Journal of Hazardous Materials 178 (2010) 1132–1136

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Journal of Hazardous Materials

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Short communication

Screening of novel low-cost adsorbents from agricultural residues to remove

ammonia nitrogen from aqueous solution
Haiwei Liu a,b , Yuanhua Dong a,∗ , Yun Liu a , Haiyun Wang a
a
State Key Laboratory of Soil and Sustainable Agriculture, Institute of Soil Science, Chinese Academy of Sciences, 210008 Nanjing, China
b
Graduate University of Chinese Academy of Sciences, 100049 Beijing, China

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

Article history: Most studies on ammonia adsorption from aqueous solution have been focused on mineral materials.
Received 2 August 2009 However, a series of batch experiments were performed in this study to screen novel adsorbent materials
Received in revised form 22 January 2010 from 80 agricultural residues, and to investigate the adsorption characteristics of six screened samples.
Accepted 25 January 2010
The results showed that the ammonia adsorption efficiencies of 11 agricultural residues were comparable
Available online 1 February 2010
to those of minerals. The equilibrium data fitted well with both the Langmuir and Freundlich models,
and the theoretical maximum monolayer adsorption capacities of strawberry leaves and stems, Boston
Keywords:
ivy leaves and stems, southern magnolia leaves and poplar leaves were 6.71, 4.62, 6.07, 5.01, 6.22 and
Adsorption
Ammonium ion
6.25 mg/g, respectively at 30 ◦ C. The adsorptions reached equilibrium at about 18 h, and the kinetics were
Isotherms well described by the Logistic model. In conclusion, these agricultural residues could be used as adsorbent
Kinetics materials for ammonia removal.
Plant material © 2010 Elsevier B.V. All rights reserved.

1. Introduction This study evaluated the adsorption of ammonia from aqueous

Excess ammonia nitrogen discharged into waterways can con-
tribute to the eutrophication of water bodies, depletion of dissolved
oxygen and toxicity to fish and other aquatic organisms. The
traditional processes of ammonia removal from wastewater are
biological nitrification–denitrification, air stripping and chemical
precipitation. However, latterly, great efforts have been made to
identify new economically feasible and environmentally friendly
treatment alternatives, of which adsorption and ion exchange have
received significant attention.
Recently, there has been increased interest in finding effective
and low-cost adsorbents or ion exchangers from nature. One mate-
rial proved to have a high affinity for ammonium ions is natural
zeolite, including clinoptilolite and mordenite [1–4]. Limestone and
volcanic tuff have also been reported to efficiently adsorb ammo-
nia from wastewater [5,6]. Agricultural residues or plant materials
are another type of low-cost material of interest and have been
studied extensively as adsorbents to remove a variety of pollutants
from aqueous solution, e.g. heavy metal [7], dyes [8], nitrate [9],
phosphate [10] and phenol [11]. However, there is little informa-
tion available in the literature on the development of agricultural
residues or plant materials as adsorbents for the removal of ammo-
nia from aqueous solution.
solution using 80 agricultural residues collected from local fields.
These agricultural residues were by-products or wastes from farm-
land, and may be good low-cost candidates for the adsorption of
ammonia. The main purpose of this paper was to screen ammo-
nia adsorbents from these agricultural residues. The isotherms and
kinetics of adsorption of six screened samples were also investi-
gated to obtain an insight into the equilibrium characteristics of
ammonia adsorption by agricultural residues.
2. Materials and methods
2.1. Preparation of the adsorbents
A total of 80 agricultural residues (Table 1 and Supplementary
Material) were collected from farmlands in Nanjing, China. The
samples were washed repeatedly with water to remove dust and
soluble impurities and were allowed to dry at room temperature
in the shade. The samples were then dried at 105 ◦ C for 15 min and
at 70 ◦ C for 10 h in an air oven. The dried samples were ground and
sieved through a 30-mesh sieve. The fine powders of these agricul-
tural residues were preserved in plastic bags for use as adsorbents.
2.2. Screening experiments

The screening experiments were performed according to the

∗ Corresponding author. Tel.: +86 25 86881317; fax: +86 25 86881000. batch method. In this method, 0.2 g of each sample was mixed with
E-mail address: yhdong@issas.ac.cn (Y. Dong). 25 mL ammonia solution at 25 or 50 mg N/L. The mixtures were

0304-3894/$ – see front matter © 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.jhazmat.2010.01.117
 H. Liu et al. / Journal of Hazardous Materials 178 (2010) 1132–1136 1133

Table 1
The removal rates and adsorption capacities (q) of ammonia nitrogen by 11 samples.

Plant Biomass 25 mg/L 50 mg/L

Removal rate (%) q (mg/g) Removal rate (%) q (mg/g)

Boston ivy (Parthenocissus tricuspidata Planch) Leaves 100.00 3.13 52.71 3.29
Stems 72.56 2.27 38.12 2.38

Phoenix tree (Platanus orientalis L.) Leaves 100.00 3.13 58.56 3.66
Sunflower (Helianthus annuus L.) Stems 93.15 2.91 48.91 3.06
Southern magnolia (Magnolia grandiflora L.) Leaves 85.81 2.68 44.37 2.77
Loquat (Eriobotrya Japonica Lindl.) Leaves 84.67 2.65 43.24 2.70
Poplar (Populus euramevicana cv. ‘I-214’) Leaves 82.21 2.57 42.00 2.63
Green pepper (Capsicum annuum L. var. grossum Sendt.) Leaves 74.39 2.32 40.39 2.52
Sweet Wormwood Herb (Artemisia annua L.) Stems 64.24 2.01 40.36 2.52

Strawberry (Fragaia ananassa Duchesne) Leaves 60.45 1.89 37.65 2.35

Stems 66.51 2.08 37.93 2.37

sealed and shaken at 250 rpm and 30 ◦ C for 24 h to reach equilib-
rium. The mixtures were then centrifuged at 4000 rpm for 5 min,
and the upper solutions were filtered using 0.45 ␮m microporous
membrane filters, respectively. The concentration of ammonia in
each filtrate was analyzed using the titrimetric method [12]. Exper-
iments were performed in triplicate and the results averaged.
Controls were obtained by mixing distilled water with each sample.
2.3. Equilibrium experiments
the removal rates in 11 samples were more than 60% at 25 mg/L
(Table 1). Furthermore, the removal rates of Boston ivy leaves
and phoenix tree leaves were 100%, and the adsorption capacities
were 3.13 mg/g, accordingly. The adsorption capacities of these 11
samples at 50 mg/L were little more than those at 25 mg/L. The con-
siderable adsorption capacities of the samples (Table 1) were close
to those of mineral materials [2]. These findings suggested that the
agricultural residues which had good adsorption of ammonia could
potentially be used as adsorbents.

Six agricultural residues were selected to study the equilibrium
characteristics of ammonia adsorption. These residues were straw-
berry leaves and stems, Boston ivy leaves and stems, southern
magnolia leaves and poplar leaves. The equilibrium experiments
were also carried out using the batch method. To assess the
effects of initial ammonia concentration, a concentration range
of 25–1000 mg/L was used. To assess the effects of contact time,
kinetic studies were carried out where the samples were shaken
from 1 h to 24 h, and the initial ammonia nitrogen concentrations
were 25 mg/L.
The ammonia removal rate (%) and adsorption capacity (mg/g)
were calculated by:
C0 − Ce
Removal rate (%) = × 100
C0
(C0 − Ce )V
q=
M
where q (mg/g) is the ammonia adsorption capacity, C0 (mg N/L)
and Ce (mg N/L) are respectively the initial and equilibrium ammo-
nia nitrogen concentrations in the solution, V (L) is the solution
volume, and M (g) is the mass of adsorbent.
3. Results and discussion
3.1. Screening results
The removal rates and adsorption capacities of 80 agricul-
tural residues were calculated, and are listed in Table 1 and
Supplementary Material. Most of the samples did not show effi-
cient adsorption of ammonia nitrogen, as the ammonia removal
rates of 61 samples were less than 50% at 25 mg NH4 + N/L. More-
over, the ammonia removal rates in eight samples were negative,
probably because the ammonia adsorbed from solution was less
than the ammonia released in these samples. The control experi-
ments also showed there were another 20 samples which might
release ammonia nitrogen into aqueous solution. The removal
rates in these 28 samples were less than 27%, and the residues
were thus considered unsuitable as ammonia adsorbents. However,
3.2. Chemistry and physical properties of the adsorbents
The chemical and physical properties of the six screened sam-
ples are listed in Table 2. Like other natural plant materials, they
were composed of cellulose, hemicellulose, lignin and protein as
the major constituents, and may contain polar functional groups,
such as alcohols, aldehydes, ketones, carboxyl, phenol and ether
groups. These groups have the ability to bind pollutants to some
extent [13]. The -potential of each sample at its natural pH was
negative and smaller than −24 mV, suggesting that the electro-
static attraction between the adsorbent surface and ammonium
ions might relate to the adsorption [14]. The -potential and total
negative charge of the sample is mainly dependent on the amount
of polar functional groups (such as –COOH and –OH) attached onto
(1)
the sample surface [14,15]. The low value of surface area indicated
low porosity [16]. The ion adsorption capacity usually increased
(2) with the increase of porosity of adsorbent, probably because the
number of available binding sites increased [5,8,16]. This would
need to be proved in future work.
3.3. Effect of initial ammonia concentrations
The ammonia adsorption capacities of the six adsorbents
increased with increasing initial ammonia concentration in solu-
tion (Fig. 1). This might be due to the high probability of collision
between ammonium ions in solution and the adsorbent surface at
high ammonia concentrations. As shown in Fig. 1, the isotherms
can be characterized by the typical L-curve isotherm. The Lang-
muir and Freundlich adsorption models are commonly used to fit
experimental data.
The Langmuir model usually describes monolayer adsorp-
tion and adsorption occurring on a structurally homogeneous
adsorbent. The linearized form of the Langmuir isotherm can be
expressed as:
Ce 1 1
= + Ce (3)
q bqm qm
where qm (mg/g) indicates the maximum monolayer adsorption
capacity of the adsorbent, and b (L/mg) is the Langmuir constant.
1134 H. Liu et al. / Journal of Hazardous Materials 178 (2010) 1132–1136

Table 2
Chemical and physical properties of six samples.

Strawberry leaves Strawberry stems Boston ivy leaves Boston ivy stems Southern magnolia leaves Poplar leaves

Holocellulose (%) 59.7 71.5 66.3 66.4 67.8 56.3

Lignin (%) 15.7 13.2 13.0 20.2 18.4 13.1
Protein (%) 17.7 8.2 9.6 6.1 4.1 18.1
Moisture (%) 9.4 10.2 8.1 7.1 6.8 7.1
pH 5.8 6.0 5.5 5.4 6.0 5.6
␨-Potential (mV) −30.0 −32.4 −27.4 −30.5 −32.3 −24.4
BET surface area (m2 /g) 0.35 0.10 31.96 0.53 1.54 –

Table 4
Maximum ammonia adsorption capabilities (qm ) of natural mineral materials from
Langmuir model in references.

Materials qm (mg N/g) Temperature (◦ C) Reference

Mordenite 8.28 21 [1]

Clinoptilolite 5.74 21 [1]

Clinoptilolite 6.32 25 [2]
Clinoptilolite 4.78 40 [2]
Clinoptilolite 4.02 55 [2]

Zeolite 8.91 25 [18]

Zeolite 7.50 21 [19]
Zeolite 4.49 30 [20]
Zeolite 8.71 25 [21]
Zeolite 5.22 30 [22]

these adsorbents was a mixture of monolayer adsorption and mul-

Fig. 1. Effect of initial concentrations on ammonia adsorption.
The essential features of the Langmuir isotherm can be
expressed in terms of the dimensionless constant separation factor
RL , as:
1 would need to be confirmed by thermodynamics in the future.
RL =
1 + bC0
There are four probabilities for the RL value: for favorable
adsorption, 0 < RL < 1; for unfavorable adsorption, RL > 1; for linear
adsorption, RL = 1; for irreversible adsorption, RL = 0 [8].
The Freundlich model was derived to describe multilayer
adsorption and the adsorption on heterogeneous surfaces. The lin-
earized form of the Freundlich model is represented by:
1
ln q = ln K + ln Ce
n Additionally, Fig. 2 shows the variation in the separation fac-
where K (mg/g) is the Freundlich constant and n (dimensionless) is
the Freundlich exponent related to adsorption intensity.
The parameters of the two models were calculated by the inter-
cepts and slopes, and are listed in Table 3. All the equilibrium data
of these six samples fitted well to both the Langmuir and the Fre-
undlich model (R2 > 0.86), of which the Langmuir model was best
(R2 > 0.98). These results suggested that ammonia adsorption onto
tilayer adsorption, as a result of the real heterogeneous nature of
the surface sites involved in ammonia adsorption. Chemisorption
is by its very nature limited to less than monolayer coverage of the
surface, whereas in physical adsorption, multilayer adsorption is
common [17]. Therefore, the adsorption of ammonia by these six
agricultural residues might be due to physisorption. However, this
(4)
The qm values from the Langmuir model could infer the poten-
tial maximum monolayer adsorption capacities of the adsorbents,
which were 6.71, 4.62, 6.07, 5.01, 6.22 and 6.25 mg/g for strawberry
leaves and stems, Boston ivy leaves and stems, southern magnolia
leaves and poplar leaves, respectively. These values were compared
with the qm values of mineral adsorbents to remove ammonia nitro-
gen in the literature, and are shown in Table 4. The qm values of the
adsorbents used in this study were comparable to those of natural
(5) mineral materials.
tor (RL ) with initial ammonia concentration. It can be seen that
the RL values were in the range of 0–1, indicating that the adsorp-

Table 3
Parameters of Langmuir and Freundlich adsorption isotherms.

Materials Langmuir model Freundlich model

qmax b (L/mg) R2 K (mg/g) n R2

(mg/g)

Strawberry 6.71 0.0117 0.985 0.938 3.63 0.990

leaves
Strawberry stems 4.62 0.0166 0.983 1.182 5.30 0.960

Boston ivy leaves 6.07 0.0208 0.995 2.006 6.44 0.994

Boston ivy stems 5.01 0.0174 0.993 1.260 5.25 0.949

Southern 6.22 0.0179 0.992 1.776 5.97 0.869

magnolia leaves
Poplar leaves 6.25 0.0172 0.992 1.650 5.56 0.890 Fig. 2. Variation in separation factors (RL ) with different initial ammonia concen-
trations.
 H. Liu et al. / Journal of Hazardous Materials 178 (2010) 1132–1136 1135

Table 5
Parameters of Logistic model and correlation coefficient (R2 ) of three classic kinetic models in fitting the ammonia adsorption.

Materials Logistic model Pseudo-first-order Pseudo-second-order Intraparticle

diffusion

q0 (mg/g) q1 (mg/g) t1 (h) p R2

Strawberry leaves 0.072 1.888 11.10 7.17 0.993 0.834 0.396 0.865
Strawberry stems 0.091 2.043 13.81 38.32 0.991 0.668 0.353 0.696

Boston ivy leaves 0.241 3.17 10.03 7.82 0.987 0.756 0.312 0.838
Boston ivy stems 0.280 1.935 13.70 12.36 0.981 0.680 0.258 0.795

Southern magnolia leaves 0.336 2.459 15.26 29.48 0.988 0.589 0.266 0.696
Poplar leaves 0.199 2.578 11.26 10.63 0.995 0.827 0.289 0.811

tion of ammonia by the adsorbents was favorable. The RL values
approached zero with increased C0 which confirmed that the
adsorption of ammonia on the adsorbents was more favorable at
high initial ammonia concentrations than at low concentrations [8].
These findings confirmed that these agricultural residues could be
used to adsorb ammonia from aqueous solution. It can also be seen
from Table 3 that the n values from the Freundlich model were
more than 1, which also showed favorable removal conditions [4].
This is a most common result and may be due to the distribution of
surface sites or factors which could cause a decrease in the inter-
action between the adsorbent and the adsorbate with increasing
surface density [23].
3.4. Kinetics of ammonia adsorption
The plots of the ammonia adsorption capacities of the adsor-
bents with time were dramatic S-curves (Fig. 3). It seems that the
ammonia adsorption process occurred in three steps. Ammonia
adsorption occurred slowly and steadily in the first stage. The time
periods for the first stage were different in the six samples, and
ranged from 6 h to 14 h. Adsorption mostly occurred in the middle
6 h, when the adsorption capacities increased sharply. The adsorp-
tion process finally reached equilibrium at 18 h, which might be
due to saturation of the efficient active sites.
As shown in Table 5, three classic kinetic models, pseudo-first-
order [24], pseudo-second-order [25] and intraparticle diffusion
equation [26], did not describe the kinetic data sufficiently
(R2 < 0.84, R2 < 0.40 and R2 < 0.87 for the three models, respectively).
These results can be attributed to the complex nature of ammo-
nia adsorption by these samples. The curves in Fig. 3 were S-type,
therefore the Logistic model (Eq. (6)) was also used to describe the
curves and the calculated parameters are presented in Table 5
q0 − q1
qt = q1 + p (6)
1 + (t/t1)
Fig. 3. Effect of time on ammonia adsorption.
The Logistic model is usually used to describe growth or dif-
fusion with a limiting factor. The good fit of the adsorption data
with this model (R2 > 0.98) implied that ammonia adsorption using
these six adsorbents might be limited, probably by the number of
efficient active sites. The q1 (mg/g) is the theoretical ammonia car-
rying capacity which might relate to the number of efficient active
sites. The t1 (h) is the time when the adsorption capacity was half
the value of q0 + q1 . The p is the temperature constant. The q0 (mg/g)
presents initial adsorption capacity, which might be achieved in a
very short contact time.
Unlike the adsorbents in this study, most kinetic data on
ammonia adsorption by zeolite and limestone fitted well with the
pseudo-second-order equation [2,4,5]. The process of ammonia
adsorption by zeolite and limestone also has three stages, however,
the first and second stages seemed to be one stage as the rates of
both were rapid [3]. These studies also suggested that the first lin-
ear portion was attributed to the boundary layer diffusion effect
and the final linear portions may be due to the intraparticle diffu-
sion effect [2]. The boundary layer diffusion in the adsorption of
ammonia by the six agricultural residues in this study were much
slower than those by mineral materials, thus the kinetic curves
of ammonia adsorption in these six samples were S-type rather
than L-type shown by the mineral materials. The different rates of
boundary layer diffusion might be due to the different adsorption
mechanisms of ammonia nitrogen between the mineral materials
and the agricultural residues. These differences in mechanism may
be the result of the differences in structure, compositions and other
characteristics between the agricultural residues and the mineral
materials.
4. Conclusions
New low-cost adsorbents were screened from 80 agricultural
residues to remove ammonia nitrogen from aqueous solution, and
the removal rates of 11 samples were more than 60% at 25 mg/L.
The characteristics of six screened samples suggested that they had
a porous structure mostly formed by holocellulose, lignin and pro-
tein, and were suitable candidate ammonia adsorbent materials.
Furthermore, the electrostatic attraction between the adsorbent
surface and ammonium ions might relate to this adsorption. Both
the Langmuir and Freundlich models fitted the equilibrium data of
the six screened samples well, suggesting that ammonia adsorption
might be due to physisorption. The maximum monolayer adsorp-
tion capacities calculated from the Langmuir model for strawberry
leaves and stems, Boston ivy leaves and stems, southern magno-
lia leaves and poplar leaves were 6.71, 4.62, 6.07, 5.01, 6.22 and
6.25 mg/g, respectively, which were comparable to those of min-
eral materials in the literature. Moreover, RL and n values from the
Langmuir and Freundlich models inferred that ammonia adsorption
was favorable. Ammonia adsorption reached equilibrium at about
18 h, and the adsorption process was well described by the Logis-
tic model rather than pseudo-first-order, pseudo-second-order or
intraparticle diffusion equation. Because agricultural residues are
1136 H. Liu et al. / Journal of Hazardous Materials 178 (2010) 1132–1136
a reproducible resource and a type of waste, which have a low-cost
or possibly no economic value, their cost in environmental waste
treatment would be an advantage.
Acknowledgements
We express sincere gratitude to the National Supporting Plan
of Science and Technology (2006BAD10B05), the National Natural
Science Foundation of China (20907058) and the Natural Science
Foundation of Jiangsu Province of China (BK2008499) for the finan-
cial support in this research.
Appendix A. Supplementary data
Supplementary data associated with this article can be found, in
the online version, at doi:10.1016/j.jhazmat.2010.01.117.
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