Iraqi Journal of Chemical and Petroleum Engineering 

 Vol.18 No.1 (March 2017) 47 - 56 

ISSN: 1997-4884 

 
 
 
 
 

Equilibrium, Kinetic and Thermodynamic Study of Aniline 

Adsorption over Prepared ZSM-5 Zeolite 

 
Ammar S. Abbas* and Sally A. Hussien 

*Chemical Engineering Department – College of Engineering – University of Baghdad (Iraq) 

*Email: ammarabbas@coeng.uobaghdad.edu.iq 

 

Abstract 

Aniline and its derivatives are common contaminants in various wastewaters 

and represent a serious worry for societies health and a challenge to ecologists due to 

their dangers effects on to the human health.  

ZSM-5 zeolite was prepared from locally available materials (kaolin and rice 

husk) for adsorption of aniline from synthetic wastewater. Characterization of the 

prepared zsm-5, kinetics and thermodynamic of the adsorption process were 

investigated. 

The characterization results of the prepared zsm-5 zeolite showed that the 

surface area was 270.1 m
2
/g and pore volume 0.21828 cm

3
/g. The silica to alumina 

ratio (Si/Al) was 166. 47 and the sodium content was 11 wt. %. The atomic force 

microscope (AFM) results showed that the average particle diameter of the prepared 

adsorbent was 70.71nm. 

Langmuir isotherm better illustrated the adsorption process with maximum 

uptakes 8.3125 mg/g. Whereas, kinetics results of the adsorption process showed it 

the pseudo-second order in different operating temperatures.  

The calculated values of ΔG showed that the adsorption process was 

spontaneous, while the ΔH results illustrated the process to be exothermic nature of 

this process with negative values of ΔS. 

   

Key words: Adsorption, aniline, zsm-5, zeolite, wastewater, kinetics, 

thermodynamic. 

 

Introduction  

Aniline is one of the supreme 

common contaminants found in wastes 

from the various industrial wastewater 

such as pharmaceutical, pesticide, 

dyestuff, petrochemicals, tanneries, 

distilleries, textile, paper and pulp 

mills, electroplating, food processing 

and agrochemical industries [1]. 

Accordingly, the elimination of aniline 

from these effluents has become a 

social worry especially for the colored 

effluents. Color being a visible 

pollutant, The water contaminated with 

aniline is not only unfit for drinking 

purpose due to transformation of 

hemoglobin to methemoglobin, which 

has a lower affinity for oxygen than 

hemoglobin, therefore decreases 

blood’s ability to transport oxygen, but 

is also not suitable for agriculture due 

University of Baghdad 
College of Engineering 

Iraqi Journal of Chemical and 
Petroleum Engineering 

 

mailto:ammarabbas@coeng.uobaghdad.edu.iq


Equilibrium, Kinetic and Thermodynamic Study of Aniline Adsorption over Prepared ZSM-5 Zeolite 

  

  

48                                   IJCPE Vol.18 No.1 (March 2017)                 -Available online at: www.iasj.net 
 

to its inhibitory action on 

photosynthetic process in plants [2], 

[3].  

Numerous methods are used to 

treat wastewater containing aniline 

such as oxidation, extraction, 

membrane separation, biochemical 

decomposition, and adsorption [3], [5], 

[6].  

Among all methods, the 

adsorption is the most effective way to 

remove aniline and such organics from 

wastewater. Adsorption technique does 

crop harmful byproducts, and the 

recycling of both the adsorbent and 

pollutants is possible. One challenge 

met by adsorption technology is the 

discovery of new adsorbents like 

activated carbons, polymer resin, clays, 

mesoporous oxides and zeolite, that 

effectively eliminate organic 

pollutants, such as aniline, from 

aqueous solutions.[1], [2], [3], [7]. 

In the design and optimization of 

adsorption processes, the adsorption 

isotherms and kinetics are of greatest 

importance to study. Adsorption 

isotherms are essential for the 

description of how adsorbate will 

interact with adsorbent and are in 

necessary optimizing the use of 

adsorbent. Thus, the correlation of 

experimental equilibrium data using 

either a theoretical or an empirical 

equation is essential for adsorption 

performance assessment. Adsorption 

kinetics involves the study of the rate 

at which pollutants are removed from 

aqueous solution onto adsorbent 

surface, which in turn controls the 

residence time of the adsorbate uptake 

at the solid-solution interface [8]. 

 

Aim of the Work 

The aim of this research is the 

removal of aniline from wastewater by 

prepared ZSM-5 zeolite. 

Characterization results of prepared 

ZSM-5 zeolite adsorbent were 

discussed. The study the isotherm 

models of adsorption to identify the 

effect of temperature and time on the 

removal of aniline in a batch 

experiments was presented. Finally, 

the study of kinetics and 

thermodynamics of the aniline 

adsorption over prepared zeolite in the 

best selected conditions, was 

illustrated. 
 

Adsorption Isotherms and 

Thermodynamics  
 

Langmuir Isotherm 
The Langmuir adsorption isotherm 

represented by Equation 1, Langmuir 

in (1918) 

 
  

  
 

 

    
 

  

  
                                …(1) 

 

Where, Ce is the equilibrium 

concentration (mg/L) of adsorbate 

(aniline) in the bulk;   is the amount 
of adsorbate (mg/g) adsorbed at 

equilibrium.   and ‘  ’ are Langmuir 
constants related to adsorption 

efficiency and energy of adsorption, 

respectively [2]. 

 

Freundlich Isotherm  
Freundlich in 1906 represented the 

adsorption isotherm as shown in 

Equation 2: 

 

Log   = log    + 
 

 
 log               …(2) 

 

Where    and    have their usual 
meanings and the constants    and n 
are measures of adsorption capacity 

and intensity of adsorption, 

respectively [2]. 

  

Hill Isotherm  
The Hill equation (in, 1910) was 

postulated to describe the binding of 

different species onto homogeneous 

substrates defined as: 
 

   
     

  

     
                                    …(3) 

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Where    , nH, and qsH (mg/L) 
are Hill isotherm constants, Hill 

cooperatively coefficient of the 

binding interaction and Hill isotherm 

saturation uptake. The model assumes 

that adsorption is a cooperative 

phenomenon by which ligand binding 

at one site of the macromolecule may 

influence different binding sites on the 

same macromolecule [9]. 

 

Sips Isotherm 
Sips (in 1948) combined the 

Langmuir and Freundlich isotherm 

type models to describe heterogeneous 

surface much better. Sips adsorption 

isotherm is given by the Equation 4: 

 

   
      

   

      
                                  …(4) 

 

Where    (mg/g) is the 
maximum adsorbed amount of 

adsorbate per unit mass of adsorbent, 

    ((l/mg) ^1/m) is sips constant 
related to energy of adsorption, and 

parameter m could be regarded as the 

parameter characterizing the system 

heterogeneity [4]. 

 

Redlich–Peterson Isotherm  
The Redlich–Peterson isotherm 

(in, 1959) is a hybrid isotherm 

featuring both Langmuir and 

Freundlich isotherms, which 

incorporates three parameters into an 

empirical equation given by: 

 

   
    

      
                                  …(5) 

 

Where    (L/g) and    (1/mg) 
are Redlich–Peterson isotherm 

constants, and g is the isotherm 

exponent. The model can be applied 

either in homogeneous or 

heterogeneous systems. It approaches 

the Freundlich isotherm model at high 

concentration and in accordance with 

the low concentration limit it 

approaches the ideal Langmuir 

condition [9]. 

 
Toth Isotherm 

The Toth isotherm model (in, 

1971) is another empirical equation 

developed to improve Langmuir 

isotherm fittings. It is useful in 

describing heterogeneous adsorption 

systems, and satisfies both low and 

high-end boundary of concentrations: 

 

   
    

       
   

                             …(6) 

 
Where KT (mg/g),    (L/mg) is 

the Toth isotherm constants. The 

correlation presupposes an 

asymmetrical quasi-Gaussian energy 

distribution where most binding sites 

have an adsorption energy lower than 

the peak value [9]. 

 

Adsorption Kinetics [7], [12]    

1- Pseudo_First Order Model 
 The psedo first-order kinetic model 

can be represented as follow:  

 
   

  
                                   …(7) 

 

Integration of Equation 7 for the 

boundary condition t=0 to t=t and qt=0 

to qt=qt: 

 

                              …(8) 
 

Where    (mg/g) and    (mg/g) are the 
amounts of adsorbed adsorbate at 

equilibrium and at time t respectively, 

and   (   
    is the rate constant of 

pseudo first order equation. 

 

2- Pseudo_Second Order Model 
The pseudo second_order kinetic 

model can be represented as follows: 

 
   

  
          

                        …(9) 

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Equilibrium, Kinetic and Thermodynamic Study of Aniline Adsorption over Prepared ZSM-5 Zeolite 

  

  

50                                   IJCPE Vol.18 No.1 (March 2017)                 -Available online at: www.iasj.net 
 

Integration Equation 9 for the 

boundary condition t=0 to t=t and q=0 

to q=  : 
 
 

  
 

 

    
 
 

 

  
                            …(10) 

 

Where    (mg/g) and    (mg/g) are the 
amounts of adsorbed adsorbate at 

equilibrium and at time t respectively, 

and    (g/mg. min) is the equilibrium 
rate constant of pseudo second order 

model. 
 

3- Intra_Particle Diffusion Model  
The intra-particle diffusion kinetic 

model can be represented as follow: 
 

      
 

 ⁄                             …(11) 
 

Where    (mg/g) is the amount 
of solute on the surface of sorbent at 

time t,    (mg/g.   
 

 ⁄ ) is the intra-

particle diffusion rate constant and c 

(mg/g) is the intercept 
 

Adsorption Thermodynamics  
Adsorption thermodynamic is an 

important tool elucidating the 

adsorption behavior of an isolated 

system. Its original concept assumes 

that energy cannot be gained or lost, 

and entropy changes. The values of 

enthalpy change (ΔH), Gibbs free 

energy change (ΔG), and entropy 

change (ΔS) were computed using the 

following equation: 
 

     
  

 
 

  

  
                          …(12) 

 

ΔG = - RT                              …(13) 
 

   
     

 

 
 

  
                                 …(14) 

 

Where R is the universal gas 

constant (8.314 J/mol. K), T is 

temperature (K), and    is the 
distribution coefficient for the 

adsorption [10].  

 

Experimental Work 

Material 

The reactant materials used in 

this study were silica SiO2 (purity 

92%) molecular weight 60.08 g/mole 

as silica source, tetrapropylammonium 

hydroxide solution (TPAOH, 

C12H29NO, 20% aqueous solution, 

Merck) as direct template agent, 

sodium hydroxide (NaOH, 98 wt%, 

Merck) and kaolin as alumina source. 
 

Zeolite Preparation 

Kaolin was sieved to a particle 

size ≤ 75µm. 4g of NaOH was 

dissolved in 70 ml of distilled water 

and then divided in two portion. 29.8 g 

of SiO2 were dissolved in one portion 

of sodium solution and stirred until 

clear solution was reached, after that 

was added 18.3 g of 20% of TPAOH to 

sodium silicate solution and stirred to 

60 min. 1.7 g of kaolin (alumina 

source) was mixed with the another 

portion of sodium solution. 

Silicate solution was slowly 

added to aluminate solution and stirred 

to 60 min. The mixture was placed in 

Teflon-lined stainless steel autoclave at 

150 C for 96 hr. The product obtained 

was filtered and washed with distilled 

water for several times until pH value 

dropped to 8.5 after that the product 

was dried in an electrical oven at 

110˚C overnight and followed by 

calcination at 550 ˚C for 3 h. 
 

Characterization and Analysis of 

Prepared ZSM-5 Zeolite 

The prepared catalyst was 

characterized by using different 

instrumental analysis techniques such 

as: X–Ray Diffraction (XRD), Atomic 

Force Microscope (AFM), BET 

specific surface area and pore volume 

by ISO-9277-2010 method, sodium 

content by ASTM D-1428-64 method, 

and X-ray Fluorescence (XRF) for 

determine the silica content and silica 

to alumina ratio. 
 

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Experimental Procedure  
Batch adsorption experiments 

were conducted in a set of 250 mL 

Erlenmeyer flasks containing 0.05 g of 

ZSM-5 zeolite per 10 ml of solution 

containing 60 mg/L of the aniline. The 

mixture was agitated in a thermostatic 

orbital shaker at room temperature   

with an agitation speed of 150 rpm. 

The aniline concentration in the 

supernatant was determined using a 

double beam UV–Vis 

spectrophotometer (Shimadzu UV160-

A, Japan) at 280 nm. Each experiment 

was carried out in triplicates under 

identical conditions and an average 

value was determined. qe (mg/g), was 

calculated by: [9] 
 

   
         

 
                             …(15) 

 

Where Co and Ce (mg/L) are the 

liquid phase concentration of aniline at 

initial and equilibrium, respectively. V 

(L) is the volume of the solution, and 

the W (g) is the mass of adsorbent used 

[9]. 
 

Results and Discussion 
X-ray diffraction pattern was 

determined for prepared zsm-5 zeolite 

as shown in Figure 1. The comparison 

between lattice spacing of prepared 

zsm-5 zeolite with standard synthetic 

one is shown in Table 1. The 

comparison in the lattice spacing 

shows that the prepared zsm-5 zeolite 

is approximately comparable with the 

standard. 

 

 
Fig. 1: XRD pattern of prepared zeolite-ZSM_5 

 

Table1: Comparison of lattice spacing between prepared ZSM-5zeolite and standard synthetic ZSM-

5zeolite 

       Prepared zsm-5 zeolite          Standard zsm-5 zeolite 

Angle (2ɵ) deg. d, spacing (Å) Angle (2ɵ) deg. d, spacing (Å) 

7.453 11.85116 7.93 11.153 

8.06 10.95828 8.01 11.033 

8.95 9.86504 8.90 9.939 

9.133 9.675 9.14 9.673 

14.945 5.92300 14.99 5.909 

15.612 5.67156 15.63 5.669 

16.045 5.51930 16.07 5.517 

19.157 4.62933 19.24 4.613 

20.981 4.23063 20.94 4.242 

23.200 3.83080 23.19 3.836 

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Equilibrium, Kinetic and Thermodynamic Study of Aniline Adsorption over Prepared ZSM-5 Zeolite 

  

  

52                                   IJCPE Vol.18 No.1 (March 2017)                 -Available online at: www.iasj.net 
 

The silica to aluminum ratio (Si/Al) of 

ZSM-5 zeolite was equal to 166.47 

according to XRF analysis which lie in 

the range of Si/Al ratio of standard 

ZSM-5 zeolite (10_∞). Also, these 
results were in a good agreement with 

Sari et al., [11] who mentioned that the 

ratio of silica to alumina in ZSM-5is 

about 177. The BET surface area and 

pore volume of ZSM-5 zeolite were 

270.1 m
2
/g and 0.21828 cm

3
/g 

respectively with sodium content equal 

to 11 wt. %. The AFM analysis was 

shown that the ZSM-5 zeolite have 

average nano particle equal to 70.71 

nm. 
 

Adsorption Isotherm 
The adsorption isotherms 

illustrate the interaction between the 

adsorbates and adsorbents. Adsorption 

equilibrium is established when an 

adsorbate has been contacted with the 

adsorbent for enough time, and the 

adsorbate concentration in the bulk 

solution is in balance with the interface 

concentration [13]. The fitting of 

adsorption data isotherm models is a 

main step to find the appropriate model 

that can be used for design purposes. 

In this work, experimental equilibrium 

data for aniline adsorption on zsm-5   

zeolite, calculated from Equation 15, 

fitted to the Langmuir and Freundlich 

isotherms, Equations 1 and 2 

respectively. Results are represented in 

Figures 2 and 3. The results of this 

fitting, as summarized in Table 2, 

show that Langmuir isotherm has the 

highest    value as compared to that 
Freundlich isotherm. The Langmuir 

model correlates the equilibrium data 

with    (correlation factor) values of 
0.9987 for aniline, suggesting the 

monolayer adsorption of aniline on 

zsm-5 zeolite. These results are in 

good agreement with [3]. For the 

Langmuir isotherm, the values of    
(separation factor) are 0.0311 for 

aniline, which indicate the favorability 

of aniline adsorption on zsm-5 zeolite. 

Also, Table 2 shows that the Langmuir 

isotherm gives maximum adsorption 

capacity of 8.3125 mg/g for aniline. 

 

 
Fig. 2: Langmuir adsorption isotherm of aniline on zsm-5 zeolite  

 

Table 2: Isotherm parameters for aniline adsorption on zsm-5 zeolite  

Isotherm Parameter 
Temperature (k) 

303 

Langmuir q, max(mg/g) 

KL (l/g) 

R
2
 

RL 

8.3125 

0.5196 

0.9987 

0.0311 

Freundlich KF ((mg/g)(l/g))1/n 

n 

R
2 

-0.3480 

2.6371 

0.9228 

0

0.5

1

1.5

2

2.5

3

3.5

0 5 10 15 20 25

C
e

/q
e

 (
g

/l
) 

Ce (mg/l) 

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Fig. 3: Freundlich adsorption isotherm of aniline on zsm-5 zeolite 

 

Adsorption Kinetics 

Two kinetic models: pseudo- 

first order and pseudo- second order 

models, Equations 8 and 10, where 

used to correlate the experimental 

kinetic data of aniline on zsm-5 zeolite 

at different temperature. The pseudo- 

first order equation is of low R
2
 values 

as compared to the pseudo- second 

order equation, as shown in Table 3. 

High deviation between the 

experimental and calculated adsorption 

capacity can be seen from this table. 

On the other hands, the linear plot of 

t/qt versus t Figures 5 for pseudo- 

second order equation has high R
2
 

values compared to pseudo- first order 

model. The results of this tables show 

that the adsorption kinetics data are 

better represented by pseudo- second 

order and the values of K2 increased 

with increasing solution temperature 

taking the values 0.02196, 0.0245 and 

0.0280 for aniline at 303, 313 and 323 

K respectively. On the contrary, the 

values of qe decreased with increasing 

temperature to 8.0515, 7.61035 and 

7.0028 for aniline at 303, 313 and 323 

K respectively. These results are in 

agreement with those reported by [1] 

and [7] for the adsorption of aniline. 

 

 
Fig. 4: Pseudo- first order kinetic for aniline on zsm-5 zeolite at different temperature 

 

0

0.2

0.4

0.6

0.8

1

1.2

-0.4 -0.2 0 0.2 0.4 0.6 0.8 1 1.2 1.4 1.6

lo
g

 q
e

 

log Ce 

-2.5

-2

-1.5

-1

-0.5

0

0.5

1

1.5

0 20 40 60 80 100 120 140

lo
g

(q
e

-q
t)

 

t (min) 

at 30 C at 40 C at 50 C

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Equilibrium, Kinetic and Thermodynamic Study of Aniline Adsorption over Prepared ZSM-5 Zeolite 

  

  

54                                   IJCPE Vol.18 No.1 (March 2017)                 -Available online at: www.iasj.net 
 

 
Fig. 5: Pseudo- second order kinetic for aniline on zsm-5 zeolite at different temperature 

 

Table 3: Rate constant for aniline adsorption on zsm-5 zeolite 

Temperature 

(K) 

Pseudo- first order model 

qe, exp (mg/g) qe, cal (mg/g) K1 (1/min) R
2 

303 7.6154 2.9289 0.0509 0.8309 

313 7.2098 12.3851 0.0829 0.9163 

323 6.7203 2.0003 0.0329 0.9204 

Temperature 

(K) 

Pseudo- second order model 

qe, exp (mg/g) qe, cal (mg/g) K2(g/mg.min) R
2
 

303 7.6154 8.0515 0.02196 0.9977 

313 7.2098 7.61035 0.0245 0.9983 

323 6.7203 7.0028 0.0280 0.9996 

 

Adsorption Thermodynamics 
According to  Eqs. 12 - 14. The 

values of ΔH, ΔS, and ΔG were 

determined from the slope and 

intercept by plotting      versus 
 

 
 as 

shown in Figure 6. Table 4 summarizes 

the thermodynamic parameters at 

different temperatures for the 

adsorption of aniline onto zsm-5 

zeolite. The negative ΔH values - 

12630.6288 J/mole illustrate the 

adsorption process to be exothermic in 

nature. The ΔS values -37.0480  J/mole 

revealed decreasing randomness at the 

solution/solid interface during the 

adsorption of aniline onto zsm-5 

zeolite. Generally, the absolute 

magnitude of the change in free energy 

for physical adsorption is smaller than 

that of chemisorptions [15]. The 

obtained Gibbs free energy (-ΔG) 

values were 1390.74, 1063.98, 647.876 

(J/mol) at different temperatures 303, 

313 and 323 K, respectively. The ΔG 

values were negative indicating that 

the adsorption process occurred 

spontaneously. Because ΔG decreased 

with the increase of temperatures, it 

confirmed that adsorption more likely 

occured at lower temperatures. These 

results are in agreement with those 

reported [14].  

 
Table 4: Thermodynamics parameter for adsorption aniline on zsm-5 zeolite 

 
 

 
 

 

0

2

4

6

8

10

12

14

16

18

20

0 20 40 60 80 100 120 140

t/
q

t 
(m

in
.g

/m
g

) 

t (min) 

at 30 C at 40 C at 50 C

-ΔG(J/mole) 

 

303 k              313 k            323 k 

ΔS(J/mole) ΔH(J/ mole) 

1390.74         1063.98     647.876 -37.0480 -12630.6288 

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Fig. 6: Thermodynamic of adsorption aniline on zsm-5 zeolite 

 

Conclusions 
According to the results obtained 

from this study, the following 

conclusions are obtained: 

1. The characterization results, i.e 
silica to alumina ratio (Si/Al) 166. 

47, surface area of  270.1m
2
/g,  pore 

volume 0.21828 cm
3
/ g and sodium 

content 11 wt% for prepared zsm-5 

zeolite were in good with  standard 

zsm-5 zeolite, Therefore is possible 

to say that the prepared catalyst 

obtained from locally kaolin and 

rice husk in this work is zsm-5 

zeolite. 

2. The average diameter of particles of 
prepared zsm-5 zeolite determined 

by AFM was 70.71 nm, and this 

means that this catalyst is nano type 

catalyst. 

3. Maximum aniline uptakes, as 
calculated from   Langmuir 

isotherm model was 8.3125 mg/.  

4. The kinetics data were fitted to 
pseudo- second order kinetic model. 

5. The thermodynamic parameters, ΔG 
values were negative from 1390.74 

to 647.876 J/mol at different 

temperature, ΔH values was -

12630.6288J/mole and ΔS values 

was -37.0480 J/mol K.  
 

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Equilibrium, Kinetic and Thermodynamic Study of Aniline Adsorption over Prepared ZSM-5 Zeolite 

  

  

56                                   IJCPE Vol.18 No.1 (March 2017)                 -Available online at: www.iasj.net 
 

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