International Journal of Phytoremediation

ISSN: (Print) (Online) Journal homepage: www.tandfonline.com/journals/bijp20

Blended Nephelium lappaceum and Durio zibethinus

wastes for activated carbon production via
microwave-ZnCl2 activation: optimization for
methylene blue dye removal

Ali H. Jawad, Ahmad Hapiz, Ruihong Wu, Ahmed Saud Abdulhameed & Zeid
A. ALOthman

To cite this article: Ali H. Jawad, Ahmad Hapiz, Ruihong Wu, Ahmed Saud Abdulhameed
& Zeid A. ALOthman (2024) Blended Nephelium lappaceum and Durio zibethinus wastes for
activated carbon production via microwave-ZnCl2 activation: optimization for methylene
blue dye removal, International Journal of Phytoremediation, 26:10, 1655-1666, DOI:
10.1080/15226514.2024.2344178

To link to this article: https://doi.org/10.1080/15226514.2024.2344178

Published online: 06 May 2024.

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International Journal of Phytoremediation
2024, VOL. 26, NO. 10, 1655–1666
https://doi.org/10.1080/15226514.2024.2344178

Blended Nephelium lappaceum and Durio zibethinus wastes for activated

carbon production via microwave-ZnCl2 activation: optimization for methylene
blue dye removal
Ali H. Jawada,b,c , Ahmad Hapiza,b , Ruihong Wua,b,d , Ahmed Saud Abdulhameede,f , and Zeid A.
ALOthmang
a
Faculty of Applied Sciences, Universiti Teknologi MARA, Shah Alam, Malaysia; bAdvanced Biomaterials and Carbon Development Research
Group, Faculty of Applied Sciences, Universiti Teknologi MARA, Shah Alam, Malaysia; cEnvironmental and Atmospheric Sciences Research Group,
Scientific Research Center, Al-Ayen University, Nasiriyah, Iraq; dDepartment of Chemistry, Hengshui University, Hengshui, China; eDepartment of
Pharmaceutical Chemistry, College of Pharmacy, University of Anbar, Ramadi, Iraq; fCollege of Engineering, University of Warith Al-Anbiyaa,
Karbala, Iraq; gChemistry Department, College of Science, King Saud University, Riyadh, Saudi Arabia

ABSTRACT KEYWORDS
Herein, this work targets to employ the blended fruit wastes including rambutan (Nephelium Activated carbon; adsorption;
lappaceum) peel and durian (Durio zibethinus) seed as a promising precursor to produce activated durian seed; methylene blue dye;
carbon (RPDSAC). The generation of RPDSAC was accomplished through a rapid and practical rambutan peel; ZnCl2 activation
procedure (microwave-ZnCl2 activation). To evaluate the adsorptive capabilities of RPDSAC, its
efficacy in eliminating methylene blue (MB), a simulated cationic dye, was measured. The Box–
Behnken design (BBD) was utilized to optimize the crucial adsorption parameters, namely A: RPDSAC
dose (0.02–01 g/100 mL), B: pH (4–10), and C: time (2–6 min). The BBD design determined that the
highest level of MB removal (79.4%) was achieved with the condition dosage of RPDSAC at
0.1 g/100 mL, contact time (6 min), and pH (10). The adsorption isotherm data is consistent with the
Freundlich concept, and the pseudo-second-order versions adequately describe the kinetic data. The
monolayer adsorption capacity (qmax) of RPDSAC reached 120.4 mg/g at 25 °C. Various adsorption
mechanisms are involved in the adsorption of MB dye onto the surface of RPDSAC, including π–π
stacking, H-bonding, pore filling, and electrostatic forces. This study exhibits the potential of the
RPDSAC as an adsorbent for removal of toxic cationic dye (MB) from contaminated wastewater.

NOVELTY STATEMENT
This research work utilizes blended fruit wastes namely rambutan peels and durian seeds to be as
potential precursor for producing an activated carbon via microwave assisted ZnCl2 activation to be
a promising adsorbent for methylene blue dye from aqueous environment.

Introduction effective approach for removing contaminants because of its

exceptional characteristics, including resistance to contami-
Cationic dyes, particularly methylene blue (MB), are com-
nants, reusability, minimum waste generation, affordability,
monly employed as pigments in producing plastics, medi-
and high efficacy (Elwakeel et al. 2017a; Reshadi et al. 2020;
cines, cosmetics, leather, and textiles during various industrial
Elwakeel et al., 2018b). Several adsorbents based on natural
processes (Zhao et al. 2019). The release of various dyes
throughout the water body at varying concentrations can materials have been applied for the removal of organic dyes
harm the aquatic ecosystems (Tian et al. 2022). Hence, the from water, for example, rubber fruit shells modified with
treatment of removing dyes before releasing the industrial 3-(aminopropyl)-triethoxysilane (Buhani et al. 2023a), carbon
effluent into aquatic environments is critical. Several methods, from rubber fruit shells (Buhani et al. 2023b), and magnetic
including photocatalytic degradation (Surender and Balakumar alginate beads (Elwakeel et al. 2017b).
2022), membrane filtration (Xiang et al. 2022), electrochemi- Activated carbon (AC) is widely recognized as a highly
cal degradation (Singh and Dhaliwal 2022), coagulation (Liu efficient adsorbent for wastewater treatment because of its
et al. 2022), and adsorption (Yousef et al. 2023; Aryee et al. extensive porous structure, significant surface area, high
2022), are commonly used to remove organic dyes from adsorption capacity, chemical stability, diverse functional
wastewater. However, secondary waste, expenses, or process groups, and recyclability (Li et al. 2020; Azam et al. 2022;
complexity inhibit the majority of these procedures. The Elwakeel et al., 2018a). However, the high expenses involved
adsorption methodology has been recognized as the most in offering commercial AC frequently make it impractical,

CONTACT Ali H. Jawad [email protected], [email protected] Faculty of Applied Sciences, Universiti Teknologi MARA, 40450 Shah Alam, Selangor,
Malaysia.
© 2024 Taylor & Francis Group, LLC
1656 A. H. JAWAD ET AL.

therefore limiting its use (Dao et al. 2021). Significant atten- AC. To conduct the adsorption investigation, the solutions
tion is being devoted to the manufacturing of ACs from containing MB (λmax: 661 nm; MW: 319.86 g/mol; R&M
agricultural residue. This is driven by the increasing need Chemicals) were produced at a concentration of 1000 mg/L
for cost-effective AC, particularly those obtained from and adjusted as required. The tests utilized analytical-grade
renewable sources (Zhang et al. 2021; Lewoyehu 2021). chemicals and reagents from R&M Chemicals, Malaysia,
Moreover, the synthesis of AC from lignocellulosic materials which included zinc chloride (ZnCl2), sodium chloride
is a prospective choice owing to its renewability, accessibility, (NaCl) powder, hydrochloric acid (HCl), and sodium
cost efficiency, and nontoxicity (Hoang et al. 2022). The hydroxide (NaOH) pellets. These chemicals were provided
synthesis of AC utilizing several lignocellulosic sources such without the need for further purification.
as the following feedstock, hawthorn kernel (Zhen et al.
2022), Althaea officinalis L. (Isinkaralar 2022), orange peel
(Jimoh et al. 2022), banana peel (Tripathy et al. 2021), and RPDSAC preparation
Aesculus hippocastanum L. biomass (Işınkaralar et al. 2022). The fruit feedstock waste (RP and DS) was washed using hot
Several activating agents such as sodium carbonate distilled water to eliminate dust and other undesirable parti-
(Na2CO3) (Uçar et al. 2014), zinc chloride (ZnCl2) (Al‐Qaessi cles. Subsequently, the precursors were subjected to drying in
2010), phosphoric acid (H3PO4) (Sirajo and Zaini 2022), and an oven set at a temperature of 100 °C for 24 h. This step was
potassium hydroxide (KOH) (Genli et al. 2022) are essential performed to eliminate any remaining moisture and to con-
in the activation process to achieve the appropriate level of firm an optimal drying process. Subsequently, the RPDS was
porosity, increase the surface area and dispersion of pores in pulverized into a fine powder and then sifted to achieve a
AC (Kula et al. 2008). Among other chemical activators, consistent particle size of 2 mm. During the activation pro-
ZnCl2 facilitates the production of AC with exceptional fea- cess, a mixture of 1 g of the precursor (RPDS, with a 50%:50%
tures including increased surface area, reduced pore volume, mixing ratio of RP and DS) and 2 g of the chemical activator
and greater pore size, which increases the carbon yield and (ZnCl2) was prepared. The mixing ratio of 1:2 was predeter-
provides an abundance of functional groups for the uptake mined to be the optimal ratio and was maintained through-
of pollutants (Luo et al. 2019). Various techniques, such as out the procedure. Afterward, the RPDS/ZnCl2 system was
microwave radiation and conventional pyrolysis, can be subjected to a 24 h heating process at 100 °C in an oven to
employed to produce AC from lignocellulosic biomass ensure thorough drying. After that, RPDS/ZnCl2 was placed
(Rashidi et al. 2022). The utilization of microwave heating inside a modified microwave oven (SAMSUNG ME711K,
has numerous advantages compared to traditional heating 20 L) and exposed to microwave radiation (800 W) for 20 min
methods, such as a substantial yield of the desired product, in presence of pure N2 (99.99%) gas, with a constant flow
enhanced thermal efficiency, precise process controls, and rate of 100 mL/min (previously determined as the best acti-
consistent heat dispersion (Hijab et al. 2021). The fruit and vation conditions). Then, boiled distilled water was applied
vegetable processing industry discharged a huge quantity of to wash off the produced RPDSAC and to achieve neutral
fruit and vegetable wastes and by-products. This huge por- pH solution. Subsequently, a drying process was carried out
tion of the fruit and vegetable wastes are usually dumped in for RPDSAC by heating inside an oven for 24 h at a tempera-
landfills or rivers which is not preparable environmental ture of 100 °C. Finally, the RPDSAC was sieved to constant
solution. Thus, recycling process livestock as feed resources particles size of 250 µm. Afterward, RPDSAC was kept inside
to extract or develop value-added products is preferable a tight desiccator for future applications.
alternative compared to disposal methods.
Hence, the primary aim of this study is to utilize a
microwave-assisted ZnCl2 activation process to transform a Characterization
mixed fruit wastes of economically worthless tropical fruit res-
idues, specifically rambutan (Nephelium lappaceum) rind (RP) The Micromeritics ASAP 2060 device was used to measure
and durian (Durio zibethinus) seed (DS), into AC material. The the pore volume and surface area of the RPDSAC. Scanning
structural characteristics of rambutan peel (RP; N. lappaceum) electron microscopy (SEM) and energy dispersive X-ray
and DS (D. zibethinus) vary, and using them for AC synthesis (EDX) analysis were employed to investigate the microstruc-
improves the general characteristics of the resulting AC. The tural features and elemental composition of the RPDSAC.
efficacy of activated carbon derived from rambutan peel and The Zeiss Supra 40 VP instrument was used for this pur-
durain seed (RPDSAC) in eliminating the toxic cationic dye pose. The analysis was performed before and after MB
MB from an aqueous environment was assessed. Furthermore, adsorption. The crystallographic structure of the RPDSAC
Box–Behnken design (BBD) was employed to statistically opti- was determined using X-ray diffraction (XRD) analysis con-
mize the critical parameters of the adsorption process. ducted on PANalytical X’Pert PRO equipment. The identifi-
cation of functional groups in RPDSAC, both before and
after MB adsorption was achieved by using Fourier trans-
Materials and methods form infrared spectra (FTIR) acquired from a Perkin-Elmer
Spectrum RX I analyzer. The spectral investigation was con-
Materials
centrated on the wavelength range from 4000 to 450 cm−1.
The residual biomass from fruit, specifically RP and DS, was The surface charge of the RPDSAC was characterized via a
obtained from kitchen wastes as a precursor for producing point of zero charges (pHpzc) method (Dalvand et al. 2016).
 International Journal of Phytoremediation 1657

Design of experimental Co − Ce
R% = ×100 (2)
Employing the BBD within the framework of the mathemat- Co
ical model, this investigation designed experiments to ascer-
tain the optimal values for the variables under consideration where the Co (mg/L) and Ce (mg/L) acronyms represent to
(RPDSAC dosage, pH, and duration) to achieve the maxi- the concentrations of MB at their initial (before adsorption)
mum response. This study employed the RSM approach with and equilibrium (after adsorption) concentration, respec-
BBD through the utilization of the statistical software Design tively. The adsorption experiments were conducted in dupli-
Expert 13 (State Ease, USA). The levels of the investigated cate under identical conditions and the results are reported
variables, including the RPDSAC dosage (A), pH (B), and as an average value.
time (C), are presented in Table 1. A second-order polyno-
mial model was applied to establish a correspondence
between the dependent response and the independent Adsorption study of MB onto RPDSAC
parameters, as shown in Equation (1).
Experiments were carried out to assess the RPDAC’s capac-
ity for adsorption using the batch adsorption technique.
According to the data presented in Table 2, run 4 (with an
β 0 + ∑βi Xi + ∑βii Xi2 + ∑∑βij Xi X j
Y= (1)
RPDSAC dose of 0.1 g/100 mL, pH of 10, and 6 min) exhib-
ited the maximum efficiency in removing MB, with a rate of
79.4%. Adsorption experiments were done under the speci-
In the context of this expression, Y represents the depen-
fied suitable conditions, with initial concentrations of MB
dent variable, Xi and X j denote input factors, β 0 signifies the
varied from 20 to 150 mg/L. Serial adsorption studies were
intercept term, βi signifies the linear effect, βij represents the
performed with MB dye using a similar methodology out-
connection effect between parameter, and βii indicates
lined in “Design of experimental” section. The mathematical
the quadratic impact. Table 2 presents the variables obtained
Equation (3) was used to measure the adsorption capacity
from the framework that was constructed, combined with
(qe, mg/g) of the RPDSAC.
the corresponding empirical result, which is the MB removal
(%). A solution of 100 mL of MB and a precisely measured
quantity of RPDSAC were combined to initiate the MB dye qe =
(Co − Ce )V (3)
adsorption test. The mixes were placed in a water bath W
shaker and gently stirred at a fixed rate (110 strokes/min) for
a certain time. Afterward, the solutions were separated from
The symbol V (L) symbolizes the MB dye solution’s vol-
the adsorbent by passing them through a 0.45 μm syringe
ume and W (g) RPDSAC’s weight.
filter. The spectrophotometer (HACH, DR 3900) was used to
quantify the remaining quantities of MB in the aqueous
solutions at λmax 661 nm. The removal efficiency (R, %) of
MB dye was determined using Equation (2). Results and discussion

Table 1. Codes and actual variables and their levels in BBD. Characterization of RPDSAC
Codes Variables Level 1 (−1) Level 2 (0) Level 3 (+1) The specific surface area analysis was carried out to deter-
A RPDSAC dose 0.02 0.06 0.1 mine the specific surface area and pore diameter of RPDSAC
(g)/100 mL
B pH 4 7 10 as shown in Figure 1(a,b) respectively, and the results are
C Time (min) 2 6 10 also summarized in Table 3. From Table 3, the RPDSAC
exhibited a particular surface area of 567 m2/g and a total
pore volume of 0.19 cm3/g. As per IUPAC (Sing 1985), the
Table 2. Experimental matrix based on BBD approach for designing experi- RPDSAC exhibits a mesoporous configuration with pore
ments and the corresponding response [MB removal (%)]. sizes ranging from 2 to 50 nm, as seen by the average pore
Run Dose (g)/100 mL pH Time (min) MB removal (%) diameter of 2.61 nm. The N2 adsorption-desorption isotherm
1 0.02 4 6 72.8 of the RPDSAC may be classified as Type-IV, suggesting that
2 0.1 4 6 77.2
3 0.02 10 6 72.5 a considerable proportion of its structure consists of meso-
4 0.1 10 6 79.4 pores (Sing 1985; Foroutan et al. 2021a, 2021b). In addition,
5 0.02 7 2 70.9 the pore size distributions of BJH (Barrett, Joyner, and
6 0.1 7 2 75.1
7 0.02 7 10 71.6 Halenda) can be utilized to definitively verify the presence of
8 0.1 7 10 78.5 mesopores in RPDSAC (see the plot inserted in Figure 1(b)).
9 0.06 4 2 71.4 The existence of tiny slit pores in the RPDSAC shape is
10 0.06 10 2 72.7
11 0.06 4 10 74.1 illustrated by the H4 hysteresis loop shown in Figure 1(a)
12 0.06 10 10 74.3 (AlAbduljabbar et al. 2021). Based on the above information,
13 0.06 7 6 73.4 the RPDSAC exhibits a substantial level of porosity, a high
14 0.06 7 6 73.1
15 0.06 7 6 73.2 volume of pores, and a big surface area. Consequently, it
16 0.06 7 6 73.2 offers a preferable porous surface for capturing MB dye
17 0.06 7 6 73.3 molecules.
1658 A. H. JAWAD ET AL.

Figure 1. (a) N2 adsorption–desorption isotherms of RPDSAC and (b) pore size

distribution of RPDSAC.

Figure 2. XRD patterns of RPDSAC.

Table 3. Surface properties of RPDSAC.

Parameter(s) Value
BET surface area (m2/g) 567
Langmuir surface area (m2/g) 977
Pore volume (cm3/g) 0.19
Total volume in pores (cm3/g) 0.33
Pore diameter (nm) 2.61

The phase structure of RPDSAC was determined using

XRD analysis. Figure 2 illustrates the XRD patterns of
RPDSAC. Figure 2(a) illustrates that RPDSAC has two
prominent peaks at 2θ = 26.1° and 44.2°, indicating the pres-
ence of the graphitic structure (Dao et al. 2021; González‐
García 2018). Furthermore, RPDSAC exhibits prominent
peaks at 2θ = 31.9°, 34.5°, 38.3°, 55.7°, and 61.4°, which can
be attributed to the presence of an activator (ZnCl2) in the
production process of OPWRAC. These peaks correspond to
ZnO as documented in the JCPDS file no. 01–079-0205
(Hadi et al. 2021).
FTIR spectroscopy was used to gain an understanding of
the relationships between RPDSAC and MB, along with the
chemical composition of RPDSAC. Figure 3 illustrates the
FTIR bands of RPDSAC and RPDSAC–MB. The RPDSAC
spectrum (Figure 3(a)) exhibit well-defined peaks in the
range of 3600–3860 cm−1, which correspond to the stretching
of O-H bonds in the group of hydroxyls found in lignin,
hemicellulose, and cellulose (Ahmad et al. 2014). Furthermore, Figure 3. FTIR spectra of (a) RPDSAC and (b) RPDSAC after MB adsorption.
various peaks were detected at specific wavenumbers:
2912 cm−1 (confirms the existence of aliphatic C–H groups),
2330 cm−1 (indicating the presence of C≡C (alkyne groups)), The SEM–EDX analysis was used to identify the morpho-
1700–1650 cm−1 (indicating the stretching of carbonyl (C = O) logical structure and elemental composition of RPDSAC and
bonds in carboxyl and hemicellulose), 1500–1450 cm−1 (indi- RPDSAC–MB. Figure 4(a–d) displays SEM micrographs of
cating the presence of aromatic C = C bonds in lignin), RPDSAC and RPDSAC–MB at two distinct levels of magni-
1014 cm−1 (indicating the stretching of C–O bonds), and fications (2.0k× and 3.0k×), whereas Figure 4(e,f) shows EDX
867–590 cm−1 (C–H out-of-plane bending; Ahmad et al. spectra of RPDSAC and RPDSAC–MB. Figure 4(a,b) demon-
2014). The FTIR bands of RPDSAC–MB (after MB adsorp- strates that the interface of the RPDSAC exhibits heterogene-
tion on the RPDSAC surface) (Figure 3(b)) show noticeable ity, roughness, and well-defined pores. Notably, the created
changes in the intensity and location of several bands which pores facilitate the penetration of the MB dye molecules into
indicates the involvement of RPDSAC functional groups in the inner surface of RPDSAC. Moreover, the adsorption of
the adsorption process of MB. the MB dye onto the surface of the RPDSAC, as shown in
 International Journal of Phytoremediation 1659

Figure 4. SEM images of (a,b) RPDSAC at different magnification power, (c,d) RPDSAC–MB at different magnification power, and (e,f) EXD analysis for RPDSAC and
RPDSAC–MB respectively.

Figure 4(c,d), the surface shows a noticeable reduction in the of the investigated factors and their variations. The ANOVA
surface porosity and the disappearance of surface cavities. results of the proposed quadratic model are displayed in
Hence, this signifies the loading and incorporation of MB Table 4. Based on Table 4, the p-value and F-value of the
molecules on the surface of RPDSAC. Moreover, the EDX recommended model were both below 0.0001 and 865.31,
analysis confirmed the presence of carbon (C), oxygen (O), respectively. This indicates that the model was highly advan-
and nitrogen (N) elements in both RPDSAC and RPDSAC– tageous and could effectively establish the correlation
MB. Additionally, the sulfur (S) element was detected in the between the assessed variables and the outcome (Kutluay
RPDSAC–MB. The sulfur (S) is originally a part from the and Temel 2021). The p- and F-values of the quadratic poly-
molecular structure of MB, which reconfirms the loading of nomial model revealed the significance and accuracy of the
MB dye on the surface of RPDSAC–MB. suggested model (Foroutan et al. 2022). The model’s signif-
icant R2 value (0.99) highlights its major significance and
indicates that the calculated and observed MB removal data
Statistical analysis of MB removal
are completely comparable. Furthermore, the F-value of
An analysis of variance (ANOVA) was conducted to deter- 0.7692 for the lack of fit indicates that it is not significant
mine the accuracy of the design and assess the effectiveness in terms of pure error (Ashrafi et al. 2021). Hence, the
1660 A. H. JAWAD ET AL.

Table 4. ANOVA for MB dye removal. data shown in Figure 6(a) demonstrates that raising the
Sum of Mean RPDSAC dosage from 0.06 to 0.1 g resulted in an enhanced
Source squares df square F-Value p-Value Remarks removal efficacy of MB. This tendency is attributed to the
Model 91.23 9 10.14 865.31 <0.0001 Significant high surface area and efficient adsorption sites of RPDSAC
A—Dose 62.72 1 62.72 5354.15 <0.0001 Significant
B—pH 1.44 1 1.44 123.35 <0.0001 Significant at increasing RPDSAC dosages. The 3D plot (Figure 6(b))
C—time 8.82 1 8.82 752.93 <0.0001 Significant demonstrates the combined effect of varying time and the
AB 1.56 1 1.56 133.38 <0.0001 Significant RPDSAC dose on the speed of MB removal when keeping
AC 1.82 1 1.82 155.58 <0.0001 Significant
BC 0.3025 1 0.3025 25.82 0.0014 Significant the pH (4) constant. Figure 6(b) illustrates that the
A² 10.35 1 10.35 883.15 <0.0001 Significant RPDSAC’s ability to remove the MB dye was consistently
B² 1.88 1 1.88 160.15 <0.0001 Significant high across various adsorption durations (2–6 min). This
C² 2.58 1 2.58 220.08 <0.0001 Significant
Residual 0.0820 7 0.0117 observation is linked to the rapid occupation of the active
 Lack of fit 0.0300 3 0.0100 0.7692 0.5682 Not significant sites of the RPDSAC. The 3D plot (Figure 6(c)) demon-
Pure error 0.0520 4 0.0130 strates the combined effect of altering the duration and pH
Cor total 91.31 16
on the rate of MB removal while keeping the RPDSAC
dose constant at 0.1 g. Figure 6(c) demonstrates that the
rate of MB removal in the alkaline media (pH = 10)
acquired model can be utilized to optimize the output. More exceeds that in the acidic medium. The RPDSAC exhibits
accurately, the model possesses substantial statistical perfor- a pHpzc value of 6.0 (see Figure 6(d)). Consequently, when
mance and is deemed suitable for investigations when the the pH is lower than pHpzc, the surface of the RPDSAC
components of the model exhibit a p-value of ≤0.05. Table carries a positive charge (Damiri et al. 2020). These find-
4 indicates that the model terms A, B, C, AB, AC, BC, A2, ings indicate that the surface of RPDSAC is primarily com-
B2, and C2 had a significant effect on removing MB. The posed of negatively charged particles when the pH is above
properties of the suggested model are considered statistically 6.0, resulting in a strong affinity for capturing MB mole-
significant if the p-value is less than 0.05 and vice versa. cules. The behavior of the cationic MB molecules is con-
The second-degree polynomial that describes the conceptual trolled in the liquid phase when the pH value exceeds the
removal of MB is represented in Equation (4). This equation pKa (3.8) value of MB (Tang et al. 2021). These findings
is derived by integrating the independent variables and MB indicate that electrostatic interactions, which play a crucial
removal components of the model, as indicated by the role in adsorption, take place at pH levels higher than the
ANOVA test. pHpzc of RPDSAC and the pKa of MB, as shown in
Equation (5).
MB removal ( % ) =
+73.24 + 2.80 A + 0.4250 B + 1.05C
+ 0.6250 AB + 0.6750 AC − 0.2750 BC (4)
RPDSAC − O− + MB+ ↔ RPDSAC − O − ⋯ + MB (5)

+ 1.57 A2 + 0.6675B 2 − 0.7825BC 2

To verify the normal distribution of the residuals, it is Adsorption study

crucial to conduct a secondary analysis of the created model
by examining the normality test (Figure 5(a)). The distribu- The adsorption capacity of the RPDSAC is affected by vari-
tion of points in Figure 5(a), following a random allocation, ations in the starting concentration (ranging from 20 to
clearly indicates that both the model’s component and the 150 mg/L) of the d MB solutions, as depicted in Figure 7.
outputs of the ANOVA are entirely appropriate (Jawad et al. Following this investigation, the pH level of the solution
2021). The observed levels for the experimental MB removal remained consistent at (10), and a consistent amount of 0.1 g
and their associated predicted MB removal values demon- of RPDSAC was used. The increase in the starting concen-
strate a significant linear correlation, as shown in Figure tration of MB from 20 to 150 mg/L led to a significant
5(b), thereby suggesting the suitability of the model. Figure improvement in the adsorption capacity of RPDSAC, rising
5(c) displays the residuals plotted against the run number from 17.3 to 119.4 mg/g. The behavior is influenced by the
for the removal of MB dye. The data points in Figure 5(c) significant concentration gradient, which enhances the
are distributed randomly about the origin, suggesting that movement of dye within the internal pores of the RPDSAC,
the model is both trustworthy and accurate. causing MB dye to migrate toward the active surface of the
RPDSAC (Jawad et al. 2018).

Dual effects of variables on MB removal

Adsorption kinetics
The 3D response surface visualizations significantly sim-
plify the understanding of the relationship between the The progress and advancement of adsorptive removal of MB
independent factors (RPDSAC dosage, time, and pH) using RPDSAC mainly relies on the data obtained from the
and the dependent variable (MB removal). The 3D plot kinetic analysis. Experimental adsorption data were utilized to
(Figure 6(a)) demonstrates the combined effect of varying evaluate kinetic models, including the pseudo-first order (PFO;
the RPDSAC dose and pH on the rate of MB removal Lagergren 1898) and pseudo-second order (PSO; Ho and
while maintaining the contact time stable t at 2 (min). The McKay 1998) models. Table 5 presents the mathematical
 International Journal of Phytoremediation 1661

Figure 5. (a) Normal probability plot of residuals for MB removal; (b) the plot of the relationship between the predicted and actual values of MB removal; and
(c) residual versus run numbers of MB removal (%).

equations for each of these models, while Table 5 provides the formula of assessed isotherm models, specifically
data on the kinetic parameters. The study revealed that the Freundlich (1906), Langmuir (1918), and Temkin (1940).
PSO model exhibited higher R2 values compared to the PFO Figure 8 displays curves that best fit for the isotherm
model (refer to Table 6). Additionally, the calculated qe values
models, while Table 8 presents the parameters of the
for the PSO kinetic model closely matched the experimental
values of qe. This suggests that the PSO model provides a rea- studied isotherms. The adsorption patterns of MB corre-
sonable explanation for the adsorption of MB on the RPDSAC. spond to the Freundlich isotherm model, as evidenced by
This finding indicates that the adsorption of MB is facilitated its significant R2 value. This confirmation suggests that
by the chemisorption process, which occurs due to the inter- MB can undergo multilayer adsorption on the heteroge-
actions between the positively charged groups of MB and the
neous RPDSAC surface (Jawad et al. 2020). The data in
negatively charged groups of RPDSAC (Theamwong et al. 2021).
Table 9 contrasted the results of the current study’s find-
Adsorption isotherms ings (the qmax of the RPDSAC toward MB = 120.4 mg/g)
with those of previous research. The synthetic RPDSAC
To further understand the equilibrium adsorption results
and the possible correlation between MB molecules and exhibits a notable ability to absorb cationic dyes. The
RPDSAC, isotherm methods were utilized to analyze the RPDSAC exhibits promising potential as an adsorbent for
experimental adsorption data. Table 7 includes the the removal of cationic dyes from wastewater.
1662 A. H. JAWAD ET AL.

Figure 6. 3D response surfaces plots of (a) AB (RPDSAC dose × pH), (b) AC (RPDSAC dose × time), (c) BC (pH × time), and (d) pHpzc of RPDSAC.

Table 6. PFO and PSO kinetic parameters for MB adsorption on RPDSAC (dos-
age = 0.1 g, solution pH = 10, temperature = 25 °C, agitation speed = 110 rpm,
and volume of solution = 100 mL).

MB PFO PSO
concentration qe exp. qe cal k1 qe cal k2 × 10−2
(mg/L) (mg/g) (mg/g) (L/min) R2 (mg/g) (g/mg min) R2
20 17.3 17.3 0.38 0.99 17.5 8.15 0.99
40 43.1 42.9 0.33 0.99 43.8 2.35 0.99
60 58.2 56.7 0.18 0.97 59.3 0.61 0.99
80 73.5 7.61 0.23 0.90 72.7 0.53 0.97
100 80.8 79.4 0.12 0.99 83.3 0.21 0.99
150 119.4 118.6 0.04 0.97 128.7 0.04 0.98

Thermodynamic properties
Figure 7. (a) Effect of the contact time on MB dye adsorption at several con- The determination of the standard deviation in thermody-
centrations (dosage = 0.1 g, solution pH = 10, temperature = 25 °C, agitation namic characteristics, such as enthalpy (ΔH°), Gibbs free
speed = 110 rpm, and volume of solution = 100 mL).
energy (ΔG°), and entropy (ΔS°), emphasizes the factors that
drive the MB adsorption pathway with RPDSAC, whether it
Table 5. Adsorption kinetics and isotherms nonlinear models. is driven by enthalpy or entropy. Subsequently, the thermo-
Models Formula Descriptions dynamic properties ΔG°, ΔH°, and ΔS°, along with the ther-
modynamic equilibrium factor kd, were determined using
qt qe (1 − e )
PFO − k1t
k1: PFO rate constant (L/min)
=
Equations (6)–(8) (Ebisike et al. 2023).
PSO qe2k2t k2: PSO rate constant
qt = (g/mg min) ∆G° = − RT lnkd (6)
1+ qe K 2t
 International Journal of Phytoremediation 1663

Table 7. Adsorption isotherms nonlinear models.

Models Formula Descriptions
Langmuir qm K aC e qm: monolayer capacity (mg/g)
qe =
1+ K aC e Ka: Langmuir constant (L/mg)

Freundlich 1 KF: Freundlich constant (mg/g) (L/mg)1/n

qe = K F C e n
n: adsorption intensity
Temkin RT K T : Temkin constant (L/mg)
qe = ln( K T C e )
bT bT: adsorption intensity (J/mol)

Figure 9. The van’t Hoff plot for the adsorption of MB onto RPDSAC (dose =
0.1 g, pH = 10, and solution volume = 100 mL).

Table 10. Thermodynamic parameters for the adsorption of MB on RPDSAC

(dose = 0.1 g, pH = 10, and solution volume = 100 mL).
T (K) kd ΔGo (kJ/mol) ΔHo (kJ/mol) ΔSo (J/mol K)
298.15 2.93 −2.26 37.1 0.132
308.15 3.26 −3.58
318.15 5.80 −4.89
328.15 11.22 −6.22

The values of ΔS° and ΔH° were determined using the

intercept and slope components of the linear van’t Hoff plot
Figure 8. Adsorption of isotherms of MB dye onto RPDSAC (dosage = 0.1 g, (ln kd vs 1/T) based on the regression parameters as shown
solution pH = 10, temperature = 25 °C, agitation speed = 110 rpm, and volume in Figure 9. The value of ΔG° was estimated using Equation
of solution = 100 mL). (6), as shown in Table 10. The negative change in Gibbs free
energy (ΔG°) observed in Table 10 indicates that the adsorp-
Table 8. The parameters of isotherm models for MB dye adsorption on RPDSAC tion of MB is a spontaneous process. Thus, the positive
(dosage = 0.1 g, solution pH = 10, temperature = 25 °C, agitation speed = change in enthalpy (ΔH°) indicates that the absorption of
110 rpm, and volume of solution = 100 mL). MB species by RPDSAC is an endothermic process (Jawad
Adsorption isotherm Parameter Value et al. 2020). Moreover, throughout the MB adsorption phase,
Langmuir qmax (mg/g) 120.4 a positive ΔS° indicates that the process is driven by entropy
Ka (L/mg) 0.16
R2 0.90 which is supported by the increased randomness at the
Freundlich Kf (mg/g) (L/mg)1/n 30.5 RPDSAC liquid interface.
N 2.93
R2 0.99
Temkin KT (L/mg) 20.08
bT (J/mol) 144.2
R2 0.90 MB dye adsorption mechanism
Multiple interactions, including π–π interaction, electrostatic
Table 9. Comparison of the adsorption capacity of RPDSAC toward MB with
interaction, hydrogen bonding, and pore-filling, contribute
different adsorbents.
to the adsorption of MB by RPDSAC. The literature has
Adsorbent(s) qmax (mg/g) References
identified these interactions as the principal constituents that
RPDSAC 120.4 This study
Banana stem-based AC 101.01 Misran et al. (2022) facilitate the adsorption of MB onto AC (Mahapatra et al.
ACs from furfural residues 562.9 Ao et al. (2021) 2021). The MB adsorption process utilizing RPDSAC is
AC from pineapple crown 292 da Silva et al. (2021) depicted in Figure 10. The BET (Brunauer–Emmett–Teller)
AC from green algae Ulva lactuca 344.83 El Nemr et al. (2021)
Silver nanoparticles loaded on AC 75.2 Ghaedi et al. (2015) and SEM analyses indicate that the RPDSAC possesses a
AC derived from waste orange and 38 Ramutshatsha-Makhwedzha mesoporous structure. Furthermore, it has been determined
lemon peels et al. (2022) that the longitudinal length of MB is 1.43 nm (Mahapatra
AC from stem palm fibers 110.79 Maia et al. (2021)
et al., 2021). This implies that the mesopores within the
RPDSAC structure can be occupied by MB molecules, as
qe illustrated in Figure 10. When the negatively charged surface
kd = (7) of the RPDSAC is exposed to a pH greater than its pHpzc,
Ce
electrostatic interactions with MB cations are facilitated. This
improves the MB adsorption mechanism through the utiliza-
∆S° ∆H ° tion of the generated electrostatic forces. Potential hydrogen
lnkd = − (8)
R RT bonding between functional groups present on the surface of
1664 A. H. JAWAD ET AL.

ORCID
Ali H. Jawad http://orcid.org/0000-0002-4827-9093
Ahmad Hapiz http://orcid.org/0000-0003-3640-0041
Ruihong Wu http://orcid.org/0009-0001-3758-9678
Ahmed Saud Abdulhameed http://orcid.org/0000-0002-6281-5868
Zeid A. ALOthman http://orcid.org/0000-0001-9970-2480

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