly sluggish at
the higher relative pressure for benzene and xylene. It is observed
that it took 6e30 min to reach the saturation level for the
normalized kinetics at the p/p0 values 0.9. The sluggish kinetics
may be attributed to the fact that pores of the activated carbons
were partially clogged due the previously adsorbed benzene or
xylene molecules and that provided some hindrance to the
diffusion of the new BTX molecules at the elevated pressure. The
opposite behavior for toluene may be attributed to the surface
diffusion of toluene molecules in the pore space in addition to the
molecular diffusion (Do, 1998).

3.3. Equilibrium and kinetic model fitting

For linear adsorption isotherms, the most obvious isotherm

model is Henry's law model and given as

qe ¼ KCe (1)

where K is the Henry's law constant (mg/g-ppm) and qe is the

equilibrium adsorption amount (mg/g) at the concentration of Ce
(ppm for liquid phase adsorption, no unit (p/p0) for vapor phase
adsorption). For liquid phase adsorption, it can be calculated by the
linear regression of qe versus Ce data, passing thorough the origin.
For the liquid phase adsorption, the values of Henry's constants are
1.64, 2.05, 1.53 mgg1 ppm1, respectively. Corresponding RMSE
values of the fitting are 16.40, 12.46 and 28.25 for benzene, toluene
and xylene, respectively.
For vapor phase adsorption, Langmuir, Freundlich and Sips
isotherm models were also employed. Langmuir isotherm model is
given as

am bCe
qe ¼ (2)
1 þ bCe

where am, b are Langmuir constants and they can be calculated

from the slope and intercepts of linear regression of 1/qe evs-1/Ce Fig. 9. Isotherm model fitting results of vapor-phase benzene (a), toluene (b) and
plot. xylene (c) adsorption.
 D. Saha et al. / Journal of Cleaner Production 182 (2018) 372e378 377

Table 2 The micropore diffusion in an adsorbent material can be

Kinetic model fitting parameters for vapor-phase BTX adsorption. modeled by the following equation (Ruthven, 1984),
Model Type Parameters Relative Benzene Toluene (T) Xylene (X)  2 
pressure (B) mt 6 p Dc t
1 ¼ 2 exp (8)
Pseudofirst k1 (s1)
p/p0 ¼ 0.1 3.68  103 2.30  103 5.53  103 m∞ p rc2
order p/p0 ¼ 0.4 5.30  103 46.1  103 5.76  103
p/p0 ¼ 0.9 13.8  103 6.91  103 2.30  103 where mt and m∞ are mass adsorbed in time t and final adsorption
Pseudosecond k2 (g mg1 p/p0 ¼ 0.1 6.80  102 5.09  102 4.22  102
1 amount, respectively, Dc is intracrystalline diffusivity (m2/s) in
order s ) p/p0 ¼ 0.4 4.72  102 3.42  102 2.42  102
p/p0 ¼ 0.9 1.14  102 1.97  102 0.545  102 micropores and rc is equivalent crystal radius (m). Dc
rc2
(s1) is also
Micropore Dc/r2 (s1) p/p0 ¼ 0.1 3.85  104 2.13  104 3.96  104
referred to as diffusive time constant and it can be calculated by the
diffusion p/p0 ¼ 0.4 3.75  104 2.94  104 5.48  104  
p/p0 ¼ 0.9 1.72  104 7.00  104 2.33  104 linear regression of ln 1  m mt
versus t with the saturation level
∞

higher than 70%. This micropore diffusion model was well fit for
vapor phase adsorption of BTX with the R2 values of 0.9 or higher
1 and the values are given in the last row of Table 1b.
a0m b0 Cen0
qe ¼ 1
(4)
1 þ b0 Cen0 4. Conclusions

where am’, b’ and n’ are Sips constants. These constants are calcu-
lated by employing solver technique in Microsoft Excel. In order to
find the degree of fit, we have utilized root mean square error
(RMSE) given by the formula
sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
Pn  2
i¼1 Xexp;i  Xmodel;i
RMSE ¼
n
where, Xexp and Xmodel are the experimental and model fitting
values of the isotherms, respectively. These isotherm constants and
RMSE values for vapor phase adsorption are given in Table 1. No
attempt was made to fit these models for liquid phase owing to the
linear nature of isotherms. The model fitting results are also shown
in Fig. 9. It is also observed that Freundlich and Sips model are the
better fit compared to Langmuir model for benzene and toluene
vapor, but for xylene, only Sips model fits better.
For adsorption kinetics modeling, the pseudofirst order rate
equation is given by
 
k1
logðqe  qt Þ ¼ log qe  t (6)
2:303
In this phase of research, a high surface area activated carbon
was synthesize by one-step chemical activation of lignin by KOH
with BET specific surface area of 2250 m2/g, total pore volume
1.1 cm3/g and with primarily microporous structure. Equilibrium
and kinetics of liquid and vapor phase adsorption of benzene,
toluene and xylene (BTX) were performed in this carbon. The liquid
(5) phase adsorption was performed in aqueous solution upto the
concentration of 100 ppm, whereas the vapor phase adsorption was
performed in automated VTS-SA þ analyzer with varying relative
saturation and nitrogen as carrier gas. The liquid phase adsorption
behavior demonstrated a linear isotherm with total uptake in the
range of 200 mg/g upto the concentration of 100 ppm in water. The
vapor phase adsorption isotherms were of type-I in nature and
adsorption uptake in the range of 600 mg/g upto the relative
pressure of 0.9. The adsorption kinetics of liquid phase and vapor
phase adsorption in low relative pressure was very fast, however, it
became significantly sluggish in the higher relative pressure of
vapor phase adsorption. The adsorption isotherms of BTX were
successfully modeled by Henry's law, Langmuir, Freundlich and
Sips equations, and kinetics models, including pseudofirst order,
pseudosecond order and micropore diffusion model.

where, qt is the amount adsorbed (mg/g) at time t (sec) k1 is Acknowledgement

pseudofirst order rate constant (s1) and calculated by linear
regression of logðqe  qt Þ versus t plot.
The pseudosecond order rate constant is given by
 
t 1 1 The authors acknowledge Karl Nelson, research engineer of School
¼ 2
þ t
qt k2 qe qe
where, k2 is the pseudosecond order rate constant (gmg1s1) and
can be calculated by linear regression of qtt versus t plot. For liquid
phase adsorption, pseudofirst order rate equation could not be fit,
but pseudosecond order rate mode fits very well with R2 > 0.99. The
pseudosecond rate constants for liquid phase benzene, toluene and
xylene are 2.07  102, 1.16  104, 6.27  105, gmg1s1, respec-
tively. For vapor phase adsorption, pseudofirst order rate constant
fits with moderate accuracy with R2 value ~0.85e0.9. Similar to
liquid phase adsorption, pseudosecond order rate model also fits
very well with R2 > 0.99. Both the rate constants for vapor phase
adsorption are shown in Table 2. It is observed that the numerical
values of diffusive times constants for benzene and xylene were
lowest at the p/p0 values of 0.9 that confirmed their sluggish ki-
netics adsorption as described earlier. The opposing trend of ki-
netics for toluene is also observed in its diffusive time constants
values.
This work was partly supported by Faculty Development Award
and provost grant from Widener University. N.M acknowledges the
Widener University summer research program for partial funding.
(7)
of Engineering of Widener University, for assistance during the
experimentation.
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