Volume 5, Issue 8, August – 2020 International Journal of Innovative Science and Research Technology

ISSN No:-2456-2165

Application of Central Composite Design to the Photo

Fenton Degradation of Methyl Orange Azo Dye
Using Fe-Activated Carbon Catalyst
Abubakar Muhammad Ahmed Lawal Mashi
Department of Pure and Industrial Chemistry Department of Pure and Industrial Chemistry
Umaru Musa Yar’adua University Umaru Musa Yar’adua University
Katsina, Nigeria Katsina, Nigeria

Abstract:- Photo-fenton oxidation technique is one of reported to be loaded with Fenton catalyst to give more
the emerging oxidation processes explored in treatment effective oxidation process [5]. In the photo-Fenton-like
of organic pollutants in aqueous solutions. This research process, the combination of Fe3+ with Activated carbon is an
is focused on utilization of Fe(II) loaded activated alternative process that can be operated in an effective, easy
carbon and H2O2(aq) in a photofenton process to to control and cost-efficient manner [6]. This offers an
generate hydroxyl radicals that mineralize methyl interesting advantage for its application on an industrial
orange dyes. Samples of activated carbon were treated scale; that is, the supported photocatalysts can be reused. As
with Fe(NO3)2(aq) and characterized using SEM, pHZPC, investigated in previous works, the reuse of supported
specific surface area and boehm’s titration. The catalysts is in line with the synergistic effect of the
degradation of methyl orange by the iron loaded adsorptive properties of catalyst support [7].
activated carbon (Fe-Ac), via photo-Fenton process, was
investigated in lab-scale defined by experimental design. Mutagenic azo dyes such as methyl orange (MO) can
Central composite design (CCD) was used to evaluate accumulate in bodies of water and sediments to a level
the effects of the five independent variables considered considered significantly toxic to the environment. A
for the optimization of the oxidative process: time, Fe- research performed by Umbuzeiro et al [8] in the
Ac dose, methyl orange concentration, pH and H2O2 Salmonella/Microsome test, showed a low to moderate
concentrations. In the optimization, the correlation mutagenic activity in Cristais River (Cajamar/SP), due to
coefficients (R2) for the quadratic model was 0.9941. the presence of azo dyes, nitroaromatic compounds and
Optimum reaction conditions were obtained at pH = 3, aromatic amines. The study detected the presence of dyes in
catalyst dose = 0.1 mg/100ml, H2O2 = 0.62ml, methyl all the samples collected (effluent of the dyeing industry,
orange concentration = 5mg/l and time = 30 minutes. raw water and water treatment station), and associated the
mutagenicity of these samples mainly of the raw water with
Keywords:- Photofenton, Photodegradation, Methyl the presence of dyes and colorless polycyclic nitroaromatic
Orange. compounds, possibly generated during the treatment of the
effluent. Oliviera [9] also showed the presence of
I. INTRODUCTION components of the black commercial dye (BDCP) and
aromatic amines in the raw and treated effluents discharged
Removal of dyes from wastewater is one of the main by a dyeing industry, indicating that the industrial treatment
problems encountered in the textile and other industries. was not efficient for the removal of these compounds, which
Color is mainly caused by colorants that blocks light and corroborated some studies performed by Lise [10], showing
penetrate into water bodies to induce toxicity. Therefore it is that activated sludge systems were not efficient in the
required that colored effluents be treated before the effluents removal of azo dyes present in industrial effluents.
are discharged into an aquatic environment [1]. Advance
Oxidation Processes (AOPs) such as Fenton and photo- Maguire and Tkacz [11] detected 15 different dyes in
Fenton like processes are being widely developed for samples of water, suspended solids and sediments of a river
effective treatment of textile and other industrial effluents of Canada, and 3 of which were identified as: C.I. Disperse
[2]. Blue 79, C.I. Disperse Blue 26 and C.I. Disperse Red 60.
Oliveira [9] showed that the presence of about 1 μg of C.I.
Some efforts concerned with modification of the Disperse Blue 373 and 10 μg C.I. Disperse Orange 37, for
photo-Fenton catalysts with some supports have been each 1 g of the sediment of two distinct environmental
reported. The supports can minimize the cost of the process samples (one located immediately below the discharge of
due to the reusability properties, and also improve the the effluent of a textile industry and the other from a
activity, stability and selectivity of the catalyst [3]. A wide collection site situated at the entrance of the water treatment
range of solid materials, such as silica, zeolites, and pillared station for public supply), which characterizes high rates of
clays, have been reported to be active in oxidative mutagenic activity for these two samples. These same dyes
degradation of organic compounds through the photo- were detected in water samples in the same area analyzed by
Fenton-like reaction [4]. Some minerals such as hematite, Umbuzeiro [12].
goethite, and vermiculite and also activated carbon were

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Volume 5, Issue 8, August – 2020 International Journal of Innovative Science and Research Technology
ISSN No:-2456-2165
In this paper, we investigated the degradation of (NO3)2(aq) and perhaps agitation during preparation of the
methyl orange dye in aqueous solution using previously photocatalysts.
unreported catalyst prepared by immobilizing Fe(III) on
activated carbon support. Response surface methodology Experimental results of pHZPC determination, is shown
(RSM) was employed to generate 50 runs of experiments in Fig.2. As evident, change in pH by activated carbon
that ultimately provided the statistical data presented in this (ΔpH) was plotted against initial pH (pHo) of the solution
report. The variables studied are: reaction time, Fe-Ac dose, having constant ionic strength (0.01 M NaNO3). The pH at a
methyl orange concentration, pH and H2O2 concentrations. point where the initial pH of the solution intersects the
(ΔpH) equilibrated by a certain amount of an material is
II. METHODOLOGY referred to as the pHZPC [14]. The effect of pH was tested to
evaluate the feasibility of Fe (II) loading. The value of
Fresh samples of activated carbon (Sigma Aldrich) pHZPC obtained was (7.95). It has been reported that the pH
were used without further purification. The Fe-Ac photo- of carbon ranging between 4 and 8 is acceptable for most of
Fenton catalyst was prepared according to the procedure the applications [15]. This value of pHZPC (7.95) suggests
reported by Fatima et al [13]. Samples of Activated carbon that the surface becomes positive at pH values less than 7.95
were dispersed in a mixture with Fe(NO3)2 (Mayer and and becomes negative at pH values above 7.95. It thus
Baker) solution followed by stirring for 24 h. The indicates that below the pH of 7.95 loading of Fe (II) via
concentration of Fe (II) used was 5 times the cation cation exchange could rapidly takes place.
exchange capacity (CEC) of Activated carbon (4mmolg-1).
The suspension was then filtered and oven dried at 60 C for
2 h. The surface morphology of the catalyst was
characterized using Scanning electron microscopy (SEM).
Catalyst surface area, Cation exchange capacity, pH of zero
point charge (pHzpc) and surface acidic functional groups are
also reported.

The photodegradation experiments were performed in

a lab-scale using a 500W halogen lamp as irradiation source.
The reaction setup consists of conical flasks set containing Fig 1:- SEM image of Activated Carbon
the dye solution and catalyst mounted on an electric shaker
stationed 1m away from the light source. For tests using The Sear’s specific surface area of the activated carbon
only the Fenton reagent, the experiment was kept away from sample is 433 m2g-1 (Table 1). This is expected considering
light by covering it with aluminium foil. The flasks that a single gram of activated carbon can have a surface
containing stated amount of reagents are mounted on the area in excess of 500 (m²g-1), with 1500 m²g-1 being readily
shaker with light turned on and shaked for the stated time achievable.
after which the absorbance of the dye left is measured using
UV/Visible spectrophotometer. Parameter Value

III. RESULTS pHZPC 7.95

Sears surface area 433 m2g-1
A. Characterization of Fe-Ac Photocatalyst
The Scanning Electron micrographs of pure activated Cation exchange capacity 4mmolg-1
carbon and Fe-Ac are shown in Fig.1. Both images display
irregular cracks and crevices on the surface which could be Table 1:- Physico-chemical parameters of Fe-Ac catalyst
attributed to the amorphous and heterogeneous nature of
activated carbon. Fig.1a shows small pores on the surface CEC is the total capacity of a solid substance to hold
and reveals sheet-like structures with troughs and crests in a exchangeable cations. The CEC value obtained for the
synchronized manner. The pores are more evident in Fig.1b activated carbon is 4mmolg-1 (Table 1). This result is
which displays a rather eroded surface. This change in comparable to 4.67mmolg -1 obtained by Kavitha [14]. The
morphology could be attributed to treatment with Fe CEC value signifies the equilibrium amount of Fe (II) that
can be loaded on to the activated carbon surface [16].

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Volume 5, Issue 8, August – 2020 International Journal of Innovative Science and Research Technology
ISSN No:-2456-2165

Table 3:- Predicted Models for photo-Fenton oxidation of

MO using Fe-Ac

Fig 2:- pHZPC of Activated carbon

Table 2 displays the result of Boehm’s titration. The

presence of acidic groups namely Lactonic, Phenolic and
carboxylic is evident. Concentration of the surface groups
(meq/g) obtained is in the order Phenolic (1.021) >
Carboxylic (0.28) > Lactonic (0.023). The results are in
agreement with 1.0, 0.3 and 0.03 for Phenolic, carboxylic
and Lactonic respectively reported by Edwin [17].

Surface Groups Concentration (meq/g)

Lactonic 0.023 Fig 3:- Preliminary experiments of photo-Fenton, Fenton,
Phenolic 1.021 adsorption and photolysis under identical experimental
Carboxylic 0.28 conditions at MO initial concentration= 5mg/L, Fe-Ac dose
Total 1.342 = 1.0g/100mL, pH = 3 and H2O2 = 1.0mL for 30 minutes
Table 2:- Results of Boehm’s titration
C. Modelling of Photo-Fenton Reaction
B. Photo-Fenton Degradation of Methyl Orange In this study, a central composite design (CCD) was
applied, because of simple models (linear, quadratic etc)
can be related to response factor (percentage degradation).
 Control Experiment
The results of control preliminary experiment Fig.3 CCD is commonly used form of response surface
shows the profile of MO reduction by varied methods: methodology (RSM) [19].
Photo-Fenton (illumination with Fe-Ac catalyst and
hydrogen peroxide), Fenton (Fe-Ac and hydrogen peroxide Table 3 displays the sequential model sum of squares
without light), Adsorption (Fe-Ac without light and for all the possible models. The prob>F value of <0.0001
hydrogen peroxide) and Photolysis (without Fe-Ac, light for both Linear model and quadratic models suggests that
and hydrogen peroxide) under identical conditions. The both models are significant and could be used to study the
experimental results presented in Fig.3 is in the order Photo- photo Fenton reaction as values <0.05 are generally
Fenton > Fenton > Adsorption > Photolysis. There is a very accepted. However, the model with highest order
significant difference in MO dye removal between photo- polynomial is most preferred [20]. Hence, the quadratic
model is preferred. Other models with prob>F of above
Fenton (75%) and Fenton (44%). This is explained by the
increased generation of hydroxyl radicals by incident light 0.05 are insignificant and thus disregarded in this analysis.
in photo-Fenton system [2]. Similarly, Adsorption (12.5%)
A model with maximum values of for both ‘Adjusted
is less than Fenton (44%) due to lack of hydroxyl radicals to
initiate photodegradation [18]. Lastly photolysis (0.6%) R-squared’ and ‘Predicted R-squared’ is recommended.
removal is attributed to slight MO dye instability in the Appendix I shows that quadratic model has Adjusted R-
presence of light. Therefore it can be concluded that in squared’ of 0.9901 and ‘Predicted R-squared’ of 0.9828
photodegradation process, the observed MO dye removal while maintaining a minimum standard deviation of 1.29.
has elements of photolysis, adsorption, Fenton and photo- With these model analyses, quadratic model is adopted for
Fenton processes. Analysis of Variance (ANOVA), diagnostics and model
graphs analysis.

The second-order polynomial response equation was

used to describe the interactions between dependent and
independent variables.

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Lack of Fit Tests
Source Sum of DF Mean F Prob > F
Squares Square Value
Linear 2684.50 37 72.55 34.14 < 0.0001
2FI 2672.50 27 98.98 46.58 < 0.0001
Quadratic 33.73 22 1.53 0.72 0.7397 Suggested
Cubic 12.38 7 1.77 0.83 0.5926 Aliased
Pure Error 14.88 7 2.13
"Lack of Fit Tests": Want the selected model to have insignificant lack-of-fit.
Table 4:- Lack of Fit Tests of the predicted models for photo-Fenton oxidation of MO using Fe-Ac

Y = b0 + b1A + b2B +b3C + b4D +b5E2 + b11A2 + b22B2 Increase Parameter D (MO) Initial concentration (-
+ b33C2 +b44xD2 +b55E2 + b12AB + b13AC + b14AD + b15AE 2.74) results in decrease in Y. its second order component
+ b23AC + b24BD + b25BE + b34CD + b35CE +b45DE D2 (0.07) increases the response with maximum Y
obtainable at optimum value of D
where, Y is the % MO dye removal, A,B,C,D and E
represents the five independent variables (pH, catalyst dose, The effect of Factor E (Time) yields more response
hydrogen peroxide concentration, MO Initial dye (Y) with increasing amount of time.
concentration and time respectively), and the b values
represent regression coefficients. The ANOVA in this case confirms the adequacy of the
quadratic model (the Model Prob>F is <0.0001which is
Eight of the experiments were conducted at the central substantially less than 0.05.) The probability values for each
points. By using the Design Expert software, the following individual term in the model can also be visualised.
quadratic model for the experimental response was obtained Independent variables of the quadratic model including
(equation 1): pH(A), hydrogen peroxide concentration (C), MO
Y(photo-Fenton)= 55.44 – 1.87A + 14.59B + 49.62C -2.74D concentration (D), time (E), and second order effects of
+0.89E -0.09A2 -7.01B2 – 18.35C2 + 0.07D2 – 0.01E2 - catalyst dose (B2), peroxide concentration (C2), MO
0.04AB + 0.17AC + 0.00AD -0.00AE – 0.17BC 0.00BD + concentration (D2), and Time (E2) are significant with
0.02 BE +0.05CD + 0.00CE + 0.00DE Prob>F value of less than 0.05. Moreover, first order effects
(1) of (B) and interaction effects of AB, AC, AD, AE, BC, BD,
BE, CD, CE and DE are insignificant with prob>F of above
The coefficients of E2, AD, AE, BD, CE and DE are 0.05.
insignificant and thus were neglected conveniently. The
equation becomes Coefficient of determination (R2) is defined as the ratio
Y(photo-Fenton)= 55.44 – 1.87A + 14.59B + 49.62C - 2.74D + of the explained variable to the total variation and a measure
0.89E - 0.09A2 - 7.01B2 – 18.35C2 + 0.07D2 - 0.04AB + of the degree of fit. When R2 is close to 1, the model fits the
0.17AC – 0.17BC + 0.02 BE (2) actual experimental data better. The smaller the value of R2,
the less relevant the model fits the actual data [22-24].
According to equation (2) above, the weight of factor Accordingly, for a good fit of a model, R2 should be at least
A (pH) on the equation is predominantly negative. There is 0.80. The R2 value for variables is higher than 0.80, which
decrease in Y for the variable A (-1.78), its second order indicates that the regression model explains photo-Fenton
component A2 (-0.09) and interactions with other parameter the methyl orange degradation process by Fe-Ac
AB(-0.04), the results explains the apparent decrease in photocatalysis well. The R2 value is 0.9941(Table 4) for the
photo-Fenton response with increasing pH. degradation rate. The lack of fit value of 0.72 confirms the
lack of fit is not significant relative to the pure error when p
There is an increase in Y for the factor B (catalyst value is 0.7395, >0.05. The non-significant lack of fit shows
dose) +14.59. However, its second order component B2 (- good predictability of the model. The coefficient of variation
7.01) is negative implying decrease in Y with increasing (C.V. = 2.13) is low, indicated high precision and good
amount of B. It can be concluded that, there is an optimum reliability of the experimental values [25]. In addition, the
value of B that yields maximum response (Y). “R2 Pred” of 0.983 is in reasonable agreement with the “R2
Adj” of 0.990 (within 0.2), which also implies good
The effect of parameter C(H2O2 dose) iss silimar to predictability of the model [26]. Adequate precision
that of B (Catalyst dose) above. Factor C (+49.62) is compares the range of predicted values at the design points
positive and its second order component C2 18.35) is to the average prediction error [27]. The adequate precision
negative. The local value of C that yields maximum of 64.097 in this study, which is well above 4 indicates
response (Y) is the optimum H2O2 dose. adequate model discrimination

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Volume 5, Issue 8, August – 2020 International Journal of Innovative Science and Research Technology
ISSN No:-2456-2165
Three-dimensional surfaces and contour plots are 1g/100mL. This is attributed to the resultant increase in
graphical representation of regression equation for the concentration of Fe2+ ions from additional catalyst.
optimization of process conditions, and very useful However, catalyst dose beyond the optimum level results in
approach in revealing the conditions of the process. a decrease of MO degradation rate. This is due to the
inherent cloudiness of the solution with addition of large
amount of catalyst which reduces the amount of light
penetrating the solution to produce hydroxyl radicals [21].
The decrease in degradation rate can also be attributed to
scavenging of Hydroxyl radicals by the excess Fe2+ ions
72
(equation 3).At the same time, the effect of hydrogen
67
peroxide concentration change on the methyl orange
61
degradation rate has similar trends. However, hydrogen
Photo-fenton

56

51
peroxide concentration beyond the optimum level results in
a detrimental decrease in methyl orange degradation rate.
This can similarly be attributed to scanvenging of free
Hydroxyl radicals by the excess hydrogen peroxide
2.00
2.00 molecules (equation 3).
1.63
1.53

Fe(II)  OH.  Fe(III)  OH-

1.25
1.05
C: Peroxide 0.88 0.58

0.50 0.10
B: Catalyst dose H2O2 + OH.  HO2. + H2O (3)

Fig 4:- Interaction plot of reaction parameters D. Optimization of photo-Fenton oxidation of MO using
Fe-Ac catalyst
Fig.4 shows the interaction effect of the main photo- The objective of the optimization is to determine the
Fenton reaction parameters: Catalyst dose (Y axis) and H2O2 optimum value of variables from the model obtained via
(X axis) on MO degradation rate (Abscissa). As can be seen experimental design and analysis. The previous works tend
in the plots, the interactions effects of catalyst dose and to concentrate on how to maximize the target product, and
H2O2 concentration on the degradation rate of MO depict a ignore some aspects of consideration with respect to
spherical response surface; there is a local maximum region reaction conditions, such as economic cost, ecological
under the certain ranges catalyst dose and H2O2 factor, subsequent treatment, etc [28].
concentration. In addition, there is an increase in the
degradation rate of MO with an increase of upto about

Number pH Catalyst dose Peroxide MO dye concentration Time Photo-Fenton Desirability

1 3 0.1 0.62 5 30 76.31 0.955 Selected
2 3.02 0.1 0.54 5.03 29.71 73.59 0.954
3 3.43 0.1 0.7 5 30 77.13 0.947
4 3 0.1 0.5 5.01 28.66 72.66 0.943
5 3.54 0.18 0.57 5.54 30 73.34 0.940
6 5.61 0.1 0.6 5 30 68.78 0.920
7 3 0.1 0.64 10.25 30 68.22 0.909
8 7 0.11 0.78 5 30 69.66 0.892
9 3 0.1 0.61 20 29.99 60.98 0.868
10 6.96 0.1 0.83 20 30 56.16 0.798
Table 5:- Results of Optimum parameters

Therefore, in present work, the higher degradation rate peroxide should be required. Based on the quadratic model
of methyl orange not only is obtained from optimization, but and the related constraint conditions (Maximizing Y while
also some special conditions of pH value, catalyst dose, varying all the other parameters within experimental range,
hydrogen peroxide concentration and methyl orange initial numerical optimization was carried out. The optimum
concentration also are considered at the same time. While, conditions for the maximum MO degradation under related
there are four aspects of considerations. First, the maximum constraint conditions were found to be pH value of 3.00,
degradation of methyl orange which is the main objective of catalyst dose of 0.1 g/100ml, H2O2 dose of 0.62ml, and MO
optimization. Second, the optimal level of pH value should initial concentration of 5.0 mg/L and for 30 minutes. Under
be as high as possible because of no readjustment after optimal conditions, the model predicted a maximum methyl
degradation process, the solution could be discharged orange degradation rate of 76.3% (Table 5). These results
directly to aquatic environment after removal of catalyst. imply that there exist optimal reaction conditions for
Third, the relative small amount of catalyst has an advantage degradation rate of methyl orange using Fe-Ac catalyst.
of subsequent treatment. Last, minimal amount of hydrogen

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Volume 5, Issue 8, August – 2020 International Journal of Innovative Science and Research Technology
ISSN No:-2456-2165
IV. CONCLUSION [11]. R.J. Maguire, and R.J. Tkacz, “Occurrence of dyes in
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chemical reaction is dictated by several factors viz: reaction evaluation of the commercial product C.I. Disperse
time, Fe-Ac catalyst dose, methyl orange concentration, pH Blue 291 using different protocols of the Salmonella
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tools embedded in central composite design to model the 49-56, 2005.
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conditions for optimal degradation. The optimal conditions “Fe(III)/TiO2-Montmorillonite Photocatalyst in Photo-
are as follows: pH = 3, catalyst dose = 0.1 mg/100ml, H2O2 Fenton-Like Degradation of Methylene Blue,”
= 0.62ml, methyl orange concentration = 5mg/l and time = International Journal of Chemical Engineering, vol. 1,
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[14]. B. Kavitha, and D.T. Sarala, “Physico-chemical
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