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Karbala International Journal of Modern Science 2 (2016) 20e28
http://www.journals.elsevier.com/karbala-international-journal-of-modern-science/

Optimization of adsorption conditions using central composite


design for the removal of copper (II) and lead (II) by defatted
papaya seed
Zaharaddeen N. Garba a,b,*, Idris Bello c, Ahmad Galadima d, Aisha Y. Lawal e
a

School of Chemical Sciences, Universiti Sains Malaysia, 11800, Penang, Malaysia


Department of Chemistry, Ahmadu Bello University, P.M.B. 1044, Zaria, Nigeria
c
Department of Pharmacology, School of Pharmaceutical Sciences, Universiti Sains Malaysia, 11800, Penang, Malaysia
d
Department of Chemistry, Federal University, P.M.B. 1001, Gusau, Nigeria
e
Department of Chemistry, Federal College of Education, Zaria, Nigeria
b

Received 26 October 2015; revised 12 November 2015; accepted 3 December 2015


Available online 30 December 2015

Abstract
The prime conditions for the removal of Cu (II) and Pb (II) onto defatted papaya seeds (DPS) from aqueous solution were
studied. The effects of three adsorption variables (adsorbent dosage, shaking speed as well as initial concentrations) were investigated using central composite design (CCD) which is a subset of response surface methodology (RSM). Quadratic models were
developed for both Cu (II) and Pb (II) percentage removals. The optimum adsorption conditions obtained were adsorbent dosage of
0.30 g, shaking speed of 180 rpm as well as initial concentration of 150 mg/L with desirability of 0.987. The predicted and
experimental values obtained were 96.65% and 97.55% for Cu (II) as well as 98.07 and 99.96% for Pb (II), showing good agreement
between the experimental values and those predicted from the models with relatively small errors which were only 0.89 and 1.89,
respectively. Langmuir isotherm model was found to be the best fit for the equilibrium adsorption data of both Cu (II) and Pb (II) on
DPS giving rise to monolayer adsorption capacities of 17.29 and 53.02 mg/g respectively.
2015 The Authors. Production and hosting by Elsevier B.V. on behalf of University of Kerbala. This is an open access article
under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
Keywords: Defatted papaya seed; Adsorption; Central composite design; Response surface methodology; Cu (II) and Pb (II)

1. Introduction
The presence of heavy metals in waste stream and
ground water pose a very serious environmental
concern since these metal ions are reported to be toxic
* Corresponding author. School of Chemical Sciences, Universiti
Sains Malaysia, 11800, Penang, Malaysia. Tel.: 60 1126116051;
fax: 60 46574854.
E-mail address: dinigetso2000@gmail.com (Z.N. Garba).
Peer review under responsibility of University of Kerbala.

to human beings as well as other living organisms


[1,2], causing serious morbidity and mortality [3]
especially if their concentration is more than the
accepted limit [4]. Their main sources include wastewater discharged from hospitals [5], metal plating and
alloy manufacturing [6e9]. Lead (Pb) serves no useful
purpose in the human body, but its presence in the
body has serious consequences for the health of children. At high levels of exposure, lead attacks the brain
and central nervous system to cause coma, convulsions

http://dx.doi.org/10.1016/j.kijoms.2015.12.002
2405-609X/ 2015 The Authors. Production and hosting by Elsevier B.V. on behalf of University of Kerbala. This is an open access article under
the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

Z.N. Garba et al. / Karbala International Journal of Modern Science 2 (2016) 20e28

and even death with hepatic and occasionally renal


changes the most common effects of copper (Cu)
reported.
Biosorption process through utilization of biomass/
biosorbents in the removal of heavy metal ions from
aqueous solution is one of the most promising alternatives in substituting conventional methods like precipitation, membrane filtration, electrolyte or liquid
extraction, electrodialysis and reversed osmosis [10].
Sorption methods are considered flexible and easy to
operate with much less sludge disposal problems
[11,12]. Various adsorbents such as halloysite nanotubes [13,14] carbon nanotubes [15], activated carbons
from agricultural waste materials [16e19], activated
clay [20] as well as biosorbents [21e23] have been
reported in the literature for the removal of contaminants from waste water; however, new adsorbents with
local availability as well as economic suitability are
still needed.
Carica papaya L. (commonly referred as pawpaw)
is a known herbaceous plant commonly found in subhumid tropical regions of Africa, South America and
Central America. Nigeria is one country where this
plant is highly cultivated. The plant bears edible and
highly nutritional fruit which may be yellowish green,
yellow or orange in colour when ripe. The seeds are
numerous, black at maturity and rich in oil, lipids and
proteins which makes it crucial that the seeds are

21

defatted before use as biosorbent [24]. Response surface methodology (RSM) is a mathematical model that
was reported to be a very useful tool in optimizing the
preparation conditions of activated carbons [25] but not
much was reported on its application in optimizing
adsorption process parameters.
The continuation of our interest in exploring safer
and cheaper alternative methods for the treatment of
wastewater and textile effluents [17,18,26] lead us to
report the optimization of the paramount parameters
for an effective adsorption of Cu (II) and Pb (II) onto
DPS from aqueous solution using CCD. CCD was
chosen to evaluate the interaction of the crucial
adsorption parameters such as adsorbent dosage,
shaking speed as well as initial concentrations.
2. Materials and methods
2.1. Preparation of adsorbent material

Fresh carica papaya seeds, collected from open


markets in Nigeria, were sun dried for 7 days after
which they were crushed using mortar and pestle and
defatted using the soxhlet extraction method with
hexane as solvent [27]. The air dried sample was then
called defatted carica papaya seeds (DPS). All the
chemicals used in this work were of analytical reagent
grade purchased from SigmaeAldrich and used

Table 1
Experimental design matrix using central composite design.
Run

1
2
3
4
5
6
7
8
9
10
11
12
13
14
15
16
17
18
19
20

Level

1
1
1
1
1
1
1
1
1.682
1.682
0
0
0
0
0
0
0
0
0
0

1
1
1
1
1
1
1
1
0
0
1.682
1.682
0
0
0
0
0
0
0
0

1
1
1
1
1
1
1
1
0
0
0
0
1.682
1.682
0
0
0
0
0
0

Ni (II) and Cd (II) adsorption variables

Cu (II) removal

Pb (II) removal

Adsorbent
dosage (g)

Shaking speed
(rpm)

Initial concentration
(mg/L)

YCu (%)

YPb (%)

0.30
0.80
0.30
0.80
0.30
0.80
0.30
0.80
0.10
1.00
0.60
0.60
0.60
0.60
0.60
0.60
0.60
0.60
0.60
0.60

120
120
180
180
120
120
180
180
150
150
100
200
150
150
150
150
150
150
150
150

56
56
56
56
149
149
149
149
103
103
103
103
25
180
103
103
103
103
103
103

55.43
63.27
93.62
44.01
54.33
40.00
86.44
54.54
70.34
34.65
43.27
74.82
89.44
98.24
69.44
68.55
70.58
67.77
68.43
69.94

54.19
78.03
89.32
45.66
55.73
45.78
80.64
90.65
57.26
51.57
46.59
96.82
44.33
88.82
38.05
37.10
38.19
37.76
38.29
36.46

22

Z.N. Garba et al. / Karbala International Journal of Modern Science 2 (2016) 20e28

Table 2
Independent variables and their coded levels using central composite
design.

Ce
1
Ce

0
KL $Q0a
qe
Qa

Variables

Q0a (mg/g) and KL (L/mg) are Langmuir constants


related to adsorption capacity and rate of adsorption,
respectively.
The essential characteristics of Langmuir model can
be described by dimensionless separation factor, RL,
given as:

Code Unit Coded variable levels

Adsorbent dosage x1
Shaking speed
x2
Initial concentration x3

a 1
0
1
g
0.10
0.30
0.60
0.80
rpm 100 120
150
180
mg/L 25
56
103
149

a
1.00
200
180

without any further purification. All the glasswares


used were washed and rinsed several times. Standard
solutions of Cu (II) and Pb (II) were prepared from
their nitrate salts. The metal solutions were prepared
from stock solutions containing 1000 mg/L of Cu (II)
and Pb (II), respectively.
2.2. Metal ions adsorption experiments

Adsorption experiments were carried out using a


batch procedure in order to examine and evaluate
variables significance on the adsorption efficiencies
(%) of Cu (II) and Pb (II) by shaking 100 ml of the
metal ions solutions in a 250-ml Erlenmeyer flask according to the adsorbent dosage, shaking speed as well
as initial concentrations as shown in Table 1. The
coded points and their corresponding values are presented in Table 2. The aqueous samples were analysed
using an inductively coupled plasma-atomic emission
spectrometer. The adsorption efficiencies were evaluated using the following equation:
Adsorption efficiency %

Co  Ce
 100
Co

where Co and Ce are the liquid-phase concentrations at initial


and equilibrium states (mg/L), respectively.

The equilibrium amounts qe (mg/g) adsorbed per


unit mass of adsorbent was evaluated using equation
(2):
qe

Co  Ce V
W

where qe (mg/g) is the equilibrium amount of the metal ions


adsorbed per unit mass of DPS; V (L) is the volume of the
solution and W (g) is the mass of DPS used.
2.3. Adsorption isotherms

The equilibrium characteristics of this adsorption


study were described through Langmuir and Freundlich isotherm models. Langmuir model presumes a
monolayer adsorption onto a surface containing finite
number of adsorption sites [28]. Its linear form is given
as:

RL

1
1 KL Co

where Co is the highest initial solute concentration. RL values


indicate whether the adsorption is unfavourable (RL > 1),
linear (RL 1), favourable (0 < RL < 1), or irreversible
(RL 0).

Freundlich model on the other hand assumes heterogeneous surface energies. Its linear form is given by
the following equation [29]:
1
logqe logKF logCe
n

where KF and n are Freundlich constants. Generally, n > 1


suggests favourable adsorption. It has also been used to
evaluate whether the adsorption process is physical (n > 1),
chemical (n < 1) or linear (n 1) [30].
2.4. Design of experiments using response surface
methodology

In this work, a subset of response surface methodology (RSM) known as central composite design
(CCD) was applied to study the Cu (II) and Pb (II)
adsorption parameters (adsorbent dosage, shaking
speed as well as initial concentrations). The detailed
CCD process was described in our previously published paper [17]. Design expert statistical software
(version 6.0.8 Stat Ease, Inc., Minneapolis, MN 55413,
USA) was used for the model fitting and significance
for the Cu (II) and Pb (II) adsorption efficiencies.
3. Results and discussion
3.1. Development of regression model equations
using CCD
The design matrix incorporating the preparation
variables, their ranges and the responses which are
percentage removal of both Cu (II) and Pb (II) (YCu
and YPb) respectively were displayed in Table 1. The
Cu (II) and Pb (II) percentage removals ranged between 34.65 and 98.24% and 36.46.17e96.82%
respectively. For the sake of comparing and correlating

Z.N. Garba et al. / Karbala International Journal of Modern Science 2 (2016) 20e28

the responses, CCD was applied for the development


of the polynomial regression equations which were all
quadratic expressions as suggested by the software.
The model expression was selected in accordance with
sequential model sum of square that is based on the
polynomial's highest order where the model was not
aliased and the additional terms were significant
[19,25,31].
The correlation between predicted and experimental
data was glaring as indicated by the model's R2 values
of 0.9238 for Cu (II) and 0.8132 for Pb (II) which were
within desirability range [31]. The final empirical
model's equations for percentage removal of both Cu
(II) (YCu) and Pb (II) (YPb) responses are given as
equations (6) and (7) respectively.

23

conducted to determine the experimental error and the


reproducibility of the data.
3.2. Statistical analysis

The synergetic and antagonistic effects of the


respective variables were informed by the positive and
negative signs before the terms [17]. The appearance of
a single variable in a term signified a uni-factor effect;
two variables imply a double factor effect and a second
order term of variable appearance indicate the
quadratic effect [32]. Quadratic model was used as
selected by the software for the two responses. The six
replicate variables at the centre points, run 15e20 were

The adequacy of the models was further justified


through analysis of variance (ANOVA). Table 3
described the ANOVA for the quadratic model for Cu
(II) percentage removal showing sum of squares and
mean square of each factor, F-value as well as
Prob. > F values.
ANOVA validated the importance and how adequate
the models are. From Table 3, dividing the sum of the
squares of each of the variation sources, the model and
the error variance by the respective degrees of freedom
gives the mean square values. The model terms with
value of Prob. > F less than 0.05 are considered as
significant [32]. With respect to Cu (II) percentage
removal as can be seen from Table 3, the model Fvalue is 13.46 and Prob. > F value of 0.0002, justifying
the model's significance. The significant model terms
were x1; x2 ; x21 , x23 and x1 x2 with x3 ; x22 , x1 x3 and
x2 x3 insignificant to the response.
From Table 4, F-value of 4.84 as well as Prob. > F
of 0.0108 indicated that the model was also significant.
In this case only x2 ; x22 and x23 were the significant
model terms with the insignificant terms being
x1 ; x3; x21 ; x1 x2 ; x1 x3 and x2 x3 . From the statistical
results obtained, it can be seen that the models were
suitable in predicting both Cu (II) and Pb (II) removals
within the range of the studied variables. Additionally,
Figs. 1 and 2 show the predicted values versus the
experimental values for Cu (II) and Pb (II) removals
respectively, portraying that the developed models
successfully captured the relation between the
adsorption process variables to the responses.

Table 3
The ANOVA for response surface quadratic model of Cu (II) by DPS.

Table 4
The ANOVA for response surface quadratic model of Pb (II) by DPS.

YCu 69:34  10:84x1 8:69x2  0:46x3  7:35x21


e 5:03x22 7:27x23 e 9:38x1 x2 e 0:56x1 x3
3:46x2 x3
6
YPb 37:59e 2:15x1 11:51x2 5:90x3 6:27x21
12:40x22 10:58x23 e 5:94x1 x2 2:48x1 x3
8:38x2 x3
7

Source

Sum of
squares

Degree of
freedom

Mean
square

F value

Prob > F

Source

Sum of
squares

Degree of
freedom

Mean
square

F value

Prob > F

Model
x1
x2
x3
x21
x22
x23
x1 x2
x1 x3
x2 x3
Residual

5519.81
1604.39
1030.66
2.83
777.91
364.80
761.81
703.50
2.49
96.05
455.52

9
1
1
1
1
1
1
1
1
1
10

613.31
1604.39
1030.66
2.83
777.91
364.80
761.81
703.50
2.49
96.05
45.55

13.46
35.22
22.63
0.062
17.08
8.01
16.72
15.44
0.055
2.11
e

0.0002
0.0001
0.0008
0.8081
0.0020
0.0179
0.0022
0.0028
0.8200
0.1771
e

Model
x1
x2
x3
x21
x22
x23
x1 x2
x1 x3
x2 x3
Residual

6989.09
62.99
1809.13
474.79
567.20
2217.40
1614.20
282.51
49.40
561.46
1605.88

9
1
1
1
1
1
1
1
1
1
10

776.57
62.99
1809.13
474.79
567.20
2217.40
1614.20
282.51
49.40
561.46
160.59

4.84
0.39
11.27
2.96
3.53
13.81
10.05
1.76
0.31
3.50
e

0.0108
0.5452
0.0073
0.1163
0.0896
0.0040
0.0100
0.2142
0.5913
0.0910
e

24

Z.N. Garba et al. / Karbala International Journal of Modern Science 2 (2016) 20e28

Fig. 1. Relationship between predicted and experimental data for Cu


(II) removal.

be observed with increase in shaking speed from


120 rpm to 180 rpm as well as decrease in adsorbent
dosage from about 0.8 to 0.3 g. Increasing the shaking
speed escalate the mobility of the adsorbate particles on
the adsorbent's surface thus increasing the percentage
removal.
From Table 4, the three variables (adsorbent
dosage, shaking speed and initial concentrations) can
also be seen to show lopsided impact on the Pb (II)
percentage removal by DPS. Adsorbent dosage had the
least effect based on its F-value which was smaller
(0.39) and also its variation did not have a significant
effect on the process. The individual factors of shaking
speed and initial concentration as well as their interactions had the most significant effect on the Pb (II)
adsorption onto DPS as can be seen by the F-values of
11.27, 2.96 as well as 3.50 respectively. The threedimensional response surfaces which were constructed to show the most significant two variables
(shaking speed and initial concentration) on the Pb (II)
removal at constant adsorbent dosage (0.60 g) is
shown in Fig. 4.
3.4. Process optimization

Fig. 2. Relationship between predicted and experimental data for Pb


(II) removal.

3.3. Effects of individual variables and their


interactions
It can be deduced from Table 3 that the individual
effects inflicted on Cu (II) removal by adsorbent dosage
and shaking speed were more superior than initial
concentration based on the F-values of 35.22 (adsorbent
dosage), 22.63 (shaking speed) and 0.062 (initial concentration). The quadratic effects of adsorbent dosage
(F-value of 17.08) and initial concentration (16.72)
were almost similar and more pronounced than that of
shaking speed (8.01). Only the interaction effect of
adsorbent dosage-shaking speed was meaningful having
F-value of 15.44. Interaction effects of adsorbent
dosage-initial concentration and that of shaking speedinitial concentration show very low F-values of 0.055
and 2.11 respectively. Fig. 3 shows the threedimensional response surfaces, the combined effect of
adsorbent dosage and shaking speed for Cu (II) removal
at constant initial concentration (103 mg/L). From
Fig. 3, an upsurge in the percentage Cu (II) removal can

The optimization of Cu (II) and Pb (II) adsorption


onto CPS was carried out by using design-expert
software (Stat-Ease, Inc., Minneapolis, MN 55413,
USA). In the optimization analysis, the target criterion
was set as maximum values for the two responses. The
optimum adsorption conditions obtained were adsorbent dosage of 0.30 g, shaking speed of 180 rpm as
well as initial concentration of 150 mg/L with desirability of 0.987, as presented in Table 5. The predicted
and experimental values obtained at optimum conditions were 96.65% and 97.55% for Cu (II) as well as
98.07 and 99.96% for Pb (II), showing good agreement
between the experimental values and those predicted
from the models, with relatively small errors which
were only 0.89 and 1.89, respectively.
3.5. Adsorption isotherm
Chi square (c2) was incorporated to help in selecting the best fitted model for the experimental data,
since correlation coefficient (R2) may not justify the
basis for selection of the best adsorption model
because it only represent the fit between experimental
data and linearized forms of the isotherm equations
while chi square (c2) represents the fit between the
experimental and predicted values of the adsorption
capacity. The lower the c2 value, the better the fit.

Z.N. Garba et al. / Karbala International Journal of Modern Science 2 (2016) 20e28

25

Fig. 3. The combined effect of shaking speed and adsorbent dosage on the removal of Cu (II) with initial concentration fixed at zero level
(Co 103 mg/L).

Fig. 4. The combined effect of initial concentration and shaking speed on the removal of Pb (II) with adsorbent dosage fixed at zero level
(W 0.6 g).

Table 6 summarizes all the constants, R2 and c2


values obtained from the isotherm models applied for
the two metal ions adsorption on DPS. The Q0a values
obtained for Cu (II) and Pb (II) from the linear

Langmuir plot (Fig. 5) were 17.29 and 53.02 mg/g


respectively. According to the fitting results listed in
Table 5, Langmuir isotherm model appeared to be
much more applicable than the Freundlich having the

26

Z.N. Garba et al. / Karbala International Journal of Modern Science 2 (2016) 20e28

Table 5
The model validation.
Model
desirability

Adsorbent
dosage, x1 (g)

Shaking
speed, x2 (rpm)

Initial
concentration,
x3 (mg/L)

Cu (II) removal (%)


Experimental

Predicted

Error

Experimental

Predicted

Error

0.987

0.30

180

150

97.54

96.65

0.89

99.96

98.07

1.89

Table 6
Langmuir and Freundlich isotherm model parameters for Cu (II) and
Pb (II) adsorption onto DPS at 30  C.
Isotherms

Parameters

Cu (II)

Pb (II)

Langmuir

Q0a

17.29
0.265
0.073
0.9923
10.713
1.951
2.315
0.8996
13.361

53.02
0.238
0.061
0.9779
7.252
8.382
3.080
0.8080
19.311

Freundlich

(mg/g)
KL (L/mg)
RL
R2
c2
KF (mg/g (L/mg)
n
R2
c2

Pb (II) removal (%)

highest R2 as well as lowest c2 values. The fitness of


the Langmuir model to the adsorption process connotes
that the metal ion molecules from bulk solution were
adsorbed on specific monolayer which is homogeneous
in nature. As can also be seen from Table 4, all the RL
values lies between 0 and 1 which confirms the
adsorption processes to be favourable under the studied
conditions. The n values obtained from the Freundlich
plot (Fig. 6) were found to be greater than unity for the
adsorbates, further indicating favourable adsorption
conditions as well as a physical adsorption processes
for the two metal ions in aqueous solution. The KF
values showed that DPS has higher adsorption capacity
for Pb (II) (8.382) compared to Cu (II) (1.951). Larger
values of KF and n indicated that the Pb (II) has higher
affinity towards the adsorbent [10].
The monolayer adsorption capacity (Q0a ) values of
17.29 mg/g for Cu (II) and 53.02 mg/g for Pb (II)
observed in this study compared well with some other
adsorbents reported from literature as shown in Table
7.
4. Conclusion

Fig. 5. Langmuir isotherm plot for Cu (II) and Pb (II) adsorption on


DPS.

Three adsorption parameters (adsorbent dosage,


shaking speed as well as initial concentrations) were
optimized with the aid of CCD for the removal of Cu
(II) and Pb (II) metal ions onto DPS with their percentage removals (YCu and YPb) as the analysis responses. Based on the data analysis obtained, the
individual effects of adsorbent dosage and shaking

Table 7
Comparison of adsorption capacity of metal ions onto different
adsorbents.

Fig. 6. Freundlich isotherm plot for Cu (II) and Pb (II) adsorption on


DPS.

Adsorbates

Adsorbents

Q0a (mg/g)

References

Cu (II)
Pb (II)
Cu (II)
Cu (II)
Pb (II)
Pb (II)
Ni (II)
Ni (II)

Defatted papaya seed


Defatted papaya seed
Polyflavonoid tannins
Olive stone activated carbon
Polyflavonoid tannins
Olive stone activated carbon
Dolomite powder
Tomato leaf powder

17.29
53.02
8.78
17.83
31.32
22.37
5.41
58.82

This work
This work
[10]
[33]
[10]
[33]
[12]
[22]

Z.N. Garba et al. / Karbala International Journal of Modern Science 2 (2016) 20e28

speed on Cu (II) removal were more superior than


initial concentration while shaking speed and initial
concentration individual effects as well as their interactions were more significant with respect to Pb (II)
removal. Highest removal percentage of the adsorbates
was obtained at the optimum conditions of adsorbent
dosage (0.30 g), shaking speed (180) rpm and initial
concentration (150 mg/L) with desirability of 0.987.
Equilibrium data analysed reveal Langmuir isotherm to
be the best fitted model.
Conflict of interest
The authors report no conflict of interest.

[11]

[12]

[13]

[14]

[15]

Acknowledgement
[16]

Zaharaddeen N. Garba would like to express his


gratitude to the Tertiary Education Trust Fund and
Ahmadu Bello University, Zaria, Nigeria for the study
fellowship offered to him.
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