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JTICE-397; No. of Pages 6

Journal of the Taiwan Institute of Chemical Engineers xxx (2011) xxx–xxx

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Journal of the Taiwan Institute of Chemical Engineers

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Zeolite 13X for adsorption of ammonium ions from aqueous solutions and hen
slaughterhouse wastewaters
Ayla Arslan *, Sevil Veli 1
Department of Environmental Engineering, Faculty of Engineering, Kocaeli University, 41380 Kocaeli, Turkey

A R T I C L E I N F O A B S T R A C T

Article history: In this study adsorption efficiencies of various zeolites were tested for removal of ammonium ions from
Received 18 May 2011 aqueous solutions. In the experiments performed with different initial ammonium concentrations,
Received in revised form 1 November 2011 highest removal was obtained for Zeolite 13X so forthcoming studies were carried out with this zeolite
Accepted 5 November 2011
type. The effects of initial NH4+ ion concentration, zeolite amount, pH and agitation time on adsorption
Available online xxx
efficiency were investigated with batch experiments. Langmuir, Freundlich and Dubinin–Radushkevich
(D–R) models were applied to experimental data and calculated correlation coefficients were
Keywords:
determined as 0.54, 0.93 and 0.89 for the models, respectively. Main energy of adsorption (E),
Ammonium removal
Zeolite
calculated as 0.542 kJ/mol, demonstrated physical characteristics of adsorption process. Optimal
Adsorption kinetics conditions determined for aqueous solutions were used also for hen slaughterhouse wastewaters. In
Hen slaughterhouse wastewater kinetic calculations it was obtained that pseudo-second order reaction kinetic model was well-fitted for
both synthetic solution and wastewater.
ß 2011 Published by Elsevier B.V. on behalf of Taiwan Institute of Chemical Engineers.

1. Introduction Slaughterhouse wastewaters contain high-strength organic

Nitrate and ammonium ions are among the most common N
compounds encountered in wastewater and groundwater. There
are several different methods for removing ammonium ions from
wastewaters: air stripping, chemical treatment, selective ion
exchange, adsorption and biological nitrification–denitrification
[1]. The application of zeolite as an ion exchanger is one of the most
effective technologies used for ammonium removal in recent
years. Zeolites are aluminosilicate minerals containing exchange-
able alkali or alkaline-earth metal cations (normally Na+, K+, Ca++
and Mg++) in addition to water in their structural framework. Their
physical structure is porous containing interconnected cavities
within metal ions and water molecules [2].
Natural and modified zeolites are evaluated as significant
potential adsorbents for removal of ammonium [3–11], and heavy
metals [12–14]. Karapınar [10], reported that zeolite can be used as
an adsorbent for the removal of ammonium and phosphorus from
the wastewaters, and ammonium uptake of zeolite was completed
within initial 5 min of adsorption period.
carbon (C), nitrogen (N) and phosphorus (P). Due to the strict
discharge standards, an efficient N removal from slaughterhouse
wastewaters is required. Despite the effectiveness of conventional
pre-denitrification activated sludge processes, they require a high
internal recycle ratio (up to 10) that may result in high operational
costs [15].
In this study, removal of ammonium ions from aqueous
solutions was investigated by choosing the zeolite type which
may provide highest removal efficiency. The effects of factors such
as pH, zeolite amount, NH4+ ion concentration and agitation time
were examined in order to obtain optimum conditions. Adsorption
isotherms were applied and adsorption constants were calculated
in order to determine the interaction between ammonium ions and
zeolite. The results obtained with aqueous solutions were applied
to the hen slaughterhouse wastewaters. Furthermore, first- and
second-order reaction kinetics were calculated for determination
of adsorption mechanisms.
2. Materials and methods

2.1. Instrumentation

* Corresponding author. Tel.: +90 262 3033195; fax: +90 262 3033003.
NUVE model shaker was used in all adsorption experiments and
E-mail addresses: ataberk@kocaeli.edu.tr (A. Arslan), sevilv@kocaeli.edu.tr
(S. Veli).
pH adjustments were performed in TESTO model pH-meter.
1
Tel.: +90 262 3033191; fax: +90 262 3033003. Ammonium analyses were conducted according to the distillation-

1876-1070/$ – see front matter ß 2011 Published by Elsevier B.V. on behalf of Taiwan Institute of Chemical Engineers.
doi:10.1016/j.jtice.2011.11.003

Please cite this article in press as: Arslan, A., Veli, S., Zeolite 13X for adsorption of ammonium ions from aqueous solutions and hen
slaughterhouse wastewaters. J. Taiwan Inst. Chem. Eng. (2011), doi:10.1016/j.jtice.2011.11.003
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2 A. Arslan, S. Veli / Journal of the Taiwan Institute of Chemical Engineers xxx (2011) xxx–xxx

Zeolite 13X is (Na86[(AlO2)86(SiO2)106]xH2O with 2 mm particle

Nomenclature
size and Zeolite 4A (Na15[(AlO2)12(SiO2)12]xH2O, with 5 mm
particle size.
Ce concentration of NH4+ ion at equilibrium [mg/L]
Co initial NH4+ ion concentration [mg/L]
3. Results and discussion
E main energy of adsorption [kJ/mol]
k equilibrium constant Optimum experimental conditions were first examined for
k1 rate constant of pseudo-first-order adsorption ammonium ion removal by using synthetic solution in order to
kinetic [1/min] choose the zeolite type, which gives the best ammonium removal
k2 rate constant of pseudo-second-order adsorption efficiency out of 4 different zeolites. In Fig. 1 ammonium removal
kinetic [g/mg min] efficiencies were presented.
Kf Freundlich isotherm constant [mg/g] As shown in Fig. 1, the highest removal efficiency for various
K0 adsorption energy constant [mol2 kJ2] initial ammonium ion concentrations were obtained with Zeolite
m adsorbent weight [mg] 13X. 90% removal efficiency was achieved with the initial
ammonium ion concentration of 25 mg/L. Therefore, the study
R2 correlation coefficient
was continued with the initial concentration of 25 mg NH4+/L and
R gas constant [kJ/K mol]
Zeolite 13X. As it is expected, Zeolite 13X provided the highest
T0 temperature [K]
t time [min]
V solution volume [L]
Vm monolayer capacity
V 0m D–R adsorption capacity [mg/g]
1/n heterogeneity factor
e Polanyi potential
qe amount of adsorbed NH4+ ion per unit zeolite mass
[mg/g]
qt the amount of NH4+ ion adsorbed at time t [mg/g]

titration method using Behr S3 automatic steam distillation

apparatus.

2.2. Experimental methodology Fig. 1. Removal efficiencies of zeolite types (zeolite dosage 0.5 g/100 ml, agitation
time 360 min, temperature 23 8C).
1000 mg/L of NH4+ stock solution was prepared by dissolving
1.486 g of ammonium chloride (NH4Cl) in 1 L distilled water.
100 mL volume samples in different concentrations of NH4+ in the
range of 10–100 mg/L were prepared by stepwise dilution of the
stock solution. Adsorption experiments were carried out by using
four different zeolite types in 150 rpm stirring rate and 23 8C
temperature. 0.5 g of zeolite was mixed with 100 mL ammonium
solutions of concentrations ranging from 10 to 100 mg/L. The
suspension was shaken for 360 min. Afterwards remaining
ammonium concentration was determined by steam distillation
apparatus. The amount of exchanged NH4+ ion qe (mg/g) by zeolite
was calculated using Eq. (1):

ðC o  C e ÞV
qe ¼ (1)
m
where Co is the initial NH4+ ion concentration (mg/L), Ce is the
concentration of NH4+ ion at equilibrium (mg/L), m is the adsorbent
weight (g) and V is the solution volume (L).
Adsorption studies were also performed for hen slaughterhouse
wastewater after the determination of optimum experimental
conditions. Characteristics of the studied wastewater are given in
Section 3.6.

2.3. Adsorbents

Experimental studies were carried out using four zeolite

samples which are Aqua-Multalite (Z1), Zeolit of Gördes-Manisa
(Z2), Zeolite 13X (Z3) and Zeolite 4A(Z4).
The chemical formula of Zeolite Aqua-Multalite is (Na,K)6[(A-
lO2)6(SiO2)30]x24H2O with 75 mm particle size, Gördes-Manisa is
(Ca,K2,Na2,Mg)4Al8Si40O96  24H2O with 65 mm particle size, Fig. 2. The SEM image of the Zeolite 13X. (a) Scala: 1000 and (b) scala: 5000.

Please cite this article in press as: Arslan, A., Veli, S., Zeolite 13X for adsorption of ammonium ions from aqueous solutions and hen
slaughterhouse wastewaters. J. Taiwan Inst. Chem. Eng. (2011), doi:10.1016/j.jtice.2011.11.003
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Fig. 3. Effect of zeolite amount on the removal efficiency (initial NH4+ concentration Fig. 4. Effect of pH on removal efficiency of NH4+ ions (initial NH4+ concentration
25 mg/L, agitation time 360 min, temperature 23 8C). 25 mg/L, zeolite dosage 0.5 g/100 mL, agitation time 360 min, temperature 23 8C).

removal efficiency due to a larger surface area and excess of cations
in the structure.
The SEM image of the Zeolite 13X is shown in Fig. 2. As seen
from Fig. 2(a), particles are arbitrarily distributed in agglomerated
fashion. Dimensions of zeolite particles are approximately 1–
4 mm. Particles are not always spheric, but may be edged and
polygonal (Fig. 2(b)).
3.1. Effect of adsorbent amount
The effect of adsorbent amount was investigated with 25 mg
NH4/L initial ammonium concentration and using 0.1–0.9 g Zeolite
13X. Fig. 3 shows the effect of zeolite amount on the removal
efficiency of ammonium ions.
According to Fig. 3, the minimum amount of zeolite to achieve
the best ammonium removal efficiency is 0.5 g.
The adsorption capacity of NH4+ ions is given in Table 1.
3.2. Effect of pH
3.4. Adsorption isotherms
Adsorption continues until equilibrium occurs between con-
centrations of the matter accumulated on the surface of adsorbent
and remaining matter in solution [16]. The adsorption isotherms
were determined with aqueous NH4+ solution (Fig. 6).
The curve in Fig. 6 is valid for adsorption isotherms in which
capillary condensation is less and the heat of adsorption is more
than that of condensation. Equilibrium concentration of the
isotherm is encountered at the mono-layer adsorption for Ce = 4,
and at the multi-layer adsorption and capillary condensation after
Ce = 4. In case of Ce = 6, adsorption has been completed due to the
filling of the pores and finally qe versus Ce value reaches vertical
point. The adsorption isotherm given in Fig. 6 was explained
mathematically by Freundlich, Langmuir and Dubinin–Radushke-
vich (D–R) isotherm equations.
Freundlich isotherm is used for modeling the adsorption on
heterogeneous surfaces [17]. It is expressed mathematically as
follows:

The removal of NH4+ ions from aqueous solutions by Zeolite 13X 1

log qe ¼ log K f þ log C e (3)
was studied under different pH in the range of 4–12 (Fig. 4). The n
maximum removal efficiencies of ammonium ions were achieved where Kf is Freundlich constant (mg/g), the measure of the
between pH 6 and 8, and the optimal value of pH was 7. NH4+ adsorption capacity of the adsorbent, and 1/n is the heterogeneity
removal efficiency was decreased above pH 8 due to the reaction of factor, a constant relating to adsorption intensity or surface
NH4+ ions with OH ions at higher pH values according to Eq. (2): heterogeneity.
Linear pilot of Freundlich isotherm of NH4+ ion adsorption on
NH4 þ þ OH $ NH3 H2 O $ NH3 þ H2 O (2) zeolite was shown in Fig. 7.
Eq. (4) explains the linear form of the Freundlich isotherm for
Also, NH4+ ions are reported to be converted to the NH3 ions the study:
above pH 9 [1].
qe ¼ 1:226 Ce1:374 ðR2 ¼ 0:93Þ (4)
3.3. Effect of agitation time
Langmuir isotherm is used for explaining monolayer homoge-
The effect of agitation time on removal efficiency was analyzed neous adsorption processes and it can be represented with the
in a batch system using previously determined optimum following equation:
experimental conditions (pH, zeolite type and amount, initial Ce 1 Ce
ammonium ion concentration). The samples were taken at ¼ þ (5)
qe kV m V m
different time periods varying between 5 and 240 min, and the
remaining ammonium ion concentrations were determined. The where qe represents the mass of adsorbate adsorbed per unit mass
optimum time is 30 min for NH4+ ions adsorption as shown in of adsorbent (mg/g), Vm is the monolayer capacity, k is the
Fig. 5. equilibrium constant and Ce is the equilibrium concentration of the

Table 1
The adsorption capacity of NH4+ ions.

Amount of Zeolite 13X (g) 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9

qe (mg/g) 17.36 9.10 6.62 5.04 4.20 3.50 3.00 2.62 2.30

Please cite this article in press as: Arslan, A., Veli, S., Zeolite 13X for adsorption of ammonium ions from aqueous solutions and hen
slaughterhouse wastewaters. J. Taiwan Inst. Chem. Eng. (2011), doi:10.1016/j.jtice.2011.11.003
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Fig. 5. Effect of agitation time on removal efficiency of NH4+ ions (initial NH4+
concentration 25 mg/L, zeolite dosage 0.5 g/100 mL, pH 7, temperature 23 8C).
Fig. 6. The relationship between adsorbed amount and solution equilibrium
concentration.
solution (mg/L). k and Vm were determined from the slope,
intercept of the Langmuir plot (Fig. 8)
For this study Langmuir isotherm can be expressed as below:
Ce
¼ 0:0495 C e þ 0:7066
qe
The adsorption equilibrium data were also tested for another
isotherm model, Dubinin–Radushkevich (D–R). The D–R equation
has the following linear form [17]:
ln qe ¼ ln V 0 m  K 0 e2
where qe is the ammonium ion amount that is removed per unit
zeolite mass (mg/g), V 0m is the D–R sorption capacity (mg/g), K0 is
the constant related to the adsorption energy (mol2 kJ2) and e is the
Polanyi potential.
According to Eq. (8), the Polanyi potansiyeli (e) can be given as:
e ¼ RT 0 lnð1 þ 1=C e Þ
Fig. 7. Linear plot of Freundlich isotherm of NH4+ ion adsorption on zeolite.
Please cite this article in press as: Arslan, A., Veli, S., Zeolite 13X for adsorption of ammonium ions from aqueous solutions and hen
slaughterhouse wastewaters. J. Taiwan Inst. Chem. Eng. (2011), doi:10.1016/j.jtice.2011.11.003
Fig. 8. Linear plot of Langmuir isotherm of NH4+ ion adsorption on zeolite.
where R is the gas constant (kJ/K mol) and T0 is the temperature (K).
The main energy of adsorption E (kJ/mol) is calculated using the
following formula:
0:5
E ¼ ð2K 0 Þ (9)
where E gives information about the physical and chemical
features of adsorption.
A plot of qe against e2 is given in Fig. 9.
D–R isotherm parameters were calculated from the slope of
curve in Fig. 8 and determined as: K0 = 1.7019 mol2 kJ2;
E = 0.542 kJ/mol; Vm0 = 15.80 mg/g (R2 = 0.89). Low value of mean
energy of adsorption demonstrated that adsorption process
exhibited physical characteristics [17].
According to the evaluated models, Langmuir isotherm does not
explain this adsorption process whereas Freundlich and D–R
models do.
3.5. Kinetic studies for aqueous solution
(6) Kinetic experiments were carried out using various NH4+
concentrations (15, 25, 30 mg/L) and optimum experimental
conditions (0.5 g/100 ml Zeolite 13X, pH 7). Samples were taken
at different time intervals and remaining NH4+ ion concentrations
were analyzed. Plots of NH4+ ion concentrations versus time were
presented in Fig. 10 for synthetic solution.
(7)
Rate constants of pseudo-first and -second order kinetics were
calculated from experimental data.
3.5.1. Pseudo-first order reaction kinetic
A simple linear equation for pseudo-first order reaction kinetics
is given below [18]:
(8) lnðqe  qt Þ ¼ lnqe  k1 t (10)
Fig. 9. Linear plot of D–R isotherm of NH4+ ion adsorption on zeolite.
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Fig. 10. Kinetics of NH4+ ion uptake by zeolite in synthetic solution.

Fig. 12. Pseudo-second order reaction kinetics for the adsorption of NH4+ ion on
zeolite from synthetic solution.

Fig. 11. Pseudo-first order reaction kinetics for the adsorption of NH4+ ion on zeolite
from synthetic solution. Fig. 13. Kinetics of NH4+ ion uptake by zeolite in wastewater.

where k1 is the rate constant of the first order adsorption, qt is the
amount of NH4+ ion adsorbed at time ‘t’ (mg/g) and qe is the amount
of NH4+ ion adsorbed at saturation (mg/g). Plot of ln(qe  qt) versus
t allows calculation of the rate constant k1 and qe for NH4+ ion
removal (Fig. 11).
Calculated pseudo-first order reaction parameters for aqueous
NH4+ solution is given in Table 2.
3.5.2. Pseudo-second order reaction kinetic
A pseudo-second order reaction kinetic can be expressed as
[18]:
t 1 t
¼ þ
qt k2 qe 2 qe
where k2 (g/mg h) is the pseudo-second order rate constant, qe the
amount adsorbed at equilibrium and qt is the amount of NH4+ ion
adsorbed at time ‘t’.
The kinetic plots of (t/qt) versus t for NH4+ ion removal at
different initial concentrations are presented in Fig. 12 for
synthetic solution. Considering kinetic parameters it was seen
that pseudo-second order kinetics explained NH4+ ion adsorption
better (Table 2).
3.6. Application to Hen slaughterhouse wastewater
Reaction kinetics was applied to hen slaughterhouse waste-
waters. Characteristics of this wastewater was; pH 7.69, NH4+ ion
concentration: 122 mg/L, SS:1523 mg/L and COD: 7020 mg/L.
Reqiured dilutions were prepared NH4+ solutions of 10, 15,
25 mg/L concentrations. Fig. 13 shows the obtained results.
Different removal efficiencies determined for aqueous solution
and raw wastewater can be explained with the presence of other
(11) cations in the wastewater [3].
Pseudo-first and -second order reaction kinetics for wastewater
are presented in Figs. 14 and 15, respectively.
All calculated results are summarized in Table 2.
Calculated pseudo-second order reactions and experimental qe
values are closer for both aqueous solutions and raw wastewater
(Table 2). Determined R2 values were also higher in second-order
reaction kinetics.

Table 2
Comparison of adsorption rate constants, experimental and calculated qe values for the pseudo-first and -second order reaction kinetics of removal of NH4+ ion by Zeolite 13X.

Initial NH4+ ion concentration (mg/L) qe,experimental (mg/g) Pseudo-first order Pseudo-second order

k1 (1/min) qe,caculated (mg/g) R2 k2 (g/mg min) qe,caculated (mg/g) R2

Synthetic
15 2.66 0.038 0.457 0.8219 1.213 2.57 0.9993
25 4.80 0.103 1.082 0.9249 0.681 4.81 1.000
30 5.10 0.024 0.529 0.5838 0.579 5.10 0.9999

Wastewater
10 1.66 – – – 0.907 1.67 0.9999
15 2.55 0.046 4.527 0.9971 1.849 2.55 1.000
25 4.21 0.062 0.246 0.5714 0.5639 4.20 0.9998

Please cite this article in press as: Arslan, A., Veli, S., Zeolite 13X for adsorption of ammonium ions from aqueous solutions and hen
slaughterhouse wastewaters. J. Taiwan Inst. Chem. Eng. (2011), doi:10.1016/j.jtice.2011.11.003
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Fig. 14. Pseudo-first order reaction kinetics for the adsorption of NH4+ ion on zeolite
from wastewater.
Fig. 15. Pseudo-second order reaction kinetics for the adsorption of NH4+ ion on
zeolite from wastewater.
4. Conclusions
In this study, various zeolite types were tested for removal of
NH4+ ions from aqueous solutions and Zeolite 13X provided the
highest removal efficiency. In the experiments performed at 23 8C
temperature and 150 rpm agitation speed optimum conditions
were determined as pH 7, zeolite amount 0.5 g/100 ml and
agitation time 30 min. Obtained experimental data were evaluated
with Langmuir, Freundlich and D–R isotherms and data fitted well
with Freundlich and D–R isotherms. Freundlich isotherm adsorp-
tion intensity was 0.728 and adsorption energy value was 0.542 kJ/
mol in D–R isotherm. Lower value of adsorption energy shows
physical characteristics of the adsorption process. Reaction studies
were also performed for hen slaughterhouse wastewaters applying
optimum experimental conditions. Data of aqueous solution and
Please cite this article in press as: Arslan, A., Veli, S., Zeolite 13X for adsorption of ammonium ions from aqueous solutions and hen
slaughterhouse wastewaters. J. Taiwan Inst. Chem. Eng. (2011), doi:10.1016/j.jtice.2011.11.003
raw wastewater both fitted pseudo-second order reaction kinetics.
qe,calculated and qe,experimental values were closer in pseudo-second
order reaction kinetics. Moreover calculated correlation coeffi-
cients were higher in pseudo-second order reaction kinetics.
The results of the study indicate that there is a significant
potential for the Zeolite 13X as an adsorbent material for
ammonium removal.
Acknowledgement
The authors thank to Burcu Özdemir for her helpful contribu-
tions.
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