Desalination 262 (2010) 31–35

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Desalination
j o u r n a l h o m e p a g e : w w w. e l s ev i e r. c o m / l o c a t e / d e s a l

Comparison study of ammonia and COD adsorption on zeolite, activated carbon and
composite materials in landfill leachate treatment
Azhar Abdul Halim a, Hamidi Abdul Aziz b,⁎, Megat Azmi Megat Johari b, Kamar Shah Ariffin c
a
Environmental Health Program, Faculty of Allied Health Sciences, Universiti Kebangsaan Malaysia, Jalan Raja Muda Abdul Aziz, 50300 Kuala Lumpur, Malaysia
b
School of Civil Engineering, Engineering Campus, Universiti Sains Malaysia, 14300 Nibong Tebal, Penang, Malaysia
c
School of Materials and Mineral Resources Engineering, Engineering Campus, Universiti Sains Malaysia, 14300 Nibong Tebal, Penang, Malaysia

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

Article history: Chemical oxygen demand (COD) and ammoniacal nitrogen have always been the crucially problematic
Received 18 October 2009 parameters in landfill leachate treatment. This study was conducted to investigate the adsorption properties
Received in revised form 12 April 2010 of ammoniacal nitrogen and COD in semi-aerobic leachate from the Pulau Burung landfill site on zeolite,
Accepted 29 May 2010
activated carbon and a new composite media in terms of adsorption isotherm and kinetic. The results show
Available online 25 June 2010
that all adsorbents fitted well with both Langmuir and Freundlich isotherms (R2 N 0.9) for ammonia
adsorption. A comparison study indicated that the adsorption capacity of composite adsorbent towards
Keywords:
Ammonia
ammoniacal nitrogen was higher than zeolite and activated carbon and comparable to activated carbon for
COD COD. Findings from a kinetic study indicated that the adsorption of ammonia on new composite adsorbent
Zeolite and zeolite follow almost all kinetic models such as pseudo-first-order, pseudo-second-order, Elovich and
Activated carbon intra-particle diffusion model, although pseudo-second-order was the most dominant. COD adsorption fitted
Composite adsorbent well with the pseudo-second-order kinetic model, while activated carbon obeys the pseudo-first-order and
Leachate intra-particle models.
© 2010 Elsevier B.V. All rights reserved.

1. Introduction or low cost adsorbents such as limestone, rice husk ash and peat.
Activated carbon provides an attachment surface for micro-organisms
Organic contaminant and ammoniacal nitrogen are two of the to bioregenerate the activated carbon [8]. Combinations of organic and
problematic parameters in landfill leachate treatment. Biological inorganic pollutants that exist in landfill leachate need adsorbents
treatment of landfill leachates have been shown to be very effective which have the ability to remove a variety of pollutants including
in removing organic matter in early stages [1] when the BOD/COD ratio organic and inorganic species. It is well known that activated carbons
of the leachate is high. This ratio decreases with the age of the landfill are the most effective adsorbents for the removal of organic pollutants
[2] and the process is less effective with time [3] due to the presence of from the aqueous or gaseous phase. Therefore, this type of adsorbent is
refractory organic matter. A high concentration of ammoniacal widely applied as a commercial adsorbent in the purification of water
nitrogen is also known to inhibit the biological degradation by the and air [9,10]. Zeolite is widely used as a natural ion exchanger to
micro organism [4,5]. Young landfill leachates are usually treated more remove ammonia and other inorganic pollutants from leachate or
easily as compared to the old ones [6]. As a landfill stabilizes with the other wastewater.
passage of time, the biodegradable organic content of the leachate However, general activated carbon does not have enough
tends to decrease, and consequently, the effectiveness of the biological adsorption capacity for ammonia because it usually possesses a
process decreases and physico-chemical processes may become one of non-polar surface due to manufacturing conditions at high tempera-
the appropriate options. The common features of stabilized leachate tures, which is a disadvantage for some applications because of poor
are high strengths of ammoniacal nitrogen (3000–5000 mg/L) and interaction with some polar adsorbates [11]. This is the reason that
moderately high strengths of COD (5000–20,000 mg/L), as well as a much research has been focused on modifying the AC surfaces or to
low ratio of BOD/COD (less than 0.1) [7]. produce composite adsorbent that have the ability to interact with
One of the physico-chemical processes is adsorption using either either polar or non-polar adsorbates.
activated carbon or other adsorbents such as zeolite, activated alumina Gao and co-workers found new composite materials of zeolite–
carbon (Z–C), which combines the excellent properties of zeolites and
carbon [12]. The surface of zeolite is hydrophilic with regular aligned
⁎ Corresponding author. Tel.: + 60 4 5996215; fax: + 60 4 5941009.
molecular level pores and cationic exchange ability, which makes it a
E-mail addresses: [email protected] (A.A. Halim), [email protected] good adsorbent for metallic ions and catalysts [13]. On the other hand,
(H.A. Aziz), [email protected] (M.A.M. Johari), [email protected] (K.S. Ariffin). the surface of carbon is hydrophobic with pore sizes in the nanometer

0011-9164/$ – see front matter © 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.desal.2010.05.036
32 A.A. Halim et al. / Desalination 262 (2010) 31–35

range or above which makes it more suitable for the adsorption of Table 2
organic substances [14]. Semi-aerobic landfill leachate characteristics [18].

A new composite adsorbent media was produced previously by Range Average

combining activated carbon, zeolite and low cost materials such as
pH 8.09–8.66 8.29
limestone, rice husk carbon waste and ordinary Portland cement. The Suspended solids (mg/L) 124–190 165.57
latest was used as a binder [15]. The purpose of this study is to compare Ammoniacal nitrogen (mg/L) 1010–2740 1890.95
the adsorption properties of new composite adsorbents, zeolite and COD (mg/L) 1478–3540 2338.29
BOD5 (mg/L) 160–345 227.58
activated carbon in terms of ammonia, COD, color and iron removal.
BOD5/COD 0.06–0.15 0.09
Fe (mg/L) 2.94–7.30 5.41
2. Materials and methods Color (mg/L) 3773–5100 4527.36

2.1. Composite adsorbent preparation

all pertinent factors, such as dose, pH, agitation speed, and contact
The development of a new adsorbent using coconut shell activated time. Subsequent adsorption experiments were carried out with only
carbon (surface area, 1240 m2/g), zeolite (mordenite, Na8Al8Si40O96•24- optimized parameters. The optimum conditions for the adsorption
H20 with cation exchange capacity of 0.31 meq/g), limestone and rice batch study taken from the previous study are pH 7, 200 rpm of
husk carbon as composite materials was based on previously reported shaking speed and 105 min of contact time [15,18,20]. A similar pH
findings [15]. This adsorbent contains 45.94% zeolite, 15.31% limestone, range was reported for ammonia removal in other batch adsorption
4.38% activated carbon and rice husk carbon respectively, and 30% of studies [21]. All of the ammonia present was expected to be in ionic
ordinary Portland cement (OPC) which was used as a binder. All the form and available for ion exchange. Adsorption isotherm tests were
materials were ground to obtain particle sizes of less than 150 μm and also carried out in the reaction mixture consisting of 100 ml of
then mixed together with OPC. About 60% (by weight) of water was added leachate solution with varying adsorbent weight. Ammoniacal
and the mixture paste was allowed to harden for 24 h and then submersed nitrogen and COD was determined using the Nesslerization method
in water for three days for curing. This composite adsorbent was crushed and closed reflux colorimetric method respectively [17].
and sieved to a working size of 1.18 mm–2.36 mm. The physico-chemical
properties of the composite adsorbent are listed in Table 1. 3. Results and discussion

2.2. Semi-aerobic landfill leachate 3.1. Adsorption equilibrium

Leachate sample was collected from the Pulau Burung Landfill Site Adsorption isotherms are essential for the description of how
(PBLS) which is situated within Byram Forest Reserve at 5° 24′ N, 100° adsorbate concentration will interact with adsorbent media and are
24′ E in Penang, Malaysia. The total area of the landfill is 23.7 ha and it useful to optimize the use of media as adsorbents. Therefore,
is equipped with a leachate collection pond but does not have other empirical equations (Langmuir and Freundlich isotherm model) are
treatments. This site has a natural marine clay liner. PBLS has a semi- important for adsorption data interpretation and predications. Both
aerobic system and it is one of only three sites of its kind found in Freundlich and Langmuir models were used for the evaluation of
Malaysia. PBSL has been developed semi-aerobically into a Level II experimental results. The Langmuir model assumes only one solute
sanitary landfill by the establishment of a controlled tipping molecule per site, and also assumes a fixed number of sites. The
technique in 1991. It was upgraded to a Level III sanitary landfill by Langmuir isotherm relates qe (mg of adsorbate adsorbed per gram of
employing controlled tipping with leachate recirculation in 2001. This adsorbent media) and Ce (the equilibrium adsorbate concentration in
site receives 1500 t of solid waste daily [16]. solution) as shown in Eq. (1) as
Samples were collected from the active detention pond with a
leachate age of less than 5 years. The sample was filled into a 30-L QbCe
qe = ð1Þ
plastic container, transported to the laboratory and stored at 4 °C. ð1 + bCe Þ
Chemical analysis was performed for the following two days,
according to Standard Methods for the Examination of Water & where coefficient Q represents the maximum adsorption capacity in
Wastewater [17]. All chemicals used for the analytical determinations mg/g and b is the Langmuir constant in L/mg. The constants in the
were of analytical grade. The characteristics of the leachate from the Langmuir isotherm can be determined by plotting 1/qe versus 1/Ce,
semi-aerobic landfill site (Pulau Burung, Penang, Malaysia) are listed where the equation can be rewritten in the linear form;
in Table 2 [18]. The leachate is considered stable because its pH
exceeds 5 and the BOD5–COD ratio is very small (b0.1) [19]. 1 1 1
= + : ð2Þ
qe Q QbCe
2.3. Batch adsorption experiments
Freundlich isotherm assumes that the uptakes of adsorbate occur
To maximize removal by the adsorbent, batch experiments were on a heterogeneous surface by multilayer adsorption and the amount
conducted at ambient temperature using the optimum conditions of of adsorbate adsorbed increases infinitely with an increase in
concentration. The Freundlich equation is given as
Table 1
Physico-chemical characteristics of composite adsorption media. 1=n
qe = KF Ce ð3Þ
Physico-chemical properties of composite media

Specific gravity (g/cm3) 2.80 where KF is, roughly, an indicator of the adsorption capacity and 1/n is
BET Surface area (m2/g) 60.94 the adsorption intensity. A linear form of the Freundlich expression
Porosity (%) 55.76
will yield the constants KF and 1/n.
Water absorption (%) 52.48
Methylene blue number (mg/g) 6.33
Iodine number (mg/g) 16.92 1
Cation exchange capacity, CEC (meq/g) 0.9204 log qe = log KF + log Ce ð4Þ
n
 A.A. Halim et al. / Desalination 262 (2010) 31–35 33

Therefore, KF and 1/n can be determined from intercept and slope of

the linear plot of log qe versus log Ce. The magnitude of the exponent 1/n
gives an indication of the favorability of adsorption. Values of n N 1 for all
parameters shown in Table 3 represent favourable adsorption [22]. The
adsorption equilibrium for ammoniacal nitrogen and COD adsorption on
composite adsorbent, zeolite and activated carbon are indicated in
Table 3.

3.2. Ammonia

Fig. 1 shows the percentage of ammonia removal in comparison

between composite media, zeolite and activated carbon in various
dosages. The results show that composite media and zeolite do not show
Fig. 1. Ammonia removal using composite media, zeolite and activated carbon as
an obvious difference in ammoniacal removal but are obviously higher
adsorbent.
than activated carbon. The isotherm constants and correlation coeffi-
cients for ammonia uptake from semi-aerobic leachate to zeolite,
composite media and activated carbon are given in Table 3. In terms of zeolite was the lowest. Table 3 presents the comparisons of isotherm
ammonia adsorption capacity, composite media was the highest constants and correlation coefficients between composite, zeolite and
(32.89 mg/g), followed by zeolite (17.45 mg/g) and the lowest was activated carbon. A high surface area, wide range of pore size
activated carbon (6.08 mg/g). These results demonstrate that activated distribution and hydrophobic surface gives advantage for activated
carbon does not have enough adsorption capacity for ammonia because carbon to adsorb organic pollutant from leachate. The same results
it usually possesses a non-polar surface due to manufacturing conditions reported that PAC was slightly more effective than zeolite for COD
at high temperatures, which is a disadvantage for some applications removal at a 5 g/L of dosage, while zeolite had higher removal
because of a poor interaction with some polar adsorbates [11]. It is well efficiency for ammoniacal nitrogen than PAC at a 1 g/L of dosage [6]. In
known that ammonium ions are removed from aqueous solutions by general, the application of activated carbon adsorption (GAC or PAC)
zeolites via cation exchange and physical adsorption mechanism. is effective for the removal of non-biodegradable compounds from
However, physical adsorption is dominant for activated carbon by the leachate, but not for ammoniacal nitrogen [23].
wide range of pore sizes that are available on its surface. Furthermore, A combination of carbon-based and minerals (zeolite) materials in
zeolite surface is hydrophilic and has more affinity towards ammonia or composite adsorbent combine the excellent properties of both
ammonium ions in aqueous solution compared to the hydrophobic adsorption materials in a single composite adsorption media.
surface on activated carbon. Both Langmuir and Freundlich model were Although COD removal by composite media was slightly lower than
applicable for all media according to the high value of R2 (above 0.9). activated carbon, it was much higher compared to zeolite. As zeolite is
an inorganic substance or specifically an alumino-silicates substance,
3.3. COD no organic leaching from fresh zeolites is expected. Possible
regeneration of adsorbent using normal salt (0.5 M sodium chloride)
Fig. 2 apparently indicates that activated carbon was the most proves that the method is practical to be applied in the field [31].
effective for COD removal, closely followed by composite media while
3.4. Kinetic study
Table 3
Ammonia and COD isotherm constant for composite media, zeolite and activated Normally, adsorption processes take place in a multistep mechanism
carbon. such as (i) diffusion across the liquid film surrounding the solid particles
Isotheram Composite Zeolite Activated carbon (a process controlled by an external mass transfer coefficient),
adsorbent (ii) diffusion within the particle itself by assuming a pore diffusion
Langmuir mechanism (intra-particle diffusion) and (iii) physical or chemical
Ammonia adsorption at a site [22]. Kinetic data was analyzed with the pseudo-
R2 0.9718 0.9680 0.9371 first-order, pseudo-second-order kinetic, Elovich and intra-particle
Q (mg/g) 24.34 17.4520 6.0790
diffusion equations. The pseudo-first-order kinetic equation is;
b (L/g) 2.15 × 10− 4 3.14 × 10− 4 1.51 × 10− 3
0:0052Ce 0:0055Ce 0:009Ce
Equilibrium qe = 1 + 2:15 × 10−4 C
qe = 1 + 3:14 × 10−4 C
qe = 1 + 1:51 × 10−3 C
e e e
isotherms
COD lnðqe −qt Þ = lnðqe Þ–k1 t ð5Þ
R2 0.965 0.8184 0.9819
Q (mg/g) 22.99 2.3458 37.88
b (L/g) 9.4 × 10− 4 1.14 × 10− 3 1.0 × 10− 3
0:2161Ce 0:0027Ce 0:038Ce
Equilibrium qe = −4 qe = qe =
1 + 9:4 × 10 Ce 1 + 1:14 × 10−3 Ce 1 + 1:0 × 10−3 Ce
isotherms

Freundlich
Ammonia
R2 0.9736 0.9631 0.9335
Kf 0.0188 0.1054 0.00175
1/n 0.8293 0.8287 0.8866
Equilibrium qe = 0.0188C0.8293
e qe = 0.1054C0.8287
e qe = 0.00175C0.8866
e
isotherms
COD
R2 0.9291 0.8051 0.9384
Kf 0.0642 1.27 × 10− 5 0.1543
1/n 0.7637 1.996 0.6875
Equilibrium qe = 0.0642Ce0.7637 qe = 1.27 × 10 qe = 0.1543Ce0.6875
− 5 1.996
isotherms Ce
Fig. 2. COD removal using composite media, zeolite and activated carbon as adsorbent.
34 A.A. Halim et al. / Desalination 262 (2010) 31–35

where k1 is the rate constant (min− 1) of pseudo-first-order model, qe Table 4

and qt are adsorption capacity (mg/g) at equilibrium and at time t Kinetic adsorption comparison for ammonia adsorption on composite adsorbent,
zeolite and activated carbon.
respectively. The plot of ln(qe − qt) versus t gives, k1 and qe values.
Pseudo-second-order kinetic model was also applied to analyze Kinetic model Adsorbent
kinetic adsorption for liquid solution kinetic adsorption in the Ammoniacal Constants Composite Zeolite Activated
following linear form [24]; nitrogen carbon

1st order R2 0.9694 0.9141 0.9089

t 1 1 K1 (min− 1)
= + ðt Þ ð6Þ 0.1488 0.0279 0.0066
qt k2 q2e qe qe (mg/g) 16.34 9.9892 8.9370
2nd order R2 0.9987 0.9933 0.8548
where k2 is the rate constant of pseudo-second-order model (g/ k2 (g/mg min) 0.0174 0.0058 0.005784
qe (mg/g) 24.81 16.0282 6.8966
(min mg)) and qt and qe are the amount of adsorbate adsorbed at time
Elovich R2 0.8672 0.946 0.8750
t and at equilibrium (mg N/g), respectively. The values of constants α (mg/g min) 93.5251 20.6291 0.3577
(k2 and qe) can be obtained from the intercept and slope of the linear β (g/mg) 0.2903 0.4331 0.7407
plot of t/qt versus t. The Elovich kinetic model is given as the following qe (mg/g) 11.57 15.8007 4.8985
Intra-particle R2 0.7291 0.9850 0.9317
equation;
Ki (mg/g min1/2) 1.4871 0.7931 0.4910
c 14.6450 7.9021 − 0.2787
dqt −βq
= αe t ð7Þ qe (mg/g) 22.7902 16.5901 4.7526
dt experimental qe(exp) (mg/g) 23.5 16.6 4.8

where α is the initial rate (mg/g min) because (dqt/dt) approaches α

when qt approaches zero, and the parameter β is related to the extent
of surface coverage and activation energy for chemisorptions (g/mg) when R2 for pseudo-second-order was 0.9933 and the calculated qe
[25,26]. The linear form of Elovich equation can be simplified as [26]; using this model was 16.03 mg/g compared to 16.60 mg/g for the
experimental qe. Previous studies have reported that the adsorption of
1 1 ammonia on zeolite obeys the pseudo-second order model [28,29].
qt = ln ðαβÞ + ln t ð8Þ
β β Different results were observed for activated carbon which tends
to obey the pseudo-first-order and intra-particle models where R2
Determination of rate parameter for intra-particle diffusion uses were 0.9089 and 0.9317 respectively. However, the calculated qe
the following equation [22]; value (8.9370 mg/g) that was obtained from the pseudo-first-order
was far deviated from the experimental qe (4.8 mg/g), while the qe
0:5
qt = ki t +c ð9Þ value (4.75 mg/g) of the intra-particle model was more agreeable.
Thus, ammonia adsorption on activated carbon tends to obey the
where C is the intercept and ki is the intra-particle diffusion rate intra-particle kinetic model. These results suggest chemisorption or
constant (mg/g min− 1/2). The plot may present multilinearity, ion exchange was the dominant mechanism for ammonia adsorption
indicating that three steps take place. The first, sharper portion is on composite media and zeolite, and physical adsorption for activated
attributed to the diffusion of adsorbate through the solution to the carbon.
external surface of adsorbent or the boundary layer diffusion of solute
molecules. The second portion describes the gradual adsorption stage,
where intra-particle diffusion is rate limiting [27]. 3.4.2. COD
Aggregate organic constituents are generally indicated by chem-
3.4.1. Ammonia ical oxygen demand or COD. Fig. 4 shows the dynamics of COD
Adsorption rate for ammonia on composite adsorbent, zeolite and adsorption on composite media, zeolite and activated carbon. The
activated carbon is shown in Fig. 3. Adsorption rate of ammonia on kinetic parameters are listed in Table 5. Zeolite showed the fastest
composite adsorbent was the fastest to reach equilibrium (30 min), adsorption rate followed by activated carbon and composite media.
followed by zeolite (60 min) and activated carbon (105 min). The rate COD adsorption (reflect to aggregate organic constituents) obeys the
parameters of this adsorption kinetic models listed in Table 4 clearly pseudo-second-order kinetic model when both gave the best
indicate that adsorption of ammonia from aqueous solution on correlation (R2 = 0.99). Activated carbon obeys the pseudo-first-
composite media obeys the pseudo-second-order kinetic model order (R2 = 0.97) and intra-particle (R2 = 9317) models, and shows a
according to R2 (0.9987), and the calculated value qe (24.81 mg/g) weak correlation (R2 = 0.5071) for the pseudo-second-order. These
agree very well with the experimental qe (23.50 mg/g). Kinetic results demonstrate that both chemical adsorption (dominant) and
adsorption ammonia on zeolite indicated almost the same results

Fig. 3. Ammonia kinetic adsorption on composite, zeolite and activated carbon. Fig. 4. COD kinetic adsorption on composite, zeolite and activated carbon.
 A.A. Halim et al. / Desalination 262 (2010) 31–35 35

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