Indian Chemical Engineer

ISSN: 0019-4506 (Print) 0975-007X (Online) Journal homepage: http://www.tandfonline.com/loi/tice20

Optimization of Copper Adsorption by Soil of

Polluted Wasteland using Response Surface
Methodology
Arpita Ghosh & Papita Das
To cite this article: Arpita Ghosh & Papita Das (2014) Optimization of Copper Adsorption by
Soil of Polluted Wasteland using Response Surface Methodology, Indian Chemical Engineer,
56:1, 29-42, DOI: 10.1080/00194506.2014.883728
To link to this article: http://dx.doi.org/10.1080/00194506.2014.883728

Published online: 05 Feb 2014.

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INDIAN CHEMICAL ENGINEER 2014 Indian Institute of Chemical Engineers

Vol. 56 No. 1 March 2014, pp. 2942
Print ISSN: 0019-4506, Online ISSN: 0975-007X, http://dx.doi.org/10.1080/00194506.2014.883728

Optimization of Copper Adsorption by Soil of

Polluted Wasteland using Response Surface
Methodology
Arpita Ghosha and Papita Dasb*
a

Department of Earth and Environmental Studies, National Institute of Technology, Durgapur, India;
Department of Chemical Engineering, Jadavpur University, Kolkata, India

Abstract: Copper is one of the heavy metals, which are essential but toxic at higher concentrations.
High uptakes of copper may cause liver and kidney damage and even death. This study was performed
to investigate copper reduction using soil as an adsorbent. A multi-step response surface methodology
was applied for the maximum reduction of Cu(II) from aqueous solution to optimize the parameters
that had an effect on the adsorption studies. A two-level, three-factor (23) full factorial central composite
design (CCD) using Design Expert Version 7.0.0 (Stat Ease, USA) was used for the optimization of the
adsorption process parameters. From the CCD design it was observed that the optimum reduction of
copper was 96.22% at pH 5.50, 31.59 g l1 of adsorbent and 90 min contact time. The deviation between
the experimental and theoretical results was 0.42%.
Keywords: Copper,
Optimization.

Adsorption,

Soil,

Polluted

Wasteland,

Response

surface

methodology,

Introduction
Copper is one of the essential trace nutrients for living organisms. It is present in the
bloodstream, and in copper-based pigments and various enzymes. However, it can be toxic if
present in high concentrations. It may hamper marine life [1, 2] or result in soil microbial
pollution, and high copper uptakes may cause liver, kidney and brain damage and even death
[3, 4]. Wilsons disease and schizophrenia also occur with high copper uptakes [5].

* Author for Correspondence. Email: papitasaha@gmail.com

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Mostly copper is present in industrial effluents from the pulp, paper and plating
industries [6, 7]. The effective methods of copper (II) reduction from wastewaters include
precipitation, ion-exchange, electrolysis, reverse osmosis and adsorption using activated
carbon. These methods have high capital and operating costs as well as high energy
requirements, and also suffer from incomplete reduction. In addition, there are also
limitations concerning their use, especially for treating a large volume of dilute metal
concentrations [8].
New cost-effective technologies are required that can reduce copper concentration to
environmentally acceptable levels oriented to adsorption based on the metal binding
capacities of different low-cost adsorbents. The adsorption is a process in which solute is
removed from the aqueous phase through the contact of a solid adsorbent that has a special
affinity for that particular solute [9].
The main advantages of the adsorption process are its cost-effectiveness, easy availability,
minimization of disposal sludge volume and regeneration of metals from the adsorbents.
Different types of natural and artificial adsorbents have been studied by various researchers
for the reduction of heavy metals. Various agro-waste or plant-derived materials, such as rice
husk, wheat shell, cereal chaff, sawdust or pine bark, can be used to adsorb heavy metals
[1014].
The objective of the present study was to investigate the capacity of copper adsorption
using the wasteland soil of Dhapa in Kolkata. Kolkata is one of the four metropolitan cities
of India and is the capital of the state of West Bengal. The city is centred on latitude 22 34
North and longitude 88 24 East. Elevation ranges from 1.5 to 9.0 m above sea level.
Response surface methodology (RSM) is a combination of statistical and mathematical
techniques that is useful for improving and optimizing the process, process parameters and
determination of mutual interactions. The application of statistical methods for adsorption
process involves less treatment time, minimum costs and higher percentage yields [1517].
The objective of the present study was optimization of copper adsorption using wasteland soil
with RSM.

Materials and Methods

Soil Sample Collection and Characterization
Soil was collected from Dhapa, a solid waste disposal site in Kolkata. The characteristics of
the soil were studied and the results are listed in Table 1.
Preparation of Adsorbents
The collected soil sample was first air-dried in a hot air oven at 110C overnight (18 h) and
sieved through a 2 mm mesh sieve. The dried soil was kept in an air-tight glass bottle for the
adsorption experiments.
Chemicals
A stock solution of copper was prepared using copper sulphate pentahydrate (CuSO4.5H2O).
A 1000 mg l1 Cu(II) stock solution was prepared by diluting 3.93 g of CuSO4,5H2O
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Table 1. Characteristics of soil

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Parameters

Results

pH
Ammoniacal nitrogen (N)
Nitrate nitrogen
Potassium (K2O)
Phosphate (P2O5)
Copper
Chromium
Clay
Sand
Gravel
Cation exchange capacity (mequiv/100 g dry soil)
BrunauerEmmettTeller surface area
Average pore diameter
Micropore area
Density of soil

7.00
15 mg kg1
20 mg kg1
112 mg kg1
Nil
5.54 mg kg1
0.65 mg kg1
1%
20% (coarse, 9%; medium, 211%; fine, 2%)
30%
30.81
61 m2 g1
2.25 nm
75%
2.645 g cm3

(obtained from Merck, Germany) in 1 l distilled water. Using this stock solution, different
copper concentration solutions were prepared.
Adsorption Experiments
Aqueous solutions consisting of different concentrations of Cu solution and different values
of pH were prepared for the experiment. For pH adjustment 0.1 M HCl and 0.1 M NaOH
solutions were used. Copper solution was kept in a conical flask and adsorbents were added
in the required amount. The flasks were placed in rotary incubator shaker. The experiment
was conducted at 30C.
After predefined time intervals, the sample was collected and centrifuged at 6000 rpm for
10 min. Supernatant fractions were analysed for the remaining copper ions spectrophotometrically at 460 nm using sodium diethyl dithiocarbamate (obtained from Loba Chemicals,
India) as the complexing agent [18]. Copper reduction percentage by adsorption was obtained
by using the following formula:
Reduction %

C0  C1
 100
C0

where C0 is the initial copper concentration (mg l1) and C1 is the remaining copper
concentration.
Batch Experiments to Determine Range of Optimization Experiments
Initially batch experiments were performed to determine the experimental range of
optimization. Adsorption experiments were performed using the range 10100 mg l1 copper
solution, using adsorbent dose 540 g l1. From that batch of experiments, 89.38% copper
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Fig. 1. Copper reduction at different initial concentration of copper.

reduction was observed at 50 mg l1 copper concentration (Fig. 1). To optimize the

experimental conditions, a batch study was conducted using RSM.
Optimization Experiments
For optimization of the process parameters RSM was applied. Face-centred central
composite design (CCD) with three factors was applied in Design-Expert 7.0.0 with the
bounds of the three factors of initial pH 3.55.5, adsorbent weight 2040 g l1 and contact
time 4590 min. The copper concentration was fixed at 50 mg l1. A 23 full factorial CCD
using Design Expert Version 7.0.0 (Stat Ease, USA) was performed for the optimization of
the adsorption process variables.
The ranges and levels of variables investigated in the research are given in Table 2. The
levels of the parameters varied from 1 to +1. Zero levels of the parameters indicate the
centre values and indicates axial levels (, +). At positive axial point (+), the percentage
reduction was 99.06 and at negative axial point the percentage reduction was 74.9. The
highest value of pH was 5.5 and lowest was 3.5. Similarly, the adsorbent dose was in the
range of 2040 g l1 and time was in the range of 4590 min.
The percentage reduction of copper was taken as the response of the system. The CCD is
an effective design that is ideal for sequential experimentation and allows a reasonable
Table 2. Experimental range and levels of independent process variables
Range and levels (coded)
Independent variables
pH (A)
Adsorbent dose, g l1 (B)
Time, min (C)

+1

2.82
13.18
29.66

3.50
20.00
45.00

4.50
30.00
67.50

5.50
40.00
90.00

6.18
46.82
105.34

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amount of information for testing lack of fit while not involving an unusually large number of
design points. The quadratic equation model for predicting the optimal point was expressed
according to Equation (2):
Y b0

K
X

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i1

bi Xi

K
X
i1

bii Xi2

X X
i1 ji1

bij Xi Xj 2

where Y is the predicted response, Xi and Xj refer to the independent variables, 0, i, ii and
ij are the regression coefficients and e is the statistical error. The optimum values of the
selected parameters were found by solving the regression equation and studying the contour
plots.
Statistical Analysis
The effects of adsorption parameters, namely, pH of the solution, weight of the adsorbents
and contact time on percentage reduction of copper were studied using statistically designed
experiments and optimization by RSM. Three factors were studied and their low and high
levels are given in Table 2. Percentage reduction of copper was studied with a standard RSM
design called the CCD.
Table 3. 23 factorial experimental setup and percent reduction response
Run
1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20

pH (A)

Adsorbent dose (B) (g l1)

Time (C) (min)

Response (percentage reduction)

5.50
4.50
2.82
4.50
4.50
3.50
3.50
4.50
3.50
3.50
4.50
5.50
5.50
4.50
4.50
4.50
4.50
6.18
4.50
5.50

40
46.82
30
30
30
40
20
30
40
20
30
20
40
30
30
30
30
30
13.18
20

90
67.50
67.50
29.66
105.34
90
90
67.50
45
45.00
67.50
90.00
45.00
67.50
67.50
67.50
67.50
67.50
67.50
45.00

89.8
60
74.9
78.5
88
70.76
65
80
70.8
60.5
80
83.86
83
80.8
80.5
80.8
80
99.06
45.8
72.06

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A total of 20 experiments were conducted according to 23 full factorial CCDs consisting

of factorial points (coded to the usual 1 notation), axial points () and six replicates at the
centre points (0). Each of the experiments was conducted in duplicate, as shown in Table 3.
The equations were validated by the statistical tests called the ANOVA (analysis-ofvariance) to determine the implication of each term in the equations fitted and to judge the
goodness of fit in each case. Response surfaces were drawn for the experimental results
obtained from the effect of different variables on the percentage reduction of copper in order
to determine the individual and cumulative effects of these variables and the mutual
interactions between them.

Results and Discussion

The results of each experiment performed are given in Table 3. The most significant response
(96.22%) was obtained at pH 5.50, 31.59 g l1 of adsorbent and 90 min of contact time.
From the ANOVA study, it was observed that the lack of fit F-value of 2.82 implies
that lack of fit was not significant relative to the pure error. Non-significant lack of fit was
signified for the study [16]. In this case, the non-significant lack of fit (>0.05) showed that the
quadratic model was valid for this study [19, 20]. The model F-value of 1349.16 implies that
the model was significant (Table 5). There was only a 0.01% chance that a model F-value
Table 4. Regression analysis by using central composite design
Model term
A
B
C
AB
AC
BC
A2
B2
C2

Coefficient estimate

Standard error

F-Value

p-Value

Remarks

7.49
4.16
2.86
0.10
1.77
1.19
2.48
9.57
1.16

0.13
0.13
0.13
0.17
0.17
0.17
0.12
0.12
0.12

3459.50
1067.77
504.00
0.38
112.93
51.42
400.67
5957.19
88.00

<0.0001
<0.0001
<0.0001
0.5497
<0.0001
<0.0001
<0.0001
<0.0001
<0.0001

Significant
Significant
Significant
Significant
Significant
Significant
Significant
Significant

R2, 0.999; adjusted R2, 0.998; predicted R2, 0.995.

Table 5. Analysis of variance for the response surface quadratic model for copper reduction
Source
Model
Residual
Lack of fit
Pure error
Core total

Sum of squares

Degree of freedom (d.f.)

Mean square

F-Value

Probablity > F

2688.83
2.21
1.64
0.58
2691.09

9
10
5
5
19

298.76
0.22
0.33
0.12

1349.16

<0.0001

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0.14

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Optimization of Copper Adsorption by Soil

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could occur owing to noise. The model F-value (1349.16) with a low probablity (p < 0.0001)
showed that the model was significant. The goodness of fit of the model was also evidenced
by the corelation coefficient (R2; Table 4). Moreover, the R2 value of 0.999 implied that more
than 99% of the data deviation could be explained by the developed quadratic model and the
predicted R2 values were in agreement with adjusted R2, which means all the terms depicted in
the model were significant. Only 0.62% (coefficient of variation) of the total variations was
not explained by the optimization model, which means that all the terms depicted in the
model were significant.
Effect of Initial Solution pH and Adsorbent Dose
The effect of initial solution of pH and adsorbent dose on adsorption can be predicted from
the contour plot shown in Fig. 2. The possible goals were: within range (for three independent
variables pH, adsorbent dose and time) and maximum (for responses only) and set to an exact
value (factors only). At the lowest level of pH (3.5) and adsorbent dose (20 g.), the percentage
reduction was very low, that is, 60.5%. At the highest level of pH (5.5) and adsorbent dose
(40 g.), the percentage reduction was 89.8%. From the contour plot it can be observed that
copper reduction percentage increased with increase in pH and adsorbent dose. Up to a
certain limit adsorption was increased by increasing adsorbent dose. After that it reached the
equilibrium. From this contour plot, a maximal reduction efficiency of 96.22% was achieved
using 31.59 g l1 adsorbent dose at pH 5.50, when time was kept fixed at 90 min. This

Fig. 2. The contour plot shows the relationship between pH and the adsorbent dose with R1.

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signified that, at a higher pH, the percentage reduction increased. However, with increasing
adsorbent dose, it increased to 31.59 g. After that it went into equilibrium owing to a lack of
free sorption sites.
Solution pH affected the chemistry of the copper ions, the activity of operational groups
on the soil surface and the competition of copper ions with hydrogen ions for the binding sites
[21, 22]. The functional groups on the soil surface were protonated at lower pH value, that is,
3.5, thereby restricting the approach of positively charged copper Cu (II) cations to the
surface of the adsorbent. In the pH range of 3.55.5, these soil particles were negatively
charged and the sorption process of copper then continued because of electrostatic attraction
between the negatively charged adsorbent surface and the positively charged copper
cations [23].
Effect of Adsorbent Dose and Time
The combined effect of adsorbent dose and time on copper reduction was shown in the
contour plot of Fig. 3. It was observed that copper reduction increased with increasing time
as well as adsorbent dose. By increasing adsorbent dose there was an increment of adsorbent
surface area and sorption sites. At the lowest levels of adsorbent dose (20 g l1) and time
(45 min), the percentage reduction was only 60.5%. At the highest level of adsorbent dose
(40 g l1) and time (90 min), the percentage reduction was 89.8%. From this contour plot, a
maximal reduction efficiency of 96.222% was achieved using 31.59 g l1 adsorbent dose at
90 min when pH was kept fixed at 5.50. This signified that, up to a certain level of increment
of time and adsorbent dose, the percentage reduction increased. Then it decreased as

Fig. 3. The contour plot shows the relationship between adsorbent dose and time with R1.

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intermolecular space between adsorbents became smaller and that led to the aggregation of
the sorption sites.
Effect of Initial Solution pH and Contact Time
The combined effect of initial solution pH and contact time on copper reduction is shown in
the contour plot of Fig. 4. It was observed that percentage copper reduction increased with
increasing pH as well as time. The maximum copper reduction 96.22% was obtained from pH
5.50 and contact time 90 min, when copper solution concentration was fixed at 50 mg/L. It
was evident from the contour plots that both of the independent variables had a strong
influence on the copper biosorption process. From this contour plot, a maximal reduction
efficiency of 96.22% was achieved at initial pH 5.50, weight of the adsorbent 31.59 g l1 and
contact time 90.00 min. At high pH, copper reduction increased, signifying that the soil is
more efficient for the adsorption in high pH.
Optimization Using Desirability Functions
In numerical optimization, the desired goal for each factor and response from the menu was
chosen. The possible goals were: maximize, minimize, target, within range, none (for
responses only) and set to an exact value (factors only). A minimum and a maximum level
had to be provided for each parameter admitted in this study. There could be two or more

Fig. 4. The contour plot shows the relationship between pH and the time with R1.

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Fig. 5. Desirability ramp for optimization of three goals, namely initial solution of pH, adsorbent dose
and time of maximum reduction of copper (R1).

maxima because of curvature in the response surfaces and their combination in the
desirability function. Starting from various points in the design improved the chances of
detecting the best local maximum [22, 23]. A multiple response method was applied for
optimization of any combination of four goals, namely, initial solution pH, adsorbent dose,
contact time and percentage reduction of copper. The numerical optimization found a point
that maximized the desirability function. Level of initial solution pH (3.55.5), adsorbent
dose (2040 g l1) and contact time (4590 min) were in the range and maximum percentage
reduction of copper (96.22) was set. Figure 5 shows a ramp of desirability that was generated
from six optimum points via numerical optimization. These optimized parameters can be
used in a fixed bed operation to achieve the higher percentage removal of copper in less time
and as a result the number of experiments needed to achieve a higher percentage removal of
copper will be decreased.
Comparison between Theoretical and Experimental Data
Figure 6 shows the comparison between the experimental and predicted data and from the
figure. There was very little deviation between experimental and RSM simulated results. The
theoretically optimum conditions for copper adsorption were pH 5.50, adsorbent dose 31.59 g
and contact time 90.00 min, and the copper reduction was 96.22%. The experimental result
was 96.6158% and the deviation from experimental and theoretical was 0.42%.
An empirical relationship between the response (R1) and the independent variables (pH,
adsorbent dose, time) are expressed by the following quadratic model:
R1 14:58  20:45A 6:454B  0:38C 0:01AB 0:08AC  0:01BC 2:48A2  0:10B2
3
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Fig. 6. Comparison of the predicted and experimental results.

where A is the pH of the solution, B is the weight of adsorbent dose (g l1) and C is the
time (min).
SEM Analysis of Soil
Scanning electron microscopy analysis of the soil sample was performed before and after
adsorption by the soil particles (Fig. 7). It was observed that surface of the adsorbent became
quite smooth after copper adsorption by the soil. Primarily, small tiny particles (two or three)
of soil were mounted on a round stainless steel stub with double-sided sticky tape and coated
with a thin layer of gold (IB2-Ion coating) in a high vacuum condition. The scanning electron
microscopy was recorded using S 530, Hitachi scanning electron microscope at an electron
acceleration voltage of 25 kV.

Conclusion
The objective of the present study was to investigate the combined effect of various process
parameters on copper reduction using response surface methodology. It was observed from
the experimental results that the initial solution pH, adsorbent dose and time significantly
influenced the copper reduction efficiency. A desirability function in RSM was obtained from
optimization conditions for the maximum reduction efficiency of copper. Based on the
analysis of statistics, the optimum conditions were obtained as pH 5.50, weight of the
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Fig. 7. Scanning electron micrograph of soil: (a) before and (b) after adsorption.

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adsorbent 31.59 g l1 and contact time 90.00 min, and the copper reduction at this condition
was 96.22%.
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INDIAN CHEMICAL ENGINEER

Vol. 56 No. 1 March 2014