Journal of Water Process Engineering 55 (2023) 104219

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Journal of Water Process Engineering

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

Functionalised mesoporous biosorbents for efficient removal of hazardous

pollutants from water environment
Jasmina Sulejmanović a, b, Minela Kojčin a, Mirza Grebo a, Adnan Zahirović a, Anela Topčagić a,
Narcisa Smječanin a, b, Abdullah A. Al-Kahtani c, Farooq Sher d, *
a
Department of Chemistry, Faculty of Science, University of Sarajevo, Sarajevo 71000, Bosnia and Herzegovina
b
International Society of Engineering Science and Technology, Nottingham, United Kingdom
c
Department of Chemistry, College of Science, King Saud University, P. O. Box 2455, Riyadh 11451, Saudi Arabia
d
Department of Engineering, School of Science and Technology, Nottingham Trent University, Nottingham NG11 8NS, United Kingdom

A R T I C L E I N F O A B S T R A C T

Keywords: Wastewater from industrial complexes contains a significant amount of non-biodegradable azo dyes that present
Biosorbents a hazard to animals, plant life and humans. The sorbents from biomass are showing a promising potential for the
Adsorption removal of azo dyes through biosorption. Hence, this research presents the capability of using pomegranate peel
Pomegranate peel
(Punica granatum) as a novel biosorbent for the uptake of azo dye Eriochrome Black T (EBT) from an aqueous
Cost study
Eriochrome Black T
solution. The effective removal of EBT was monitored by adjusting sorption parameters including pH value, mass
Kinetic models of the biosorbent, EBT concentration and consecutively studying the sorption kinetics. The samples of biomass
Wastewater remediation were analysed by various instrumental techniques and physio-chemical methods. After sorption experiments
concentration of Eriochrome Black T was analysed by UV–Vis spectrophotometer. The removal of EBT was found
to be optimal at the pH value of 3 with 100 mg of biosorbent by EBT concentration of 150 mg/L during a contact
time of 90 min at room temperature. Under these conditions, the adsorption capacity was determined as 46.10
mg/g. By examining the adsorption kinetics, it was found that biosorption takes place through a combination of
different mechanisms from which the pseudo-second-order model (r2 = 0.99), takes up the major role. The values
of the correlation coefficients for the investigated models of isotherms show the best agreement with Langmuir's
(r2 = 0.97) and Temkin's (r2 = 0.92) models. The novel data of cost evaluation classifies pomegranate peel as a
low-cost adsorbent with promising potential for the removal of investigated azo dye, while the adsorption
process is economically feasible (0.034$ for the uptake of 1 g dye molecule) paving the way for new biotech­
nological advances in wastewater decontamination.

1. Introduction pollution of water, dyes hinder the transmission of sunlight and thus
reduce the activity of photosynthesis, thereby disrupting the balance in
Water is the most important natural resource and a basic element of the food chain [6]. Of all the different types, azo dyes require special
human, animal and plant life so its proper use and protection are very scientific and technological attention. Azo dyes form the biggest and
important and concern the entire population of the planet. One of the most diverse class of organic, synthetic and aromatic dyes. As xenobiotic
most concerning pollutants which lead to extensive water pollution is chromophores, they contain more azo groups (–N– – N–) as well as
high production and consumption of chemical dyes [1]. Various indus­ sulfonic groups (–SO−3 ) that make them resistant to the oxidative
trial complexes discharge dye-enriched water such as textile [2], food, metabolism of bacteria [7].
cosmetic and leather industries [3]. According to the study by Samsami Consequently, these dyes are very difficult to biodegrade in nature
et al. [4] textile industry is causing over 54% of the entire industrial [8], are subject to bioaccumulation [9] and represent a threat to human
wastewater pollution. Of all the mentioned polluters, the textile industry health and environmental protection because of their carcinogenic and
poses the largest danger as it is heavily dependent on chemical dyes for mutagenic properties [10]. The process of treating all types of waste­
the processing of different kinds of fibres [5]. Aside from the chemical water including those containing azo dyes is often limited by high prices,

* Corresponding author at: Department of Engineering, School of Science and Technology, Nottingham Trent University, Nottingham NG11 8NS, United Kingdom.
E-mail address: [email protected] (F. Sher).

https://doi.org/10.1016/j.jwpe.2023.104219
Received 5 June 2023; Received in revised form 23 August 2023; Accepted 25 August 2023
Available online 1 September 2023
2214-7144/© 2023 The Authors. Published by Elsevier Ltd. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
J. Sulejmanović et al. Journal of Water Process Engineering 55 (2023) 104219

the need to dispose of the resulting harmful sludge or the creation of EBT solution of 1000 mg/L concentration, 1 g of the solid salt of Erio­
toxic decomposition components [4]. Conventional wastewater treat­ chrome Black T was dissolved in a 1000 mL volumetric flask. The stock
ment techniques have proven to be ineffective at removing these solution was then diluted to 10, 20, 30 and 40 mg/L. The potassium
dangerous, persistent and water-soluble chemicals [11,12]. One of the bromide used for recording the FTIR spectra was purchased from Merck
more problematic azo dyes regarding water pollution is the anionic dye (Darmstadt) and other chemicals were purchased from Semikem (Sar­
Eriochrome Black T (EBT). It has a complex chemical structure and ajevo) and Alkaloid (Skopje). The waste pomegranate peel was collected
shows resistance to bleaching when exposed to light and chemicals [13]. as household waste. The collected biomass was combined and manually
Additionally, degradation products of EBT like naphthoquinone are broken into pieces of several cm2. The sorbent was then washed with
highly carcinogenic [14], making the eradication of this dye from water distilled water, air dried and then in an oven at 105 ◦ C. After the process
even more important. of drying, the sample was grounded in a mill and sieved through sieves
Due to the high toxicity of EBT coupled with a rising urgency of of different dimensions. The particle size fraction of 0.25–0.50 mm as
wastewater treatment, many research groups are pursuing the devel­ well as a smaller fraction of particle sizes (< 0.25 mm) were utilized
opment of a wastewater decontamination technique that is efficient, further in this work for the sorption experiments.
fast, affordable and environmentally friendly [2]. Some of the tech­
niques for EBT uptake from wastewater are electrochemical oxidation 2.1. Determination of physicochemical parameters
[15], adsorption using nanoparticles [16] and photocatalytic removal
[17]. However, one of the methods that has garnered particular interest The moisture (at 105 ◦ C) and ash content (at 650 ◦ C) of powdered
is biosorption of wastewater pollutants, including EBT due to its effi­ pomegranate peel were determined by procedures previously described
ciency, low costs and overall simple and easy implementation [18]. The in the study of Nocoń et al. [37]. The content of cellulose in biomass was
adsorbents come from renewable sources, they are biodegradable, easily determined by the Kürschner-Hoffer method [38] from the difference
obtainable and affordable, mostly being fruits like lemon [19] and between the initial mass of the sample and the rest of the mass while the
watermelon [20], industrial waste material [21] or even algal material content of lignin is determined by the Klason method by treating the
[22]. The removal of EBT from wastewater employing biosorption has biomass with H2SO4. Determination of the amount of total proteins was
gained interest in the last few years, promoting researchers to investi­ done by the Biuret reaction [39] and the result was given as mg of al­
gate many biomass-based materials such as macroalgae [23], rice hulls bumin per g of the analysed sample. The content of total phenols was
[24], avocado pear [25] and basil seeds [13]. However, the data on established by the method of Singleton and Rossi [40]. The results are
using fruit-based material is scarce at best, creating opportunities for given as equivalents of gallic acid (mg GAE/g) and represent the non-
some conventionally available materials. Pomegranate (Punica gran­ flavonoid fraction of the phenolic mixture. The content of flavonoids
atum) is a shrub from the Punicaceae family, originally from Iran thrives was established from the concentration of total phenols and non-
in certain Balkan areas such as southern Dalmatia and western Herze­ flavonoids difference [41].
govina making it easily accessible. By the method previously described in the study of Noreen et al. [42]
Pomegranate peel is rich in flavonoids (Mainly flavonols and an­ determination of pHPZC of the powdered pomegranate peel suspension
thocyanins) [26] as well as ellagitannins from which two compounds was performed at room temperature and the values of pHPZC were
characteristic only for pomegranate [27] have been identified. determined from the graph representing the dependence of pHfinal = f
Hydroxybenzoic and hydroxycinnamic as well as catechins and epi­ (pHstart). In addition, the determination of suspension pH was investi­
catechins are also present in the peel [28]. Pomegranate is also rich in gated by mixing 0.2 g of the used sorbent with 30 mL of distilled water in
ascorbic acid [29] and reducing sugars [30]. This data suggests that a closed PVC container and by occasionally stirring for 72 h. The cation
pomegranate peel has various functional groups that could facilitate the exchange capacity (CEC) value is determined by suspending 0.2 g of
process of EBT sorption. The chemical composition of pomegranate biosorbent in 30 mL of 0.1 mol/L NaOH solution in PVC vials for a
makes it a formidable candidate for the biosorption of anionic com­ period of 72 h. After that, the suspensions were filtered and filtrate
pounds, such as phosphates [31] and dyes [32]. It was investigated in its containing 20 mL was taken and pH-metrically titrated with a 0.1 mol/L
native or modified form for the removal of various heavy metals [33] HCl solution. The cation exchange capacity is calculated from the dif­
and some of the dyes such as Rhodamine B [34], Methylene Blue [35] ference in the amount of Na+ ions in the titrated solutions before and
and Basic Red 46 [36], but not for the sorption of Eriochrome Black T. after contact with the biosorbent.
Hence, the current research aimed to explore whether pomegranate The Boehm's titrations were utilized to evaluate the oxygen func­
peel, a common household waste product has the potential to serve as a tional group content on the pomegranate peel surface. Acidic functional
biosorbent for the adsorption of EBT from wastewater. In addition, the groups are determined by shaking 0.5 g of the sample with 30 mL of 0.1
pomegranate peel in its raw form has been characterized by different mol/L solution of Na2CO3, NaOH and NaHCO3. Prepared suspensions
instrumental techniques, analyzing the point of zero charge (pHPZC) and are transferred into PVC vials with stoppers to prevent access to oxygen
physical and chemical composition. The sorption potential was tested by or evaporation of the solution. After shaking for 24 h, the suspensions
investigating selected sorption parameters (pH value, sorbent mass, were filtered and 20 mL aliquot was titrated with a standard HCl solu­
contact time and pollutant concentration), which were then used to tion of 0.1 mol/L concentration. To evaluate the total functional groups
assess the kinetics of the biosorption process on Punica granatum. The which are basic, 0.5 g of the sorbent was added to 30 mL of 0.1 mol/L
results from this study provide a comprehensive view into the possible HCl and after stirring for 24 h, the suspension was filtered as in the
biosorption mechanism of the novel biosorbent based on powdered previous case. Aliquots of 20 mL were titrated with standard NaOH
pomegranate peel, placing this biomass-based material in the category solution having a 0.1 mol/L concentration assuming that HCl has pre­
of powerful biosorbents that are candidates for the remediation of viously neutralized all basic functional groups on the surface. The
wastewater. Furthermore, a detailed comparison of the optimized endpoint of the titration was determined pH-metrically [43].
adsorption process by pomegranate peel as a sorbent as well as a cost
study of the used process was performed to get knowledge about the 2.2. Particle size and active centres
techno-economic relevance of this study.
The wet method, using distilled water as a dispersant, was performed
2. Materials and methods to evaluate the distribution of particle sizes. The particle size distribu­
tion of the pomegranate peel-based biosorbent was analysed with the
All the used chemicals were of analytical grade. Eriochrome Black T laser diffraction method by using Malvern Mastersizer 2000 system
was purchased in powder form from Himedia (Mumbai). To prepare an coupled with Hydro 2000S (A) which enables the determination of the

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J. Sulejmanović et al. Journal of Water Process Engineering 55 (2023) 104219

particle size 0.2–2000 μm distribution. Fourier transform infrared Expenditures (OPEX), and the cost of biosorbent application [48] in an
spectrum (FTIR) was utilized in the 4000–400 cm− 1 spectral range by sorption operation process [49]. A very common, quantitative metric for
using a Perkin Elmer BX FTIR instrument [44]. The correction factor for the comparison of adsorbent cost is the dollar expense of preparing and
spectrum subtraction was set so that the absorbance value at 1100 cm− 1 utilizing 1 g of a biosorbent for the sorption of 1 mol of a pollutant (azo
is equal to zero. The band close to 1100 cm− 1 refers to the vibrations of dye, Eriochrome Black T) from the water phase in accordance with the
the skeletal pyran ring, which are not easily affected by dye adsorption, theoretical point of the chosen analyte maximum removal, called as
so it could be utilized as a point of reference for calculating the spectrum ‘adsorbent cost performance’ (Ĉ), developed by Ighalo et al. [49] was
of difference [45]. Scanning electron microscope analysis (SEM) was used to evaluate the cost study in this research. The calculation is based
done by a scanning electron microscope, model JEOEL JSM-6610 LV as on the conversion of the capacity of adsorption from mg/g to $/mol. The
follows: the biomass sample (pulverized pomegranate peel) was dried cost evaluation and economic feasibility of the above agro waste
for 4 h at a temperature of 105 ◦ C and then the sample was coated with a adsorbent in this research used to adsorb a hazardous pollutant like
very thin conductive layer of gold. The working acceleration voltage was Eriochrome Black T from water has been done for the first time to the
25 keV. Examination of the sample is carried out by recording at best of our knowledge.
different magnifications (×500 and ×1000). Electron-dispersive spec­
troscopy analysis (EDS) was performed with an electron-dispersion 3. Results and discussion
spectroscopy unit [46].
3.1. Chemical composition analysis
2.3. Batch biosorption procedure
Based on the chemical analysis of the pomegranate peel, it was
The general procedure for the sorption of Eriochrome Black T onto determined that it contains a significant amount of lignin and cellulose
(Table 1). That represents the basic structural components of biomass.
powdered pomegranate peel as a biosorbent involved the preparation of
a suspension of 0.1 g of sorbent into 50 mL flask with 40 mg/L con­ Other citrus fruits such as lemons which have been used for the sorption
of Methylene Blue in the study of Dai et al. [50] also showed similar
centration of EBT working solution. Then, the suspension with the
adjusted pH value (3–6) was mixed at 250 rpm of speed for 60 min. The characteristics regarding the chemical analysis. The high content of the
lignin allows the sorbent to be used in a new sorption cycle without a
obtained suspension was filtered and the remaining EBT concentration
in the filtrate and the control sample was analysed on a UV–Vis spec­ visible change in mass after one sorption cycle due to its resistance to
trophotometer at 560 nm. For every round of testing, one of the water, weak acids and bases. In addition, the high content of lignin is
experimental parameters varied while the others were held constant. also responsible for the biosorbent's properties, such as thermal stability
Based on the obtained results, the removal efficiency Reff (%) of dye by and hydrophobicity [51]. The functional groups present in lignin mol­
the used biosorbent was calculated according to Eq. (1) [21] and ecules (hydroxyl, methoxyl, carbonyl and carboxylic groups) could also
adsorption capacity at a certain time, qt (mg/g) was calculated using Eq. contribute to the higher sorption of investigated sorbate. The share of
cellulose was 11.88%, which is favourable for the biosorption processes
(2) [21].
( )
Ci − Cf
Reff = × 100 (1) Table 1
Ci
(a) Chemical composition of powdered pomegranate peel (b) The content of
( ) acidic and basic functional groups determined by Boehm titrations and (c)
Ci − Cf
qt = ×V (2) Proportion of elements present in the questioned peel of pomegranate according
m
to EDS analysis.
where ci and cf are the initial and final concentration (mg/L) of dye in (a) Chemical composition
the filtrate, V is the volume (in L) of the dye solution and m is the sorbent Compound Content (%)
mass (g). For the investigation of the kinetics of the adsorption process,
Lignin 22.34
three models (pseudo-first, pseudo-second-order and intraparticle
Cellulose 11.88
diffusion) were applied. Additionally, for interpretation of the mecha­ Moisture 7.53
nism; Langmuir, Freundlich and Temkin isotherm models based on the Ashes 2.93
equations described by Smječanin et al. [22] were investigated. The Proteins 2.03
coefficient of correlation (r2) was utilized for the assessment of the
experimentally obtained results to fit the investigated process to a ki­
netic/adsorption model. All performed experiments were done in trip­ (b) Functional groups
licate at room temperature and the mean values data have been utilized Acid groups (mmol/g) Base groups (mmol/g)
for the assessment of obtained results. In addition, due to the variation of
Carboxylic 2.68 Total 0.75
the obtained experimental data all results were within the error mea­ Lactones 1.48
surement (±3 %). Phenolic 0.78
Total 4.95

2.4. Cost analysis

(c) Elemental composition
Although there are a lot of successful adsorption processes in the
uptake of hazardous pollutants (i.e. heavy metals, dyes, pesticides etc.), Element Quantity (%)

many studies lack with sections that deal with economic aspects. The C 26.78
most significant factor that defines adsorbent convenience for the usage Cl 0.19
K 0.82
in water remediation regarding other competing and valuable technol­
Ca 0.09
ogies is attributed to the costs of biosorbent preparation and utilization Cu 0.27
[47]. These studies applied different approaches related to the cost study N 0.15
and among others include: the price of raw, native materials, cost Pb 0.22
indices, discounted cash flow, costs of removed adsorbate per gram of O 71.78
Total 100
adsorbent, Annual Capital Expenditure (CAPEX) and Operating

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J. Sulejmanović et al. Journal of Water Process Engineering 55 (2023) 104219

because cellulose makes a certain sorbent chemically and mechanically suspension (pHsus) was determined with a value of 3.90, which corre­
stable and resistant to aqueous solutions. Cellulose is a macromolecule sponds to a higher concentration of functional groups that are acidic in
which in its structure has hydroxyl and carbonyl functional groups and the composition of the biomass. The capacity of the cation exchange
which partially charge is dependent on pH of the solution [52]. (CEC) of the investigated pomegranate peel was found to be 3.37 mmol/
Due to their role in the biosorption of various analytes, there are g. With a higher obtained value of the cation-exchange capacity, greater
many investigated sorbents based on cellulose. Thus, in the study of Basu removal of certain cations from the solution is expected, through the
et al. [52] that used a cellulose from rice husk as a biosorbent and coated exchange process with protons or cations from the inorganic fraction of
it with humic acid it was found that adsorption capacity was 12.41 and the sample. This CEC value is greater compared to other similar sorbents
19.39 mg/g for Ni and Cr. In the current study, the total content of lignin from the literature. In the study of Wang et al. [62] mango seeds were
and cellulose was over 30%, which further indicated that the mentioned applied as a sorbent for the efficient sorption of lead and cadmium ions
sorbent has a high number of different oxygen functional groups that and it was found that mango seeds have a significantly less cation ex­
could be responsible for binding different types of analytes [53]. Hence, change potential of 0.15 mmol/g [62] compared with the current study.
the examined pomegranate peel represents a favourable biosorbent for Given the high value of the cation exchange, the mentioned sorbent can
the biosorption experiments. The amount of moisture in the air-dried, remove cationic species from the solution, meaning that the investigated
powdered pomegranate peel was 7.53%, which assumed that the sor­ biosorbent could be used for the simultaneous uptake of both anionic
bent could be stored in the air without changes such as particle and cationic species from the defined sample [63]. Furthermore, after
agglomeration and changes caused by granulation. A lower percentage finishing the Boehm titrations, the concentrations of acidic and basic
of moisture contributes to a better adsorption power of the biosorbent, functional groups per unit of mass of the native sorbent were calculated
making the pores and channels in the sorbent structure more accessible and the results are shown in Table 1. The results showed that functional
for ions from the solution [54,55]. Furthermore, a lower content of groups which are acidic on the surface of the biosorbent are present to a
moisture will contribute to the increased yield and better quality of the greater extent compared to basic groups.
biosorbent. The total content of acidic functional groups was 4.95 mmol/g of
Compared with the study of Bayuo et al. [54] who found 8.41% which the carboxyl groups represent 2.68 mmol/g and 1.48 mmol/g are
moisture content in the Arachis hypogea husk used as a biosorbent, lactone groups and phenolic groups 0.78 mmol/g. The occupancy of the
pomegranate peel should have better biosorption properties due to the mentioned functional groups on the surface of the biosorbent enables
lower content of moisture. The ash content, corresponding to the inor­ the sorption of the dye ions from the solution, where the sorption
ganic fraction of the composition, has shown a value comparable to mechanism in a neutral and weakly acidic environment is based mainly
orange peel which contains about 4% ash [56]. The inorganic ions are on the mechanism of ion exchange through carboxyl groups and the
mostly incorporated into the highly developed porous structure of the complexes forming through lactone and phenolic functional groups.
biomass. In addition to the above components, the content of total These obtained results are in accordance with the obtained pHPZC and
phenolics was analysed, yielding 0.21 mg GAE/g of biosorbent for the pHsus values, according to which pomegranate peel has more pro­
total phenol content and 0.12 mg GAE/g of biosorbent for the flavonoid nounced acidic properties. Similarly in the study of Pathirana et al. [64]
content. Other biowastes such as peel from tomato has a much higher it was shown that functional groups with acidic properties are respon­
content of total phenolics with the value of 199.35 mg GAE/g compared sible for the capability of several biosorbents and high adsorption ca­
to determined content of phenolics in pomegranate peel [57]. Phenolic pacity for the uptake of lead, copper and cadmium. Pomegranate peel
compounds in any of their forms represent the compounds that are shows a significant acidic character overall, best seen by comparing it
responsible for most of the beneficial properties of pomegranate peel for with other samples of biomass, like biochar which has a noticeably
biosorption. The amount of phenols is greater than the amount of fla­ lower content of carboxylic (0.317 mmol/g), lactone (0.447 mmol/g)
vonoids, although this difference is not very significant, which makes and phenolic (0.420 mmol/g) groups contributing to its acidity [65]. In
pomegranate peel a bad source of phenolics for industrial purposes [58] comparison to lemon peel [66], a well-known source of vitamin C with
and even further strengthens its single role as a potential biosorbent. acidic properties, pomegranate still shows a larger overall amount of
Determination of the particle size distribution supports the claims acidic group available for EBT sorption. The presence of total basic
about the reactivity of the used biosorbent in terms of its active surface functional groups showed a much smaller share of 0.75 mmol/g, which
available for EBT sorption, through knowledge of its particle size. Ac­ could be related to the share of proteins that contain nitrogen atoms in
cording to the results, the largest share consists of large (diameter 0.9 their structure.
μm) and medium diameter (0.5 μm) particles, while the share of small
particles (0.1 μm) is less significant. Only 10% of raw pomegranate peel 3.2. Functional group composition
particles have a diameter < 15 μm and 90% have a diameter of <465
μm. In more detail, from the fraction of particles with a diameter < 465 The characterization of the functional groups of powdered pome­
μm, 50% of the particles are smaller than <150 μm. Compared with the granate peel was performed by FTIR analysis. The resulting spectra
study of Su et al. [59] bisorbent utilized for the removal of Congo red showing the biomass (1) before, (2) after sorption of EBT, (3) the azo dye
and Methylene blue showed an average 27.5 μm particle size distribu­ itself and (4) the differences of the first two bands are shown in Fig. 1.
tion. According to the value of the specific surface of the sorbent in the Although pomegranate peel has a very complex chemical nature, IR
scope of this analysis, which is 0.156 m2/g of sorbent, good surface spectra (1) and (2) are relatively simple and are dominated by bands
adsorption could be expected [60]. The determination of the pHPZC of immanent to pectin molecules [67]. Therefore, pectin is the most
powdered pomegranate peel shows a value of 3.68. Based on the ob­ abundant ingredient in crushed pomegranate peel. Pectin helps in the
tained value, pomegranate waste biomass will be positively charged if efficient sorption of heavy metals [68], which contributes to the positive
the pH value of the solution is lower than the pHPZC and it will attract properties of pomegranate peel as an adsorbent. It was found that iso­
negatively charged ions of EBT. On the contrary, a higher pH value will lated pectin from biowastes such as sugar beet pulp, apples and citrus
make the surface of the sorbent negative (pH > pHPZC), shifting the af­ peels could be modified and used as a very efficient sorbent for pollutant
finity towards positively charged ions from the solution. In comparison removal. Hence, in the study of Jacobin-Kolon [69] hybrid pectin bio­
with another biosorbent used for EBT sorption based on black tea leaves sorbent was found as very efficient for the removal of zinc ions in the
[61], where pHPZC was determined to be 4.6, pomegranate peel provides wide range of pH values from aqueous solution. The very broad and
a narrower range of EBT adsorption with respect to solution pH in terms strong band of absorption located at 3414 cm− 1 is assigned to the O–H
of electrostatic attraction. bond stretching vibrations. After EBT adsorption, this band moves to
In addition to pHPZC, the pH of the powdered pomegranate peel higher wave numbers and appears in the IR spectrum (2) at 3432 cm− 1.

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J. Sulejmanović et al. Journal of Water Process Engineering 55 (2023) 104219

3.3. Morphological analysis

To determine the morphology of native pomegranate peel, SEM and

EDS analyses were done. The obtained results are given in Fig. 2 and
Table 1, respectively. As expected from the PSA analysis, particles of
different shapes, sizes and particle size distribution are observed on SEM
micrographs. In the images, pores, cavities and channels are additionally
visible, which are considered potential locations for pollutants adsorp­
tion as found in the study of Dey et al. [73]. The biosorbent surface is
also smooth and irregular, which is in agreement with the research of
Gunduz et al. [74] who have investigated the removal of Malachite
green by using pomegranate peel as a biosorbent. At a magnification of
×100, these free locations in the form of channels, or pores, are even
more pronounced. The presence of pores and channels in the native peel
of pomegranate facilitates the movement of the aqueous phase through
the very structure of the material, and the binding of analytes with the
surface groups of the lignocellulosic material. In addition to the
mentioned possibilities, they also contribute to intraparticle diffusion,
which is considered one of the possible processes in the binding of EBT
from an aqueous solution.
The results of the EDS analysis showed that the biomass-based
pomegranate peel has the largest amount of carbon and oxygen, corre­
Fig. 1. FTIR spectrum of powdered pomegranate peel; (1) Before, (2) After the sponding to the characterization analysis with FTIR and Boehm's titra­
sorption of EBT, (3) Bare EBT spectrum and (4) Difference spectrum. tions. Similar results were found in the study of Ben-Ali et al. [75] which
used the same sorbent for the removal of copper ions from the aqueous
Two bands located at 2927 and 2856 cm− 1 arise from the stretching solution. The examined sample also contains small amounts of potas­
vibrations of CH methyl and methylene groups. The intensity of these sium, copper, lead and chlorine. Traces of calcium and nitrogen are also
bands was slightly increased after EBT sorption. Two bands of strong present. The similar pomegranate peel composition was also determined
intensity at 1741 and 1622 cm− 1 arise from the vibrations of the in the study of Sulejmanović et al. [76] were pomegranate peel was used
carbonyl residues of galacturonic acid (GAC). The first arises from the as a biosorbent for the preconcentration of seven heavy metals with the
vibrational stretching of ester groups, while the second arises from the difference in nitrogen content which was not found as a constituent of
asymmetric stretching of the free carboxyl group. This region of the IR the biomass. Furthermore, the results of the current study are in
spectrum is particularly useful for estimating galacturonic acid content, agreement with the study of Giri et al. [77] which have investigated the
as the area under these peaks is directly proportional to its content [70]. removal of chromium by also using pomegranate peel as a biosorbent.
According to the obtained calculation, the proportion of GAC in the The content of Ca and K is consistent with the value of the cation ex­
pomegranate peel after sorption of EBT is slightly lower compared to the change capacity, while the value of nitrogen is with the protein amount.
native pomegranate sample (Table 2). The degree of methylation (DM) The percentage of chloride ions can also be beneficial in the case of ion
of the native peel of pomegranate is 75% and it complies with the exchange of the same charge, which favours the removal of EBT.
available literature data [71]. However, the DM value of pomegranate Furthermore, the results correspond with other biomass samples like
peel after EBT sorption abnormally decreases to 40% and is not sugar beet pulp investigated in the study of Nuhanović et al. [21] that
considered relevant, because no decrease in absorption at 2927 and largely consist of carbon and oxygen and which have been used for the
2856 cm− 1 was observed. sorption of pollutants.
The change in the value of DM is a consequence of the fact that the
area under the peak at 1622 cm− 1 after EBT sorption corresponds not 3.4. Biosorption of EBT
only to the carbonyl part but also to the mode of water bending (ν2). This
could be seen from the difference spectrum (3) where a new band at Considering the results of the pHPZC determination, the adsorption of
1656 cm− 1 could be observed, which corresponds to the mentioned vi­ EBT was better in an acidic environment, so pH values were tested in the
bration. The inclusion of water molecules after the sorption of EBT on 3–6 range. The results of the efficiency of the adsorption process (%), as
the crushed pomegranate peel is also evident from a very broad band of well as the adsorption capacity (mg/g) dependence on the pH value, are
low intensity in the 1800–2400 cm− 1 (ν2+ L2) region [72]. This explains shown in Fig. 3. The best results were obtained for a pH value of 3, where
that hydrogen bonding and the inclusion of water molecules could be a removal efficiency of 78% was recorded. The obtained result is in
important for the EBT sorption mechanism on pomegranate peel. The agreement with the pHPZC value, according to that electrostatic attrac­
difference spectrum shows a new band at 1538 cm− 1. This band does not tion of the sorbent (positive charge) and EBT (negative charge) should
originate from the pectin molecule but is assigned to the C–C aromatic be most effective at the pH value of the solution <3.68. At the pH value
vibrations of the accumulated EBT. Sorption processes do not signifi­ of 3, the 15.50 mg/g capacity of adsorption was observed. Hence, the
cantly affect the position and intensity of the bands below 1500 cm− 1. removal efficiency is slightly decreased by changing the pH from 3 to 6,
due to a smaller share of positively charged functional groups on the
sorbent surface with affinity towards EBT ions. For the same investi­
Table 2 gated pH of the solution, a small difference is observed regarding the
Degree of methylation and content of galacturonic acid in dried pomegranate
sorption capacity value.
peel; (1) Before and (2) after EBT sorption.
Therefore, considering all, the sorption processes are much more
A1630/AU A1740/AU A1840–1550/AU DM GAC complex and could include different mechanisms than ion exchange and
(cm− 1) (cm− 1) (cm− 1) (%) (%)
complex formation, because the removal efficiency at pH > 3.68 is also
(1) 21.77 30.06 96.16 75 76 high and uniform. The removal efficiency from pH 4 to 6 was in the
(2) 31.32 13.26 86.20 –a 68
range 73.8–75.1%. In all cases, standard deviations of <3% were
a
40% - Irrelevant for the evaluation of degree of methylation. recorded in the case of removal efficiency, i.e. 0.71 mg/g of sorbent in

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J. Sulejmanović et al. Journal of Water Process Engineering 55 (2023) 104219

Fig. 2. SEM images of powdered pomegranate peel; (a, c) before and (b, d) after sorption of EBT, at magnifications of ×1000 for particle size of 10 μm (a, b) and
×500 for particle size of 50 μm (c, d).

Fig. 3. Effect of the pH value on the efficiency of EBT removal using pomegranate peel showing the adsorption capacity and removal efficiency.

6
J. Sulejmanović et al. Journal of Water Process Engineering 55 (2023) 104219

case of adsorption capacity. Since the differences are not significant in a mostly takes place on the outer surface of the adsorbent. It is important
relative sense, all pH values can be considered as optimal. Therefore, the to emphasize that the increase of adsorbed ions is proportional to the
pH value of the solution was not specially adjusted but was kept within time until the maximum adsorption capacity is achieved. This happens
the limits of pH interval 3–6. In the study of Ali et al. [78] which studied due to the filling of all available adsorption centres, after which time no
the removal of Methylene Blue and Eriochrome black T by activated longer affects the adsorption process.
carbon from the seeds of Datura metal optimal pH values were pH 2 and Therefore, to establish a dynamic equilibrium, but also to monitor
6 established respectively. the influence of higher analyte concentrations, 90 min was selected as
To determine the optimal mass of sorbent during the sorption pro­ the optimal time for the observed process, where the removal efficiency
cess, masses of 100, 200, 300, 400 and 500 mg were tested to obtain the was 74.7% and the adsorption capacity 14.9 mg/g. In this phase, the
best results of adsorption capacity and efficiency of removal that is process is somewhat slower, because fewer effective binding centres are
presented in Fig. 4. With the tested biosorbent mass of 100 mg, the remaining, which are more difficult to access due to the appearance of
highest removal efficiency of 71.1% was achieved. Also, along with the repulsive forces between the dye in the diffusion film of the solution and
stated mass, the highest value of adsorption capacity was recorded with the surface-bound analytes, which results in a slower penetration of the
the amount of 13.38 mg/g. In general, it can be noted that with dye into the pores of the adsorbent and binding on the inner surface. The
increasing mass from 100 to 500 mg, the removal efficiency does not obtained results of the current study are in agreement with the results of
change significantly (≤3%). At the same time, the value of the sorption Choudhry et al. [80] have also established 90 min as the optimal time for
capacity significantly decreases with an increase in mass from 100 to the removal of toxic dye by using nanocomposites biosorbent. Further­
200 mg, after which the change does not exceed 40% of the previous more, it can be noted that with a further increase in the time of the
value. It is expected that by increasing the mass and therefore obtaining sorption process from 90 to 120 minutes, there is no visible change in
more active sites on the surface, the removal efficiency would also in­ both the removal efficiency and the value of the adsorption capacity,
crease. However, due to the limitation of functional groups, i.e. their which has also been shown in the study of Saxena et al. [81] where a
weaker availability on the surface of the biosorbent, EBT finds its way to carbon nanotube-based sorbent was used for the adsorption of toxic dye.
the active centres more difficult, which is the reason that the removal Under the current scenario of increasing pollution levels [82,83], there
efficiency, regardless of the mass of the sorbent, is limited to the is still a need to develop and apply eco-friendly materials to eliminate
maximum value of 71.1%. environmental pollution [84–86]. Therefore, waste biomasses are
A comparable trend was found in the biosorption research of Hadadi excellent for the adsorption of various types of toxic pollutants [87].
et al. [79] which used potato peel for the adsorption of Methylene Blue
and Eriochrome Black T where an increase in removal efficiency, but a 3.5. Kinetics analysis
decrease in adsorption capacity with an increased amount of biosorbent
was noted. The optimal dose of potato peel for the uptake of EBT was Obtained data for the calculated parameters of used kinetics models
around 200 mg. Since it is very important from the economic and are given in Table 3. The experimentally obtained value of equilibrium
technical adaptation of the process to utilise the smallest amount of adsorption capacity of 14.90 mg/g best correlates with the theoretical
sorbent, with which a high value of removal efficiency and adsorption value of adsorption capacity (15.27 mg/g), which was determined by
capacity could be achieved, the optimal mass of the biosorbent was the pseudo-second-order model. Considering that the value of correla­
therefore chosen to be 100 mg. It is important to note that with all tion coefficient was highest for the mentioned model, this model best
mentioned masses, excellent reproducibility of the results was achieved, describes the kinetics of EBT on waste pomegranate peel. In addition, it
which is further confirmed by the values of the standard deviations. To implies the binding of adsorbate particles to the surface of the solid
assess the effect of the analyte-sorbent contact time on the dye sorption adsorbent by establishing certain chemical bonds. In this case, it is
efficiency, the biosorption experiments have been carried out in assumed that the step of the process which is limiting is chemisorption
different durations ranging from 5 to 120 minutes with a 10 minute and the main difficulty that occurs is irreversible sorption. The entire
increase in every new experiment. As given in Fig. 5. an increase in sorption is controlled by the ion exchange process or the exchange of
contact time up to 40 minute s leads to a greater value of removal effi­ valence electrons between the sorbate and the sorbent, according to
ciency and capacity of adsorption. This phase is quite fast, which is most previous studies regarding adsorption kinetics [88]. Hence, sorption is
likely a result of the high initial activity of the biosorbent and adsorption limited by the interaction between the pomegranate peel-based surface
and Eriochrome Black T functional groups [89]. Furthermore, the ki­
netics of adsorption could also be described by the first phase of diffu­
sion model (r2 = 0.98), according to which external diffusion is present,
as well as by the pseudo-first-order model (r2 = 0.92), which states that
the rate of adsorption is in accordance with the free sites number for
analyte binding on the surface of the adsorbent.
In addition, following the intraparticle diffusion model, there is a
dependence on the biosorption rate and the speed with which the
investigated sorbate (EBT) diffuses onto the used biosorbent [90]. From
all the above, the kinetics of biosorption removal of EBT on lignocellu­
losic waste pomegranate peel is a complex combination of several
mentioned mechanisms. The speed of the biosorption process is not only
restricted by the surface interactions but also with the diffusion [89].
The initial concentration of the EBT represents the driving power of the
process of mass transfer among the aqueous and solid phases (bio­
sorbent), after which the process of chemical binding of ions to sorption
centres takes over. Fig. 6 shows the mentioned impact, achieved by
determining the value of efficiency of EBT removal or capacity change in
the pomegranate peel biosorbent. It is assumed that a better removal
efficiency is achieved at lower dye concentrations as there are more free
Fig. 4. Effect of biosorbent mass on the efficiency of EBT removal using active centres to which the dye can bind and thus adsorption equilib­
pomegranate peel showing the adsorption capacity and removal efficiency. rium can be reached more quickly [91,92]. Since the solution is not rich

7
J. Sulejmanović et al. Journal of Water Process Engineering 55 (2023) 104219

Fig. 5. The effect of contact time on the efficiency of EBT removal using pomegranate peel showing the adsorption capacity and removal efficiency.

Table 3
Summary of kinetic parameters adsorption isotherms for sorption of EBT ions on pomegranate peel.
Kinetic models

Pseudo-first order Pseudo-second order Intraparticle diffusion

qe (mg/g) k1 r2 qe (mg/g) k2 r2 k1 r21 k2 r22 k3 r23

5.74 0.06 0.92 15.27 0.02 0.99 0.56 0.98 0.31 0.80 0.12 0.82

Isotherm models

Langmuir model Freundlich model Temkin model

qe (mg/g) KL RL r2 n KF r2 AT r2
81.30 0.015 0.87 0.97 1.14 1.21 0.87 4.70 0.92

in ions, the driving force is weaker and this is the reason that the
removal efficiency is lower, as in our investigation, because the dye
needs more time to find the way to the pores of the adsorbent.
In this case, removing EBT using pomegranate peel as a biosorbent at
a concentration of 10 mg/L, yields to removal efficiency of about 50%.
With a slight increase in EBT concentration, the effect of diffusion on the
adsorption process is observed, whereby the removal efficiency in­
creases slightly and reaches the highest value of 71.63% at 40 mg/L
concentration. At the same time, the value of adsorption capacity was
14.33 mg/g. This trend can be attributed to the higher ionic strength of
the solution and diffusion as a driving force that causes more efficient
penetration of dye molecules to the surface of the active centers and
helps to overcome the resistance in mass transfer between the aqueous
and solid phases. However, with an increase in EBT concentration up to
60 mg/L, a slight drop in removal efficiency is observed, followed by
stagnation (up to 150 mg/L), which indicates that the surface functional
groups are occupied by the dye molecules. Furthermore, there is a
certain repulsion of the same charge on the surface of the sorbent itself
meaning that the only possible mechanism of analyte binding is its
penetration due to constant mixing of the solution and accelerated
Fig. 6. Effect of initial EBT concentration on the efficiency of EBT removal
diffusion only into the pores and channels of the sorbent.
using pomegranate peel showing the adsorption capacity and
removal efficiency. However, the capacity of sorption increases along with the dye

8
J. Sulejmanović et al. Journal of Water Process Engineering 55 (2023) 104219

increase in the solution, because the concentration of the dye in the Table 4
tested aqueous solution is higher. Therefore, the best value of the Comparison of various sorbents for the removal of EBT with the results of the
adsorption capacity was achieved precisely during the dye removal at a current study.
200 mg/L concentration where the value of sorption capacity was 47.50 Sorbent Pollutant Adsorption Optimal Reference
mg/g. The EBT concentration of 150 mg/L is considered the best capacity parameters
compromise between these two variables, with a sorption capacity of (mg/g)

46.10 mg/g and removal efficiency of 60.7%. The data gained for the NaOH-modified EBT 90.71 pH 2–4, m = 20 [95]
utilized isotherm models are shown in Table 3. The values of the linear steel dust mg, T = 25 ◦ C
Tea waste EBT 8.80 pH 2, Cinitial = [96]
correlation coefficients for the three isotherm models suggest that the
200 mg/L, t = 60
Langmuir isotherm model with r2 = 0.97 shows the best correlation with min, m = 11 g/L
the experimental data and it is the best model for evaluation of EBT Surface modified EBT 10.20 pH 3, m = 12 mg, [16]
biosorption onto pomegranate peel within the observed concentration ZnO-NPs t = 30 min, Cinitial
interval. This agreement of the Langmuir model with the experimentally = 6 mg/L
Polyvinyl EBT 2.17 pH 3, Cinitial = 10 [97]
obtained data suggests an involvement of chemisorption for the inves­ alcohol/ mg/L, room
tigated removal of EBT by pomegranate peel. Furthermore, considering starch/ZSM-5 temperature
the value of the separation coefficient (RL = 0.87) and the low KL value zeolite
(0.015), it can be said that the biosorption process is favoured. A very membrane
Pomegranate EBT 46.10 pH 3–6, Cinitial = Current
low value of KL constant is obtained for the sorbents that have high af­
peel 150 mg/L, t = 90 study
finity towards investigated sorbates. Similar, in the study of Smječanin min, m = 100 mg,
et al. [46] very low value of KL (4.5 × 10− 5 L/g) suggested a very high room temperature
affinity for the red beet peel towards uranium ions in investigated bio­
sorption process by using a similar batch procedure.
Hence, for the 100 mg/L of analyte concentration adsorption ca­ 3.7. Techno-economic analysis
pacity was 41.21 mg/g. The obtained low value for KL in the current
study indicates a high affinity of the biosorbent for the investigated dye Since the adsorbent material was collected in a household and was
[93]. According to this model, it is assumed that the biosorbent has free used in its raw form, the cost of biosorbent preparation is estimated only
active centres to which EBT ions from the solution can bind that are by the electricity used for drying Punica granatum (3 h). Furthermore,
homogeneously distributed and that once they are occupied, biosorption the cost of adsorbent utilization in sorption process depends only on the
does not occur further. Therefore, the maximum capacity of biosorption energy consumption of the orbital shaker used for running an adsorption
for pomegranate peel was 81.3 mg/g. Previously mentioned further batch process (90 min). As well as there being no chemical requirements
suggests that there are additional factors that influence the biosorption needed for modification processes for pomegranate peel and similar, all
process, or that sorption takes place by several mechanisms. These data other costs were excluded. The energy costs correspond to the electricity
are in accordance with the data obtained for kinetic analysis, since they costs per kWh used and were based on the average energy price in
revealed involvement as well of several mechanisms, including chemi­ Bosnia and Herzegovina for 2022 (0.024$/kWh). Therefore, the energy
sorption and diffusion. As the results have shown, the sorption of EBT cost in $ has been estimated as the product of an amount of kWh spent at
onto pomegranate peel could be also described by the Temkin model, the price of 1 kWh in Bosnia and Herzegovina, where the study was
due to the value of a high correlation coefficient of 0.92. Given that no performed. The results obtained for the cost of Eriochrome Black T
single adsorption model can completely describe the EBT sorption pro­ removal by pomegranate peel are shown in Table 5 and are compared
cess on the pomegranate peel, it is assumed that the mentioned mech­ with similar research data since there were no other results regarding
anism is highly complex and consists of several steps. However, such the cost study for EBT removal. The comparison was done regarding
findings align with previous studies of biosorbents that show that the similar types of sorbents, the molar mass of the analyte and adsorption
complex nature of the sorption process is due to the effect of many capacity to better understand the cost evaluation and economic feasi­
different sorption parameters that do not act completely in synergy with bility of used waste as an adsorbent in this research.
one another [94]. The resulting data from Table 5 implicate that the use of pome­
granate peel as adsorbent is economically very feasible (0.034$ for the
3.6. Comparison of adsorption parameters uptake of 1 g dye molecule) in comparison to tomato seeds used to
remove Acid Blue 92 [98] or coconut shell biochar and groundnut shell
Table 4 gives different biosorbents and adsorbents for the sorption of for Basic Red 09 [99] removal. However, better cost properties showed
EBT for comparison with the current study. The adsorption capacities modified Bambusa Tulda used to adsorb Crystal Violet [100] and tomato
varied from 8.8 to 90.71 mg/g. Considering obtained adsorption ca­ seed used for Acid Red 14 [98] removal from the water environment.
pacities pomegranate peel (46.1 mg/g) has shown as a very promising Better adsorption properties could be achieved through more active sites
biosorbent. In addition, it has advantages such as it was used in its raw after the modification process of the adsorbent or through the sorbent
form without any chemical treatment. Moreover, it is an abundant and affinity as the main factor. Pomegranate peel, tomato seeds and modi­
environmentally friendly sorbent compared to NaOH-modified steel fied Bambusa Tulda are considered as biosorbents while others are
dust [95]. Furthermore, it was found that all compared sorbents are classified as biochar (coconut shell biochar and groundnut shell biochar)
binding EBT at the acidic pH value of the aqueous solution, which is due [101]. Pomegranate peel is economically feasible and could be consid­
to its anionic form in the solution. The optimal initial concentration of ered a low-cost adsorbent. In addition, this is biodegradable waste and
EBT tested in various studies varied from 10 to 200 mg/L. As found in there is no need for chemical modification to achieve results with
the study of Bansal et al. [96] the biosorbent based on tea waste could remarkable attention for scaling up this adsorption procedure to plant
remove from the aqueous solution 200 mg/L of EBT and pomegranate systems.
peel 150 mg/L, but with a higher adsorption capacity. Thus, considering
other similar studies for the removal of EBT by the means of adsorption 4. Conclusion
process pomegranate peel represents one of the most promising
biosorbents. Pomegranate peel was characterized as a lignin-rich material. The
analysis of native pomegranate peel revealed the presence of pores,
channels and cavities, which, in addition to surface functional groups,

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J. Sulejmanović et al. Journal of Water Process Engineering 55 (2023) 104219

Table 5
Calculated adsorbent cost performance and comparison with published literature.
Adsorbent Target pollutant Adsorption capacity (mg/g) Molar mass (g/mol) Cost per treatment ($/g) Ĉ ($/mol) Reference

Tomato seeds Acid Blue 92 36.23 656.200 0.118 2137.22 [98]

Tomato seeds Acid Red 14 125.00 502.431 0.034 136.66 [98]
Coconut shell biochar Basic Red 09 46.30 237.258 0.141 723.05 [99]
Groundnut shell biochar Basic Red 09 44.00 237.258 0.150 810.99 [99]
Modified Bambusa Tulda Crystal Violet 20.84 407.979 0.0009 17.62 [100]
Pomegranate peel Eriochrome Black T 46.10 461.381 0.034 626.92 This study

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