Alexandria Engineering Journal (2016) xxx, xxx–xxx

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Alexandria University

Alexandria Engineering Journal

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ORIGINAL ARTICLE

Adsorption of rhodamine B and methylene blue

dyes using waste of seeds of Aleurites Moluccana,
a low cost adsorbent
Debora Luiza Postai, Carla Albertina Demarchi, Francielle Zanatta,
Danielle Caroline Cipriani Melo, Clóvis Antonio Rodrigues *

Núcleo de Investigações Quı´mico-Farmaceˆuticas (NIQFAR), Universidade do Vale do Itajaı´ (UNIVALI), Itajaı´, 88302-901 Santa
Catarina, Brazil

Received 20 October 2015; revised 7 March 2016; accepted 15 March 2016

KEYWORDS Abstract Removal of the cationic dyes rhodamine B (RhB) and methylene blue (MB) by waste
Aleurites moluccana; seeds Aleurites moluccana (WAM) was studied in a batch system. The adsorbent was characterized
Low cost adsorbent; by Fourier transform infrared spectroscopy (FTIR), thermogravimetric analysis (TGA), point of
Cationic dye; zero charge measurement, and the Boehm titration method. The effects of contact time and pH
Adsorption were investigated for the removal of cationic dyes. An increase in pH from 3 to 9 was accompanied
by an approximately three-fold increase in the amount of dye adsorbed. The adsorptions
equilibrium values were obtained and analyzed using the Langmuir, Freundlich, Sips, and
Redlich–Peterson equations, the Sips isotherm being the one that showed the best correlation with
the experimental values. The maximum adsorption capacities of the dyes were 178 mg/g for the MB
and 117 mg/g for the RhB. The kinetic sorption was evaluated by the pseudo-first-order,
pseudo-second-order, and intraparticle diffusion models, where it was observed that sorption
follows the pseudo-second-order kinetic model. The study of thermodynamics showed that the
adsorption is a spontaneous and endothermic process. The results indicate that waste seeds of A.
moluccana could be used as a low cost material for the removal of cationic dyes from wastewater.
Ó 2016 Faculty of Engineering, Alexandria University. Production and hosting by Elsevier B.V. This is an
open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).

1. Introduction tries, with highly toxic components and serious environmental

impacts. It is believed that the dyeing industry is responsible
Dyes are organic compounds that represent an important for releasing 100 tons of dyes per year into the environment,
group of pollutants. They are used in various areas, such as contaminating rivers and springs [1,2]. Of these dyestuffs,
the textile, plastics, rubber, leather, cosmetics and paper indus- 5–10% is lost in industrial effluents, and consequently,
wastewater treatment is one of the biggest problems we face
* Corresponding author. Fax: +55 (47) 341 7601. today [3].
E-mail address: crodrigues@univali.br (C.A. Rodrigues). Once the dyes are exposed to water, they are difficult to
Peer review under responsibility of Faculty of Engineering, Alexandria remove, as they are of synthetic origin and have a very
University.
http://dx.doi.org/10.1016/j.aej.2016.03.017
1110-0168 Ó 2016 Faculty of Engineering, Alexandria University. Production and hosting by Elsevier B.V.
This is an open access article under the CC BY-NC-ND license (http://creativecommons.org/licenses/by-nc-nd/4.0/).
Please cite this article in press as: D.L. Postai et al., Adsorption of rhodamine B and methylene blue dyes using waste of seeds of Aleurites Moluccana, a low cost
adsorbent, Alexandria Eng. J. (2016), http://dx.doi.org/10.1016/j.aej.2016.03.017
2 D.L. Postai et al.
complex molecular structure, with stability designed to with-
stand degradation by light, chemical, biological and other fac-
tors. This makes them very difficult to degrade [4].
There is no universal method capable of removing dye efflu-
ents. The best choice depends on the types of dyes to be
removed, their composition, concentrations and production
flow into the wastewater. Different physical, chemical, and
biological methods for the removal of dyes from aqueous solu-
tions have been investigated [3].
Of the removal methods, adsorption is one that is gaining
increasing attention due to its potential efficiency, low energy
consumption, high selectivity at molecular level, easy opera-
tion, and ability to separate various chemical compounds
[5,6]. Adsorption is a physical–chemical treatment of wastew-
ater in which the dissolved molecule is attached to an adsor-
bent surface by means of physical and chemical properties.
Depending on the nature of the adsorbent and the origin of
the dyes, different interactions may be performed, such as elec-
trostatic interaction and Van der Waals forces [3].
In order to meet the growing demand for clean and renew-
able sources of energy, the production of biodiesel from veg-
etable oils is growing at a remarkable pace, generating a
considerable amount of residual cake composed mainly of cel-
lulose, hemicellulose and lignin. It is estimated that for each
ton of seed, about half a ton of cellulose cake is generated. Bio-
diesel production is increasing every year, the volume of waste
generated is becoming a major environmental issue, and the
best form of disposal of this byproduct (agro-industrial waste)
requires study [7–9]. Therefore, one of the main problems to be
solved by the biodiesel industry is the adequate disposal of
these wastes [10–15].
One of the alternative materials for removing effluent waste
is seeds of Aleurites moluccana, which have features that enable
them to be used as adsorbent. The plant has the advantage of
large-scale production of seeds all year round, low cost, and
easy access. Thus, the aim of this study was to evaluate the
potential application of waste from the seeds of A. moluccana
for the removal of methylene blue dye (MB) and Rhodamine B
(RhB) from aqueous solution.
The effects were investigated of various parameters on pH,
dye concentration and temperature. The kinetics of adsorption
and maximum adsorption capacity were also studied, through
the application of mathematical models of adsorption.
2. Material and methods
2.1. Adsorbent material
The exocarp of chestnuts and almonds was removed, and
ground. The ground material was dried at 80 °C for 2 h. To
a round-bottomed flask equipped with heating mantle and
reflux condenser, 350 g of previously ground seed and
500 mL of hexane were added. The system was heated under
reflux for 24 h to remove the oil. After cooling, the mixture
was filtered and washed with hexane and hot water. The resi-
due was dried, crushed and sieved through a 35 mesh sieve.
2.2. Characterization of the adsorbent
The pHzpc of the waste seeds A. moluccana (WAM) was deter-
mined by the method described by Ponnusami et al. [16]: 0.05 g
Please cite this article in press as: D.L. Postai et al., Adsorption of rhodamine B and methylene blue dyes using waste of seeds of Aleurites Moluccana, a low cost
adsorbent, Alexandria Eng. J. (2016), http://dx.doi.org/10.1016/j.aej.2016.03.017
of waste seeds of A. moluccana was added to 20 mL of 0.1 M
NaCl. The pH values were adjusted to between 2 and 12, using
either 1.0 M HCl or 1.0 M NaOH. The solutions with the
WAM were stirred for 24 h. The pH was then recorded. The
DpH value was calculated by the difference between the initial
and final pH values (DpH = pHi
pHf) and a plot of DpH vs
pHf was prepared. The pH zero point charge (pHzpc) was
defined as a pH value DpH of zero.
The surface chemistry of waste seeds of A. moluccana was
characterized by Boehm method, as follows: 0.5 g WAS were
dispersed in 50 mL of 0.05 M NaHCO3, 0.025 M Na2CO3,
0.05 M NaOH, 0.05 M HCl, contained in conical flasks of
250 mL capacity and stirred for 24 h. After 24 h, the samples
were filtered through filter paper and titrated in triplicate with
0.1 M NaOH or 0.1 M HCl depending on the starting solution
used. The number of groups on the surface of WAM was ana-
lyzed as follows: NaHCO3 (carboxylic groups), Na2CO3 (car-
boxylic groups and lactones), NaOH (carboxylic groups,
lactones and phenolic groups) and HCl (basic sites) [17].
The method used for determining specific surface area
(SSA) of WAM was performed as follows [18]: 0.05 g of
WAM was mixed with 20 mL of deionized water. The MB
solution (100 mg/L) was then added to the WAM suspension
with 0.5 mL increments. The suspension was mixed continually
for about 2 h with a shaker. 2 mL of the solution was then
removed, and centrifuged. The remnant concentration of MB
in the solution was determined.
The value of SSA was derived from the point of complete
cation replacement determined on the titration curve. When
the curve deviates from the 45° line, this means that the MB
added cannot be completely adsorbed by WAM. In other
words, all the exchange sites of the adsorbent were covered
by the MB molecules. At this optimum point, the SSA is com-
puted from the amount of adsorbed MB, by the following
equation:

m   
MB 1
SSA ¼  Av  AMB  ð1Þ
319:85 ms
where mMB = mass of the adsorbed MB (mg/g) at the point of
complete adsorption, Av = the Avogadro’s number
(6.02  1023 mol
1), AMB = area covered by one MB molecule
(assumed to be 130 A2), and ms = mass of JB (mg).
The Fourier transform infrared spectra (FTIR) of adsor-
bents (in the form of KBr pellets) were measured using a
IRPrestige-21 Shimadzu, in the range of 700–2000 cm
1.
The TGA analyses were performed on equipment model
Netzsch STA 449 F3 Jupiter at a temperature range of
30–500 °C and a heating rate of 10 °C/min, using about
10.0 mg sample in cell alumina with nitrogen gas flow of
50 mL/min.
2.3. Batch adsorption experiment
2.3.1. Influence of pH
The pH effect on dyes adsorption was studied in the range
2–10. Dyes solutions were prepared using buffers tris hydrox-
ymethyl aminomethane (TRIS buffer) (pH 9.0), monochloroa-
cetic acid (pH 3.0) and not buffered (pH 6.0). Amounts of
50 mg of adsorbent were contacted with 20 mL of 300 mg/L
congo red (CR) rhodamine B (RhB) and methylene Blue
(MB) solutions, respectively, a shaker agitation under constant
Adsorption of rhodamine B and methylene blue dyes
speed of 250 rpm for 60 min to ensure equilibrium. Afterward,
all samples were centrifuged for 10 min at 3500 rpm and the
concentration of each dye was calculated from the measured
absorbance in the supernatant at their corresponding maxi-
mum absorption wavelength (554 nm for RhB, 540 nm for
CR and 668 nm for MB). The adsorption capacity (qe) was cal-
culated according to Eq. (2):
ðC0
Ce Þ  v
qe ¼
m
where C0 and Ce (mg/L) are the initial and equilibrium dye
concentrations in the liquid phase, respectively, v (L) is the
volume of solution and m (g) is the amount of adsorbent.
2.3.2. Adsorption isotherm study
Equilibrium adsorption isotherms were obtained by contacting
50 mg of adsorbent with 20 mL of MB or RhB solutions of
different initial concentrations (50–300 mg/L), agitation time
of 60 min, temperature of 25, 35, 45, 55 °C and pH of 3.0,
6.0 and 9.0. The concentration of the dye in the solution and
the adsorption capacity were determined as described above.
2.3.3. Adsorption kinetics
Kinetic experiments were performed by agitating 50 mg
of adsorbent with 20 mL of 100 mg/L MB and RhB solutions,
individually, at the same constant speed (250 rpm) and at the
temperature 55 °C, and pH 9.0 (the pH of the solution was
selected as the optimum from the pH effect experiments). Sam-
ples were withdrawn at appropriate time intervals (15, 30, 60,
90, 120 and 160 min), and absorbance in the supernatant was
measured. The concentration of the dye in the solution and
adsorption capacity were determined as described above.
2.4. Error analysis
To assess the adequacy of the equations applied on the
experimental data, we used the statistical parameters sum of
squared residuals (SSR), Eq. (3):
X
n
SSE ¼ ðqe;calc
qe;meas Þ2i
i¼1
where, qe,cal and qe,meas are the values of adsorption capacity
(mg/g) obtained by applying the model and the experimental
values, respectively. The lower the value the better the SSR
curve fits the experimental values.
Chi-square (v2) was also used, to analyze the model, Eq. (2):
X before and after the adsorption process, Fig. 2. The presence
n
ðqe;calc
qe;meas Þ2
v2 ¼
i¼1
qe;meas
where, qe,cal and qe,meas are the values of adsorption capacity
(mg/g) obtained by applying the model and the experimental
value, respectively. If the data from the model are similar to
the experimental data, v2 will be a small number; if they are
different, v2 will be a large number.
Please cite this article in press as: D.L. Postai et al., Adsorption of rhodamine B and methylene blue dyes using waste of seeds of Aleurites Moluccana, a low cost
adsorbent, Alexandria Eng. J. (2016), http://dx.doi.org/10.1016/j.aej.2016.03.017
3
4
3
2
pH=pHi-pHf
1
ð2Þ 0
-1
-2
2 4 6 8 10 12
pH f
Figure 1 Determining the point of zero charge.
3. Results and discussion
3.1. Characterization of the adsorbent
The pHzpc of solid surface is the pH values at which the
amount of acidic and basic functional groups is equal. Fig. 1
shows the plot of DpH vs pHf. The pHZPC of the WAM was
found to be 5.84, indicating that acidic groups are predomi-
nant on the surface of the adsorbents, and below these pH is
most suitable for the adsorption of anionic dye. The pHPCZ
is slightly below that found in shells of Jatobá, which was
pH 6.25 [19] and well below that of waste processing mustard
oil, which was pH 9.0 [20], but well above that of waste radish,
which was pH 3.4 [14] and Jatropha oil cake which was 5.0
[12]. The specific surface area (SSA) of WAM was found to
be 54.56 m2/g. This specific surface area is large when com-
pared with residue of Madhuca indica seeds (28.24 m2/g) [16],
powdered activated mustard cake (26 m2/g) [21], pongamia
oil cake (0.6 m2/g) [22], and rapeseed oil cake (11.98 m2/g)
[23]. However, the SSA is lower when compared with other
adsorbents obtained from plants, such as Opuntia ficus-indica
fruit waste 348 m2/g [24], waste tea leaves 480.16 m2/g [25],
and Moringa oleifera 787.34 m2/g [26].
ð3Þ
The functional groups present on the surface chemistry of
WAM were characterized through the Boehm, showing a
prevalence of acidic sites, particularly phenol (46.06 mg/g), lac-
tones (1.8 mg/g), and carboxylic acid (9 mg/g) compared with
the basic functional group (5.6 mg/g). The higher amount of
acid sites shows that the surface is rich in OH groups, which
results in greater ability to adsorption cationic dyes [27].
The infrared spectrum of the WAM waste was performed
ð4Þ of peaks at 1743 cm
1 represented the carbonyl (AC‚O)
stretching vibration present in WAM. The peaks observed at
1675 cm
1 are of strong stretching vibrations of (AC‚O).
The bands at 1035 cm
1 (CAO) can be assigned to esters.
These peaks are attributed to the carbonyl of the long-chain
acids and esters that still remained in the residue after the
extraction of oil. A peak at 1450 cm
1 indicates the presence
of a (ACH) group. A peak at 1240 cm
1 was assigned to
4 D.L. Postai et al.
100
95
Transmitance (%)
90
85
80
2000 1500
wavenumber (cm -1)
Figure 2 FTIR in the region 2000 cm
1 and 700 cm
1 for waste
of seed A. moluccana before and after adsorptions to the dye
methylene blue (MB) and rhodamine B (RhB).
CH‚CH stretching, and small peaks ranging from 1100 to
1000 cm
1 were assigned to CAO stretching [28].
Fig. 2 also shows the FTIR spectra of WAM after RhB or
MB adsorption. The spectra show new peaks, which are absent
from the spectrum of the WAM Peaks at 1647 cm
1 and
1655 cm
1 corresponding to the stretching vibration of
(C‚C) bonds, and the peaks found at 1537 cm
1 and
1542 cm
1 confirm the presence of aromatic bonds of
(C‚C) in both dyes. However, in the spectra after adsorption
of both dyes, the peaks of the WAM were predominant, due to
the small amount of dye adsorbed.
Thermogravimetric analysis (TGA) of the WAM was per-
formed before and after the adsorption process, in order to
investigate the thermal characteristics of the adsorbent, and
TGA is shown in Fig. 3(A), which shows that at approximately
150 °C, there was a small loss of weight due to elimination of
moisture retained in the material. Another mass loss starts at
approximately 250 °C, caused by the thermal degradation of
cellulose and hemicellulose. At 400 °C it is observed that the
WAN before the adsorption process had greater weight loss
than compared with the material after the adsorption process,
which can be attributed to decomposition of the dye. The final
weight loss occurs at about 450 °C, and may be attributed to
the degradation of lignin, which has a much higher thermal
stability than either cellulose or hemicellulose polymers.
Fig. 3(B) further displays DTG profiles of WAM and dye
adsorbed on WAM samples. For WAM combustion presents
two peaks centered at 100 °C and 350 °C. For both dyes
WAM–RhB and WAM–MB combustion was occurring at
lower temperatures with the TG peak centered at 330 °C.
Therefore, adsorption of the dyes on WAM introduced func-
tional groups, resulting in reduced stability of WAM.
3.2. Effect of pH
The initial pH is an important factor affecting adsorption. The
influence of pH on the adsorption of the dyes MB, RhB was
investigated by varying the initial pH of the solutions (3.0,
Please cite this article in press as: D.L. Postai et al., Adsorption of rhodamine B and methylene blue dyes using waste of seeds of Aleurites Moluccana, a low cost
adsorbent, Alexandria Eng. J. (2016), http://dx.doi.org/10.1016/j.aej.2016.03.017
6.0 and 9.0). Table 1 shows the effect of pH on the adsorption
of the dyes.
The values in Table 1 show an increase in adsorption capac-
ity with increasing pH for the dye MB, while for RhB, this
trend was not observed. This behavior could be explained by
pHpzc of the material, as well as the molecular nature of the
dyes. At pH 3.0 the adsorbed amount of MB was very low
(near zero) and may result in decreased negative charge on
adsorbent [2]. Thus, when the solution pH was less than the
pHpzc of WAM (pH below 5.84), the sorbent surface was likely
to have a net positive charge, and therefore cationic dye
adsorption was low because of the repulsive forces between
WAM-RB the positive surface of the adsorbent and the cationic
WAM-MB molecules.
WAM On the other hand, when the solution pH was higher than
1000 5.84, the adsorbent surface was likely to have a net negative
charge that favored cationic dye adsorption. This behavior
can be observed for the results of the adsorption capacity of
anionic dye CR, Table 1, which is well below those for cationic
dyes.
The adsorption of cationic dyes is favored when the pH is
higher than pHPCZ, due to the presence of functional groups
such as ANH2A+ and S+ in the different classes of dyes.
The reduction of MB adsorption capacity with decreasing
pH was also reported by Vieira et al. [2], employing the residue
as adsorbent and Macauba due to the decreased amount of
negative charge on the adsorbent.
The results indicate that the main mechanism of adsorption
is the electrostatic interaction between the surface of the adsor-
bent negative and the positive parts of the dye molecule.
Due to the low adsorption capacity of CR, it was not used
further in the studies.
3.3. Adsorption isotherm
The adsorption isotherm is the relationship between the
amount of dye adsorbed and its concentrations in the equilib-
rium solution at constant temperature. This experiment
enables the maximum adsorption capacity of a given adsor-
bent to be calculated, depending on the mathematical model
applied. We tested four different models, in order to find the
most appropriate one: Langmuir, Freundlich, Sips, and Red-
lich–Peterson.
The experimental isotherms were used as the non-linear
Langmuir Eq. (5), valid for monolayer adsorption [29]. This
model contains a limited number of sites and provides a homo-
geneous distribution of adsorption energies.
KL qm Ce
qe ¼ ð5Þ
1 þ KL Ce
where qe is the amount of dye adsorbed at equilibrium (mg/g),
Ce the dye concentration at equilibrium (mg/L), KL the Lang-
muir adsorption constant (L/mg), related to adsorption
energy, and qm is the maximum adsorption capacity (mg/g).
The Freundlich Eq. (6) can be applied to describe heteroge-
neous systems, as well as multilayer adsorption [30].
qe ¼ KF Ceð1=nÞ ð6Þ
where KF is the Freundlich adsorption constant (L/mg) related
to adsorption capacity, and n is the heterogeneity factor that
Adsorption of rhodamine B and methylene blue dyes 5

Figure 3 TGA (A) and DTA (B) curves of WAM (___), WAM–RhB (- - -) and WAM–MB (.....) in nitrogen atmosphere, heating rate:
10 °C/min.

Table 1 Effect of pH on the adsorption capacity (mg g
1) of The combination of the Freundlich and Langmuir gave the
the dyes at the WAM dye initial concentration of 300 mg/L; Sips model Eq. (7) [31].
solution volume 20 mL; adsorbent mass 0.05 g, agitation time KLF qm Cne
60 min. qe ¼ ð7Þ
1 þ KLF Cne
pH 25 °C 55 °C
where KLF is the adsorption constant of Sips (L/mg). At low
CR MB RhB MB RhB dye concentrations, this model reduces to the Freundlich iso-
3 16 –* 40 – 20 therm; while at high concentrations, it characterizes a Lang-
6 12 60 40 47 42 muir type isotherm. When the heterogeneity factor is 1, the
9 – 105 41 106 22 model assumes the Langmuir model, and when n > 1, positive
*
(–) The amount of dye adsorbed, for these conditions, was not cooperativity is assumed, while when 0 < n < 1, negative
significant. adsorption cooperativity is expected.
The Redlich–Peterson isotherm Eq. (8) is another mathe-
matical model used to describe adsorption processes [32].
KRP qm Ce
indicates whether the type of isotherm is irreversible (n = 0), qe ¼ ð8Þ
favorable (0 < n < 1) or unfavorable (n > 1). 1 þ aRP Cne

Please cite this article in press as: D.L. Postai et al., Adsorption of rhodamine B and methylene blue dyes using waste of seeds of Aleurites Moluccana, a low cost
adsorbent, Alexandria Eng. J. (2016), http://dx.doi.org/10.1016/j.aej.2016.03.017
6 D.L. Postai et al.

The molecular structure of MB (thiazine) and RhB (xanthene)

60
is flatter, so the adsorption capacity is higher [19].
Nonlinear regression was used to determine the best-fitted
50 model, and two error functions were evaluated: SSR and v2.
The results of its application to the experimental data of
40 adsorption isotherms are presented in Tables 2–5. By compar-
qm (mg/g)

ing the results of the values of SSR and v2 for Langmuir, Sips
30 isotherms are smaller than other isotherms for all conditions.
The WAM used in this study had maximum adsorption
20 capacity for the MB 178 mg/g. This value, for example, is
above those reported for palm Macauba (57.5 mg/g), a by-
10 product of biodiesel production reported in the literature, in
same working conditions and using the same mathematical
0 model of Sips [2]. This value is also higher compared with
20 40 60 80 100 120 140 160 the adsorption of MB by residues of wild radish, another waste
Ceq (mg/L) from the process of obtaining biodiesel, where the maximum
adsorption capacity is only 19.8 mg/g [33]. The WAM presents
Figure 4 Isotherm of adsorption of the MB on WAM. adsorption capacity approximately 10 times higher than the
Temperature 25 °C, agitation time 60 min, pH 6.0 and quantity cake of sunflower oil (15.80 mg/g), a by-product from the pro-
of adsorbent 0.05 g. The lines represent the result of the duction of sunflower oil [34]. The adsorption capacity of MB
application of mathematical models: Langmuir (___), Freundlich by WAM is about five times higher than for solid waste of
(.-..-..-), Sips (- - - -), and Redlich–Peterson (. . .. . ...). Madhuca indica oil cake (31.4 mg/g) [26]. Higher adsorption
capacities for MB are reported in the literature, for example,
Dragon fruit skin (640 mg/g) [35], Breadnut core (369 mg/g)
30 [36], and Breadnut peel (409 mg/g) [37]; but it is important
28 to emphasize that these are not a by-product of biodiesel pro-
26 duction like WAM.
24 The maximum adsorption capacity of RhB by WAM is
105 mg/g almost 70 times higher than that of mustard seed resi-
22
qe (mg/g)

20
18
16
14
12
10
8
0 25 50 75 100 125 150 175
Ceq (mg/L)
Figure 5 Isotherm of adsorption of the RhB on WAM.
Temperature 25 °C, agitation time 60 min, pH 6.0, quantity of
adsorbent 0.05 g. The lines represent the result of the application
of mathematical models: Langmuir (___), Freundlich (.-..-..-), Sips
(- - - -), and Redlich–Peterson (....).
where KRP is the Redlich–Peterson adsorption constant (L/mg)
and aRP is the affinity coefficient (L/mg). If the value of n is
equal to 1, the Redlich–Peterson isotherm is reduced to the
Langmuir and aRPCne where the term is much greater than 1;
the model approximates the Freundlich equation.
Figs. 4 and 5 show the application of different mathemati-
cal models for the dyes MB and RB. The parameters obtained
for the different mathematical models, different pH and tem-
perature conditions are shown in Table 2–5.
As can be seen, the model that applies to the adsorption of
the dyes in the adsorbent MB and RhB is the Sips model, since
the values of r2 are close to 1 and for c > 1, indicating a high
factor of heterogeneity. The molecular structure of the dyes
plays a very important role in their adsorption with WAM.
due 1.52 mg/g using the same conditions and Langmuir model
[38]. Meanwhile, Jatoba bark showed adsorption capacity of
54.8 mg/g under the same conditions and mathematical models
[19].
Therefore it is possible to confirm the advantage of using
WAS when compared with other by-products of obtaining
biodiesel.
3.4. Adsorption kinetics
200 225 250
The contact time between the adsorbent and the dye is of sig-
nificant importance in the treatment of waste water by adsorp-
tion. The adsorption kinetics can be studied by adsorption on
the basis of constant speed. This adsorption constant is an
important factor in the choice of material to be used for
adsorption.
Figs. 6 and 7 show the adsorption of RhB and MB on
WAM from aqueous solution as a function of contact time.
It can be noted from Figs. 6 and 7 that the adsorption of both
dyes increased as contact time increased. The maximum
adsorption of RhB and MB was achieved almost within 120
and 160 min respectively.
In order to establish an equilibrium time for maximum
adsorption, different mathematical models have been used to
explain the adsorption kinetics of dyes. In a review of the liter-
ature, it was identified that two kinetic models have been
widely used to describe the adsorption models, with the model
of pseudo first order and pseudo second order obtained under
conditions far from equilibrium.
The model of pseudo-first order, also known as Lagergren
equation is represented in Eq. (9) [39]:
qt ¼ qe ð1
e
k1 t Þ ð9Þ

Please cite this article in press as: D.L. Postai et al., Adsorption of rhodamine B and methylene blue dyes using waste of seeds of Aleurites Moluccana, a low cost
adsorbent, Alexandria Eng. J. (2016), http://dx.doi.org/10.1016/j.aej.2016.03.017
Adsorption of rhodamine B and methylene blue dyes 7

Table 2 Isotherm parameters of Langmuir and Freundlich for RhB adsorption by WAM; solution volume 20 mL; adsorbent mass
0.05 g, agitation time 60 min.
Langmuir Freundlich
T (°C) KL (mg L
1) qm (mg g
1) r2 SSR v2 KF (mg L
1) n r2 SSR v2
pH 9
25 3.8  10
3 101 0.996 5 3 2.8 0.4 0.962 11 4
35 3.3  10
3 94 0.971 94 23 0.5 0.8 0.963 23 110
45 5.3  10
3 76 0.991 11 3 1.2 0.7 0.991 3 12
55 7.3  10
3 50 0.969 16 5 1.2 0.6 0.963 19 6
pH 6
25 4.1  10
3 81 0.993 8 2 0.9 0.7 0.991 11 3
35 3.1  10
3 85 0.984 50 10 1.0 0.7 0.967 29 12
45 5.1  10
3 99 0.974 54 13 1.3 0.7 0.957 89 22
55 2.9  10
3 119 0.996 6 2 0.8 0.8 0.994 9 2
pH 3
25 5.8  10
3 57 0.932 45 15 0.9 0.7 0.905 61 20
35 3.3  10
3 94 0.971 14 7 0.5 0.8 0.963 9 9
45 1.7  10
2 30 0.944 15 7 2.8 0.4 0.901 26 13
55 1.9  10
3 64 0.993 3 1 0.2 0.8 0.987 0 1

Table 3 Isotherm parameters of Sips and Redlich–Peterson for RhB adsorption by WAM. Solution volume 20 mL; adsorbent mass
0.05 g, agitation time 60 min.
Sips Redlich–Peterson

1
1
T (°C) KL (mg L ) qm (mg g ) n r2
SSR v
2
KRP (mg L1) aRP (mg L
1) n r2 SSR v2
pH 9
25 7.4  10
4 31 1.3 0.992 3 1 3.0  10
2
1.2
0.1 0.903 34 17
35 1.8  10
4 58 2.1 0.989 74 25 1.9  10
2
1.1 0.1 0.977 16 8
45 6.3  10
3 101 0.9 0.992 11 4 2.1  10
2
1.0 0.1 0.986 18 10
55 3.1  10
3 23 3.9 0.972 7 4 1.8  10
2
1.1 0.1 0.954 23 12
pH 6
25 4.2  10
3 82 0.9 0.993 8 3 1.4  10
2
1.0 7.8 0.988 14 5
35 1.8  10
3 95 1.1 0.997 6 5 1.2  10
3
1.0 6.4 0.975 16 6
45 2.0  10
4 105 1.7 0.993 76 25 2.8  10
1
1.1 3.7 0.995 11 4
55 2.8  10
3 145 1.0 0.996 6 2 8.6  10
3
1.0 5.8 0.993 10 4
pH 3
25 2.8  10
6 28 3.1 0.995 10.4 3.5 2.3  10
1
1.1 5.5 0.984 10.9 5.5
35 1.8  10
4 34 2.1 0.989 5.4 5.4 2.1  10
3
0.9 4.2 0.962 18.7 18.7
45 5.2  10
4 23 2.1 0.973 7.3 7.3 2.4  10
2
1.2 3.5 0.801 48.6 48.6
55 2.9  10
4 27 1.7 0.999 0.07 0.02 1.0  10
1
1.0 3.2 0.997 1.2 0.4

where qt is the amount of dye adsorbed on the time (t), qe
(mg/g) is the value in the state of equilibrium and K1 (min
1)
is the adsorption constant of the pseudo-first order.
The model of the pseudo-second order, developed by Ho
and McKay, is represented by Eq. (10):
k2 q2e t
qt ¼
1 þ k2 q2e t
where K2 is the rate constant of pseudo-second order adsorp-
tion (mg/g min) [40].
Another model uses intraparticle diffusion, represented in
Eq. (11), to identify a possible mechanism of intraparticle dif-
fusion as a limiting step:
qt ¼ ki t0:5 þ Ci
where Ki is the intraparticle diffusion constant (mg/g min0.5)
and Ci is a constant related to the extent of the boundary layer
effect. In this equation it is assumed that the intraparticle dif-
fusion is the rate limiting step in the overall adsorption, and
has been used to describe the values obtained on this occasion
[41].
ð10Þ The results of the adsorption kinetics were obtained for MB
and RhB. The parameters obtained are shown in Table 6. The
adsorption kinetic curves are shown in Figs. 6 and 7. Usually
the best fit can be selected based on the value of the correlation
coefficient (r2).
Based on the results it can be seen that the adsorption
kinetics of RhB and MB can be well explained by the
pseudo-second order adsorption model with high r2 (0.949
ð11Þ and 0.959 respectively). Error analysis reveals that the SSR

Please cite this article in press as: D.L. Postai et al., Adsorption of rhodamine B and methylene blue dyes using waste of seeds of Aleurites Moluccana, a low cost
adsorbent, Alexandria Eng. J. (2016), http://dx.doi.org/10.1016/j.aej.2016.03.017
8 D.L. Postai et al.

Table 4 Isotherm parameters of Langmuir and Freundlich for MB adsorption by WAM. Solution volume 20 mL; adsorbent mass
0.05 g, agitation time 60 min.
Langmuir Freundlich
T (°C) KL (mg L
1) qm (mg g
1) r2 SSR v2 KF (mg L
1) n r2 SSR v2
pH 9
25 1.2  10
3 61 0.912 250 72 8.5  10
2 2.6 0.937 814 203
35 4.6  10
3 42 0.965 48 42 1.4  10
2 2.5 0.926 881 220
45 3.9  10
3 89 0.954 96 51 9.1  10
8 5.4 0.912 1022 255
55 2.8  10
3 43 0.962 101 25 2.9  10
3 2.9 0.947 650 162
pH 6
25 9.9  10
3 105 0.900 357 89 3.3 0.6 0.879 428 107
35 6.8  10
3 142 0.930 196 65 1.9 0.7 0.912 245 82
45 6.9  10
3 90 0.919 196 49 1.9 0.6 0.885 274 68
55 2.1  10
3 178 0.953 61 20 0.67 0.8 0.946 69 23

Table 5 Isotherm parameters of Sips and Redlich–Peterson for MB adsorption by WAM. Solution volume 20 mL; adsorbent mass
0.05 g, agitation time 60 min.
Sips Redlich–Peterson
T (°C) KL-F (mg L
1) qm (mg g
1) n r2 SSR v2 KRP aRP n r2 SSR v2
pH 9
25 8.9  10
23 266 13.9 0.883 787 262 2.9 1.9  1045
29 0.961 85 256
35 4.6  10
14 103 9.0 0.895 220 241 2.7 8.9  1026
18 0.991 18 55
45 2.5  10
6 153 7.8 0.951 103 310 3.8 2.7  1012
8.6 0.950 106 319
55 1.7  10
15 112 10.0 0.999 2 5 4.2 1.0  1012
1.9 0.897 649 162
25 2.2  10
4 63 2.3 0.926 267 90 0.7492 2.8  10
6 2.5 0.919 290 98
35 2.6  10
4 57 3.6 0.997 9 5 1.792 3.7  10
1 0.9 0.841 182 546
45 2.2  10
4 64 7.5 0.958 46 139 0.4279 9.8  10
12 4.8 0.980 49 16
55 1.1  10
7 48 3.7 0.994 7 4 0.3164 4.5  10
14 5.6 0.967 42 21

31,5 24

31,0
22
30,5

30,0 20
q e (mg/g)

q e (mg/g)

29,5
18

29,0
16
28,5

28,0 14

0 20 40 60 80 100 120 0 20 40 60 80 100 120 140 160 180

time (min) time (min)

Figure 6 Kinetics of adsorption of the RhB at WAM. RB
concentration of 100 mg/L, 0.05 g adsorbent mass, temperature
55 °C, and pH 9.0. The lines show the result of mathematical
models: pseudo-first order (___), pseudo-second order (- - - -), and
intraparticle (. . .).
Figure 7 Kinetics curve adsorption of the MB on WAM. MB
concentration of 50 mg/L, 0.05 g adsorbent mass, temperature
55 °C, pH 9.0. The lines show the result of application mathe-
matical models: pseudo-first order (__), pseudo second-order (- - -),
and intraparticle (. . .).

Please cite this article in press as: D.L. Postai et al., Adsorption of rhodamine B and methylene blue dyes using waste of seeds of Aleurites Moluccana, a low cost
adsorbent, Alexandria Eng. J. (2016), http://dx.doi.org/10.1016/j.aej.2016.03.017
Adsorption of rhodamine B and methylene blue dyes 9

Table 6 Kinetic parameters for adsorption of MB and RhB at Table 7 Thermodynamic parameters for the adsorption of
WAM; solution volume 20 mL; adsorbent mass 0.05 g, dye RhB and MB on WAM.
solution concentration 100 mg/L. DH0 DS0 DG0 (kJ mol
1) r
Pseudo first order MB RhB (kJ mol
1) (J mol
1) (T K)
qe (mg g
1) 30.3 21.23 RhB
12.97
57.12 5.05 (298) 0.9927
K1 (1/min 0.17 0.06 4.92 (308)
r2 0.847 0. 866 4.73 (318)
SSR 1.5 14.4 4.25 (328)
v2 0.51 3.61
MB
12.09
32.26
1.36 (298) 0.9913
Pseudo second order
1.74 (308)
qe (mg g
1) 31.2 23.65
2.17 (318)
K2 (mg g
1 min) 0.019 0.004
2.67 (328)
r2 0.959 0.949
SSR 0.42 5.7
v2 0.14 1.41
Intraparticle 1,0
C (mg g
1) 26.9 10.81
Ki (mg/g min0.5) 0.394 0.308 0,5
r2 0.977 0.972
SSR 0.25 3.2
0,0
v2 0.08 0.81

and v2 are very low for this mathematical model. The intra-
particle model also shows a high r2 value and v2 value and very
low SSR, and this model has a high Ci value, which is not con-
sidered good for this model, since it should be close to zero.
For MB the qe, experimental (31.2 mg/g) is equal to qe calcu-
lated (Table 4) for the pseudo-second order model. For RhB,
the qe, experimental (22.3 mg/g) and the qe, calculated values
(23.68 mg/g) are very close to one another for the pseudo-
second order model compared with the value of the pseudo-
first order. The r2 are also closer to unity for pseudo-second
order kinetics than that for the pseudo-first order kinetics.
Usually the model pseudo-second order is the model that best
represents the adsorption of cationic dyes. The same behavior
was reported for the adsorption of MB by Jatoba bark [19],
Mhaduca indica oil cake [28], waste of palm Macauba [2] and
in the adsorption of RhB using termite feces [42].
The value of K2 found in this work is close to that reported
for adsorption of MB by the waste palm Macaúba 0.055 mg/
g min [2]. However, the value found is lower than that
observed for the adsorption of MB in Mhaduca indica oil cake
(0.760 mg/g min) [28].
3.5. Thermodynamic parameters
The thermodynamic parameters of adsorption, shown in
Table 7, including Gibbs free energy (DG0), enthalpy (DH0)
and entropy (DS0), were calculated by the following equations
[43]:
Cs
KD ¼
Ce
DG ¼
RT ln KD
DS DH
ln KD ¼
ð14Þ
R RT
where KD is the equilibrium constant, Cs is the amount of dye
adsorbent (mg/g), Ce is the equilibrium concentration of dye in
LnKD
-0,5
MB
RB
-1,0
-1,5
-2,0
0,00305 0,00310 0,00315 0,00320 0,00325 0,00330 0,00335
1/T
Figure 8 Plot of ln KD vs 1/T.
the solution (mg/L), R is the gas constant (8.314 mol/K) and T
is the absolute solution temperature (K). The plot of ln KD vs
1/T is linear (Fig. 8). Values of DH0 and DS0 were calculated
from the slope and intercept respectively (Table 7).
The negative value of DG0 indicates that the MB dye
adsorption process is spontaneous and favorable, and that
the more negative the value of DG0 is, the more energetically
favorable the process is. Positive values of DG0 for the dye
RhB represent an increase in randomness of the system during
the adsorption process. The values of DH0 were negative for
both dyes, indicating that the process is exothermic in nature.
The negative values of DS0 show the decreased affinity of
WAM toward the dyes. In general, adsorption can be ascribed
to physical or chemical adsorption. DH0 for physical adsorp-
tion ranges from
4 to
40 kJ mol
1, compared to that of
chemical adsorption ranging from
40 to
800 kJ/mol. The
values in Table 7 suggest that dye adsorption on WAM may
be due to physical binding.
ð12Þ
4. Conclusions
ð13Þ
The results obtained show that the seed residue of A. moluc-
cana can be used as a low cost adsorbent for removal of dye
methylene blue and rhodamine B. The pH at the point of zero
charge, indicating that it was 5.84 in the adsorbent, has the
property of adsorption of cationic dyes such as methylene blue

Please cite this article in press as: D.L. Postai et al., Adsorption of rhodamine B and methylene blue dyes using waste of seeds of Aleurites Moluccana, a low cost
adsorbent, Alexandria Eng. J. (2016), http://dx.doi.org/10.1016/j.aej.2016.03.017
10 D.L. Postai et al.

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