Microchemical Journal 130 (2017) 129–136

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Microchemical Journal

journal homepage: www.elsevier.com/locate/microc

Use of response factorial design for process optimization of basic dye

adsorption onto activated carbon derived from Persea species
Abdelmajid Regti a, My Rachid Laamari a, Salah-Eddine Stiriba b,c, Mohammadine El Haddad a,⁎
a
Equipe de Chimie Analytique & Environnement, Faculté Poly-disciplinaire, Université Cadi Ayyad, BP 4162, 46000 Safi, Morocco
b
Equipe de Chimie Moléculaire, Matériaux et Modélisation, Faculté Poly-disciplinaire, Université Cadi Ayyad, BP 4162, 46000 Safi, Morocco
c
Instituto de Ciencia Molecular/ICMol, Universidad de Valencia, C/. Catedrático José Beltrán, 2, 46980 Paterna, Valencia, Spain

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

Article history: Full factorial design is a powerful and efficient mathematical approach widely applied in the optimization of re-
Received 30 May 2016 sponse. The important parameters which affect the removal efficiency of methylene blue such temperature, ini-
Received in revised form 20 July 2016 tial pH of the solution, concentration and adsorbent dosage were optimized. They coded as A, B, C and D,
Accepted 26 August 2016
consecutively, and were investigated at two levels (+1 and −1). A linear mathematical model representing
Available online 27 August 2016
the influence of the different variables and their interactions was obtained. Main effect, Normal probability
Keywords:
plot of residuals, analysis of variance (ANOVA), surface plots, and contour plots were used to study the effects
Factorial design and interaction effects between operational parameters.
Optimization © 2016 Elsevier B.V. All rights reserved.
Adsorption
Persea species
Cationic dye

1. Introduction
Effluents of textile industries are highly colored and disposal of these
wastes into receiving waters causes drastic damages to the environ-
ment. Indeed, they may significantly affect photosynthetic activity and
also be toxic to some aquatic life due to the presence of metals, chlo-
rides, etc. [1]. Most of dyes released during textile clothing, printing
and dyeing processes are considered as hazardous and toxic to some or-
ganisms and may cause direct destruction of aquatic creatures. In addi-
tion, dye wastewaters are commonly characterized by high salts
content and low biodegradation potential [2] which makes effective re-
moval by conventional wastewater treatment processes difficult [3].
The dyes have low biodegradability. Conventional biological waste-
water treatment processes are not efficient in treating dyes present in
wastewater [4–6]. Therefore, dye-wastewater is usually treated by
physical and chemical methods, such as sonochemical, photochemical,
electrochemical, coagulation and flocculation, membrane separation,
bio-degradation, photo-fenton processes, oxidation or ozonation
[7–16]. However, in developing countries, these methods are still too
expensive to be used widely. Physical adsorption is generally consid-
ered to be the most efficient method for quickly lowering the concentra-
tion of dissolved dyes in an effluent [17].
Currently, the most widely used and effective adsorbent in industry
is activated carbon because of their high surface area (its high surface
area), microporous character and the chemical nature of their surface.
Consequently, the scope of this study was not only to removal of meth-
ylene blue dye from aqueous solutions, but also to investigate the inter-
action between operating parameters. The technique of statistical
design for experiments can be used for optimization and modeling. It
has been widely accepted in manufacturing industry for improving
product performance and reliability, process capability and yield.
In the statistical design experiments, the factors involved in an ex-
periment at their respective levels, were simultaneously varied. Thus,
a lot of information can be taken with a minimum number of experi-
ment trials [18–21]. The experiments in which the effects of more
than one factor on response are investigated are known as full factorial
experiments. The most important advantages are that not only the ef-
fects of individual parameters but also their relative importance in
given process are obtained and that the interactional effects of two or
more variables can also be known [22–23].
In the present work, the experimental work is carried out using a 24
factorial design in order to examine the main effects and the interac-
tions between temperature, pH, initial concentration and adsorbent
dosage.
2. Materials and methods
2.1. Materials

⁎ Corresponding author. The Persea Americana nuts were washed with distilled water
E-mail address: elhaddad71@gmail.com (M. El Haddad). and dried in a drier at ambient temperature for several days. The

http://dx.doi.org/10.1016/j.microc.2016.08.012
0026-265X/© 2016 Elsevier B.V. All rights reserved.
130 A. Regti et al. / Microchemical Journal 130 (2017) 129–136
Fig. 1. Optimized structures of the MB using DFT at the B3LYP/6-31G (d,p).
unmodified Persea Americana nuts were assigned as PAN. The carboni-
zation of PAN was carried out using an appropriate weight of PAN and
25 mL concentrated phosphoric acid with a mass ratio (1:4) a glass bea-
ker of 100 mL, heated at 500 °C for 1 h producing a black carbonaceous
residue. The solid material was neutralized with KOH solution until neu-
tral pH. Afterwards, the found carbonized Persea Americana nuts (C-
PAN) was filtered and washed intensively with water. The C-PAN was
then dried at 100 °C for 2 h and kept in desiccators for further use. Meth-
ylene blue as azo dye was used as received without any purification; its
color is stable within the pH range of the study. The chemical structure
of methylene blue is given in Fig. 1.
A stock solution of 1000 mg/L was prepared by dissolving the re-
quired amount of dye in distilled water. Working solutions of the de-
sired concentrations were obtained by successive dilutions of the
stock solution.
The characterization of C-PAN was achieved by FT-IR spectrosco-
py and X-ray powder diffraction measurements. FT-IR spectra
(4000–450 cm− 1 range) were recorded with a Nicolet 5700 FT-IR
spectrometer on samples prepared as KBr pellets. The polycrystalline
sample of adsorbent was lightly ground in an agate mortar, pestle
and filled into 0.5 mm borosilicate capillary prior to being mounted
and aligned on an Empyrean PANalytical powder diffractometer
using Cu Kα radiation (λ = 1.54056 Å).
Fig. 2. FT-IR spectrum of C-PAN adsorbent.
Three repeated measurements were collected at room temperature
in the 10° b 2θ b 60° range with a step size of 0.01°. Scanning Electronic
Microscopy (SEM) images were obtained with HITACHI-S4100 equip-
ment operated at 20 kV.
2.2. Procedure and analysis
The principal steps of statistically designed experiments are: de-
termination of response variables, factors and factor levels; choice
of the experimental design; and statistical analysis of the data.
The 2 n factorial designs are widely applied in the experiments
that are taking into account several factors where it is necessary to
study the interaction effect of factors on the response, where each
variable is investigated at two levels. Only factors that affect re-
sponse can be chosen. Sixteen experiments were carried out by vary-
ing the temperature 293 K or 323 K, pH 2 or 10 initial concentration
25 mg/L or 50 mg/L, C-PAN dosage 0.1 g/L or 0.4 g/L. After 30 min, the
residual dye concentration in the reaction mixture was analyzed by
centrifuging the reaction mixture and then measuring the absor-
bance by UV–Visible spectroscopy of the supernatant at the wave-
length that correspond to the maximum absorbance of the sample
at 664 nm.
Fig. 3. XRD spectrum of C-PAN adsorbent.
 A. Regti et al. / Microchemical Journal 130 (2017) 129–136 131

Table 2
Estimated regression coefficients of factors and their effects for MB removal.

Term Effect Coefficient % contribution

Constant – 75.37 –
A 9.42 4.71 4.08
B 12.03 6.01 6.64
C −9.92 −4.95 4.52
D 39.68 19.84 72.29
AB −1.18 −0.59 0.064
AC 1.73 0.86 0.14
AD −6.88 −3.44 2.17
BC 4.95 2.47 1.13
BD −9.34 −4.67 4.01
CD 8.38 4.18 3.22
ABC 2.72 1.36 0.34
ABD 0.44 0.22 0.009
ACD −0.97 −0.48 0.043
BCD −2.02 −1.01 0.19
ABCD −5.02 −2.5 1.16

Fig. 4. SEM image of C-PAN adsorbent.

and aromatic C_C stretching vibration. Band at 1149 cm−1 is ascribed

to C\\O stretching in alcohol or ether or hydroxyl group [25,26]. The
bands at 1074 cm−1 and 876 cm−1 could result from ionized linkage
The amount of equilibrium adsorption qe (mg/g) was calculated P+ O– in acid phosphates esters, to symmetrical vibration in a chain
using the formula: of P\\O\\P and to P\\C phosphorus-containing compound [27,28].
These function groups are due to the present of H3PO4 acid as an activa-
C0 −Ce tion agent in the preparation of C-PAN.
qe ¼ V ð1Þ
W The XRD spectrum of C-PAN adsorbent was explored in Fig. 3, indi-
cates the presence of very few peaks because when the C-PAN is treated
where Ce (mg/L) is the liquid concentration of dye at equilibrium, C0 with acids the majority of those peaks disappear due to leaching out the
(mg/L) is the initial concentration of the dye in solution. V is the volume corresponding minerals during activation and washing with water [29].
of the solution (L) and W is the mass of dye biosorbent (g). The MB re- An amorphous peak with the equivalent Bragg angle at 2θ = 24.6 was
moval percentage (%) can be calculated as follows: recorded, together with other peaks recorded at 2θ = 17.5°, 31.2° and
47.5°.
C0 −Ce
Removal dye ð%Þ ¼  100 ð2Þ The surface morphology of the C-PAN adsorbent is shown in Fig. 4,
C0
The SEM image indicates that the surface is relatively smooth and con-
tains many pores. The SEM of C-PAN show very distinguished dark spots
where C0 is the initial dye concentration and Ce (mg/L) is the concentra-
which can be taken as a sign for effective adsorption of dye molecules in
tion of dye at equilibrium.
the cavities and pores of this adsorbent.
The results of the experimental design were analyzed using DESIGN
EXPERT 7.0 statistical software to evaluate the effects as well as the sta-
tistical parameters,
3.2. Development of regression model equation for the dye removal
3. Results and discussion
The 24 Factorial experimentations were carried out, in two levels
high and low. The higher level of variable was designed as ‘+’ and the
3.1. Characterization of C-PAN adsorbent
lower level was designed as ‘−’. For ease of notation, the effects were
designed as in Table 1 which shows the values of the factors selected
In order to investigate the surface characteristic of C-PAN ad-
in this study. This factorial design results in sixteen tests with all possi-
sorbent, FT-IR and XRD spectrums were studied. The bands posi-
ble combinations of A, B, C and D. The coded mathematical model can be
tions shown in FT-IR spectrum Fig. 2, are 876, 1074, 1149, 1563,
2916 and 3415 cm− 1. In this fact, the wide band at 3415 cm− 1 is
attributed to the hydroxyl groups [24]. The bands at 2916 cm− 1,
1563 cm− 1 and 1381 cm−1 correspond respectively to unsymmet-
rical aliphatic C\\H stretching, C_C stretching of aromatic rings
Table 3
Analysis of variance reduced model.

Factor Degrees of freedom Sum of square Mean of square F-value P-value

A 1 355.03 355.03 31.24 0.0014

Table 1 B 1 578.76 578.76 50.92 0.0004
Factors and levels used in factorial design study. C 1 393.52 393.52 34.62 0.0011
D 1 6298.4 6298.4 554.21 b0.0001
Parameter study Code Low (−1) High (+1)
AD 1 189.4 189.4 16.66 0.0065
Temperature (K) A 293 323 BC 1 98.05 98.05 8.62 0.026
pH B 2 10 BD 1 349.22 349.22 30.72 0.0015
Concentration (mg/L) C 25 50 CD 1 280.81 280.81 24.7 0.0025
Adsorbent dosage (g/L) D 0.1 0.4 ABCD 1 100.75 100.75 8.86 0.0247
132 A. Regti et al. / Microchemical Journal 130 (2017) 129–136

Table 4 Table 3, Sum of squares (SS) of each factor quantifies its importance
Factorial design matrix of four variables along with experimental and predicted responses in the process and the value of the SS increases the significance of the
for MB removal by C-PAN.
corresponding factor in the undergoing process also increases.
Run number Coded values of independent MB removal % The main effects and interaction effects of each factor having P
variables value b 0.05 are considered as potentially significant, and value that
A (T) B (pH) C (con) D (A.d) Observed Predicted Residual N0.1 indicate the model term is not significant. The adsorbent dosage
1 −1 −1 −1 −1 46.00 45.81 0.186 (D) had the greatest effect on removal efficiency ,followed by pH (B), con-
2 1 −1 −1 −1 68.97 67.13 1.835 centration (C), pH-adsorbent dosage interaction (BD), temperature (A),
3 −1 1 −1 −1 69.77 67.25 2.516 concentration-adsorbent dosage (CD), temperature-adsorbent dosage
4 1 1 −1 −1 74.00 78.53 −4.537 (AD), temperature-pH-concentration-adsorbent dosage (ABCD) and pH-
5 −1 −1 1 −1 25.77 27.58 −1.813
6 1 −1 1 −1 38.66 38.86 −0.207
concentration (BC).
7 −1 1 1 −1 48.00 48.88 −0.888 Furthermore, some coefficients in Eq. (4) are negligible, the final em-
8 1 1 1 −1 73.12 70.21 2.910 pirical model for the capacity adsorption in equilibrium becomes:
9 −1 −1 −1 1 96.00 98.36 −2.360
10 1 −1 −1 1 96.22 95.88 0.338 Y ¼ 75:38 þ 4:71 A þ 6:01 B−4:96 C þ 19:84 D−3:44 AD
11 −1 1 −1 1 94.20 91.07 3.125
þ 2:48 BC−4:67 BD þ 4:19 CD−2:51 ABCD: ð5Þ
12 1 1 −1 1 97.53 98.63 −1.103
13 −1 −1 1 1 88.47 86.85 1.62
14 1 −1 1 1 94.81 94.4 0.401 The experimental and predicted dye removal (%) is presented in
15 −1 1 1 1 97.12 99.50 −2.385 Table 4. Analysis of variance (ANOVA) was conducted to examine
16 1 1 1 1 97.39 97.02 0.363
the reliability of the model [30]. ANOVA shows whether the varia-
tions related to the model is significant compared to the variations
of the experimental results or not [31]. Fig. 5 shows a good agree-
given as: ment between the predicted and corresponding experimental re-
sults. The regression model had a high coefficient of determination
Y ¼ a0 þ a1 A þ a2 B þ a3 C þ a4 D þ a5 AB þ a6 AC þ a7 AD þ a8 BC þ a9 BD þ a10 CDþ (R2 = 0.9922), implying that 99.22% of the variations in dye removal
a11 ABC þ a12 ABD þ a13 ACD þ a14 BCD þ a15 ABCD: can be explained by the model and the model does not explain only
ð3Þ 0.78% of the variations. The Adequate precision for the ANOVA was
obtained to be 26.98, which is favorable. The preferred value for ad-
where Y is the theoretical response function, a0 is the global equate precision is N4 [32].
mean; ai and aij represent the regression coefficient corresponding to The lower coefficient of variation (CV% = 4.47) clearly demonstrat-
the main factor effects and interactions, respectively. By substituting ed that the deviations between actual and predicted values were low
the regression coefficients in Eq. (3) by their numerical values as and affirmed the precision and reliability of conducted experiments.
given in Table 2 we get:
3.3. Estimation of quantitative effects of the factors
Y ¼ 75:38 þ 4:71 A þ 6:01 B−4:96 C þ 19:84 D−0:59 AB
þ 0:87 AC−3:44 AD þ 2:48 BC−4:67 BD þ 4:19 CD þ 1:36 ABC Analyzing Fig. 6 and the coefficients of Eq. (5), it can be inferred
þ 0:22 ABD−0:48 ACD−1:01 BCD−2:51 ABCD: ð4Þ that the adsorbent dosage (D) was the most important variable of
the adsorption efficiency procedure since its coefficient was the larg-
The interacting factors affecting the removal of dye were est. The positive sign of this coefficient meant that dye removal was
determined by performing the analysis of variance (ANOVA) in favored at high adsorbent values. Increasing the dose of C-PAN from

100.00
Predicted color removal %

81.25

62.50

43.75

25.00

25.77 44.20 62.64 81.07 99.51

Actual color removal %

Fig. 5. The plot of predicted versus experimental decolorization efficiency.

 A. Regti et al. / Microchemical Journal 130 (2017) 129–136 133

98 98

79.75 79.75
color removal (%)

color removal (%)

61.5 61.5

43.25 43.25

25 25

-1.00 -0.50 0.00 0.50 1.00 -1.00 -0.50 0.00 0.50 1.00

Temperature pH

98 100

79.75 81
color removal (%)

61.5 62

43.25 43

25 24

-1.00 -0.50 0.00 0.50 1.00 -1.0 -0.5 0.0 0.5 1.0

Concentration Adsorbent dose

Fig. 6. Main effect plots for MB removal efficiency.

0.1 to 0.4 g/L increased the adsorption efficiency from 55.53% to
95.21%. This was due to the increase of sites or surface area at higher
amounts of the sorbent. The solution pH (B) also had an effect on re-
moval efficiency. An increase in the pH from 2 to 10 resulted in a
12.03% increase in adsorption efficiency due that at higher pH
value, the surface is negatively charged which increases the electro-
static attraction of the positively charged cationic dye, but an in-
crease on solution concentration from 25 mg/L to 50 mg/L resulted
in 9.92% decrease in color removal percentage.
The response of contour plot was analyzed and plots were obtain-
ed to assess the response of each factor graphically. The response of
certain factors is function that describes how the response moves
as the level of those factor changes, when the other factors are
fixed at their optimum levels. From the contour plots and surface
plots for the significant interactions were shown in Figs. 7 and 8.
The interaction plots showed that interactions of temperature and
adsorbent dose, pH and adsorbent dose, concentration and adsorbent
dosage were greater than pH-concentration interaction, but still less im-
portant than main effect of adsorbent dosage. This result was proved by
the values of the effects in Table 2.
For the statistical analysis of the experimental data, it is necessary to
assume that the data come from a normal distribution [31]. To deter-
mine whether or not the data set is normally distributed, the normal
probability plot of residual values is shown in Fig. 9. The data set has
normal distribution if the points fall close enough to the straight line.
It is evident from the Fig. 9 that the experimental points follow a straight
line suggesting normal distribution of the data.
3.4. Process optimization
One of the main aims of this study was to find the optimum
process parameters at which activated carbon produced will have a
high MB removal. The optimized conditions were around a Tem-
perature 293 K, pH 10, the initial dye concentration of 29.5 mg/L
134 A. Regti et al. / Microchemical Journal 130 (2017) 129–136

1.00 1.00

66
88

0.50 0.50 69

80
Adsorbent dose

Concentration
73

0.00 0.00

72 77

80

-0.50 -0.50
64

55

-1.00 -1.00
-1.00 -0.50 0.00 0.50 1.00 -1.00 -0.50 0.00 0.50 1.00

Temperature pH

1.00 1.00

88 88

0.50 0.50
Adsorbent dose

Adsorbent dose

79 79

0.00 0.00

71 71

-0.50 -0.50
62 63

53 55

-1.00 -1.00
-1.00 -0.50 0.00 0.50 1.00 -1.00 -0.50 0.00 0.50 1.00

pH Concentration

Fig. 7. Contour plots for interaction effects for MB removal efficiency.

and adsorbent dose of 0.4 g/L. In such optimal combination of
parameters, the adsorption reached approximately 98%. Desirability
was found equal to 1 when the adsorbent dosage is fixed on max-
imum value in range of values of other parameters which prove
clearly that adsorbent dosage is the major factor influencing the
removal efficiency.
3.5. Comparison of adsorption capacities of C-PAN with those of various AC
adsorbents
The values of the adsorption capacity of MB on C-PAN for the sixteen
experiments are shown in Fig. 10, the maximum uptake was 365.6 mg/g.
Table 5 lists the comparison of the maximum adsorption capacity of MB
on various adsorbents. Compared with some data in the literature, it's
shown that the Persea Americana activated carbon studied in this work
has a very large adsorption capacity.
4. Conclusion
A novel, low cost adsorbent prepared from agricultural waste,
Persea Americana, is successfully applied for the removal of MB
from its aqueous solution. The effect of temperature, pH, initial dye
concentration and adsorbent dose on the adsorption was studied
with the 16 experiments designed by the 24 full factorial designs.
Factorial experimental design approach is an excellent tool and
could successfully be used to develop empirical equation for the pre-
diction and understanding of MB removal efficiency, the statistical
analysis results proved the significance of the model developed
from experimental data to optimize the parameters.
 A. Regti et al. / Microchemical Journal 130 (2017) 129–136 135

97 84

84.5 78.25

72 72.5

59.5 66.75

47 61

1.00 1.00 1.00 1.00

0.50 0.50 0.50 0.50
0.00 0.00 0.00 0.00
-0.50 -0.50 -0.50 -0.50
Adsorbent dose Temperature Concentration pH
-1.00 -1.00 -1.00 -1.00

97 96

83.75 83.5

70.5 71

57.25 58.5

44 46

1.00 1.00 1.00 1.00

0.50 0.50 0.50 0.50
0.00 0.00 0.00 0.00
-0.50 -0.50 -0.50 -0.50
Adsorbent dose pH Adsorbent dose Concentration
-1.00 -1.00 -1.00 -1.00

Fig. 8. 3D surface for interaction effects for MB removal efficiency.

The most effective parameter influenced was adsorbent dosage

because of increasing of sites number and surface area. The most sig-
99 nificant interaction was observed in MB removal with the combina-
tion effects of C-PAN dosage and initial pH.
95
90
color removal (%)

80 400
70
350
50
300
30
20
Uptake (mg/g)

250
10
200
5
150
1
100

50

-2.20 -1.27 -0.34 0.59 1.51 0

1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16
Studentized Residuals Run Number

Fig. 9. Normal probability plot of residuals for MB removal efficiency. Fig. 10. Experimental adsorption capacity versus run number.
136 A. Regti et al. / Microchemical Journal 130 (2017) 129–136

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