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© 2023 The Authors Water Practice & Technology Vol 00 No 0, 1 doi: 10.2166/wpt.2023.110

Linear and nonlinear regression methods for isotherm and kinetic modelling of
iron ions bioadsorption using Ocimum sanctum Linn. leaves from aqueous
solution

Praveda Paranjape * and Parag Sadgir

Department of Civil Engineering, College of Engineering, Pune, Maharashtra 415005, India
*Corresponding author. E-mail: [email protected]

PP, 0000-0002-3918-9870

ABSTRACT

Iron concentration in drinking water higher than the recommended value imposes different health problems. There are
advanced chemical-based iron extraction techniques, in spite of having certain limitations in developing countries. Due to
this, iron removal by using locally available plants is a paramount sustainable option. Therefore, the current study was intended
to explore the iron removal efficiency of the powder of Ocimum sanctum Linn. (OSL) leaves from water and investigate its capa-
bility by assessing various conditions of operation. The bioadsorption equilibrium isotherm and kinetics of iron extraction onto
OSL leaf powder were studied and modelled. The experimental adsorption equilibrium observations served as the basis for a
comparison of linear and nonlinear regression techniques for predicting the optimal isotherms and kinetics. The optimum con-
ditions for the extraction of iron were observed to be pH of 5, biomass concentration of 0.2 g, contact time of 2 h, speed of
agitation of 150 rpm at 25 °C temperature, while maximum bioadsorption capacity was 123.26 mg/g. The batch bioadsorption
of iron obeys the Fritz–Schlunde isotherm and the pseudo-first-order-kinetic model. The isotherm and kinetics parameters
obtained using the nonlinear regression method outperformed the linear approach. Moreover, the potential applicability of
OSL leaves-based bioadsorbent could be further examined on a large-scale for industrial application.

Key words: adsorption kinetics, iron removal, isotherm models, linear and non-linear regression, plant based bioadsorbents

HIGHLIGHTS

• The potential of Ocimum sanctum Linn. (OSL) leaf powder for iron removal under various experimental conditions was pre-
sented.
• Maximum adsorption capacity of OSL leaf powder was 123.26 mg/g at pH 5.
• Thermodynamic parameters indicate that the bioadsorption process was possible, spontaneous, and exothermic.
• The comparison of linear and nonlinear regression approaches for isotherm and kinetics modelling was discussed.

This is an Open Access article distributed under the terms of the Creative Commons Attribution Licence (CC BY 4.0), which permits copying,
adaptation and redistribution, provided the original work is properly cited (http://creativecommons.org/licenses/by/4.0/).

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GRAPHICAL ABSTRACT

INTRODUCTION
Since heavy metals are amongst the most harmful pollutants to the environment, researchers have long been
interested in their presence in water and their removal (Ostad-Ali-Askari 2022). Heavy metal-laden toxic waste-
water is being discharged directly or indirectly into water bodies, particularly in evolving countries, and poses a
hazard to the environment because of anthropogenic activities, urbanization, and rapid industrialized develop-
ment, such as metal plating services, mining/ore processing and extraction, fertiliser industries, tanneries,
wood processing industries, battery manufacturing, paper and pulp industries, and pesticides (Celik & Demirbaş
2005; Costa et al. 2021; Gunarathne et al. 2022; Singh et al. 2022). Fluoride, nitrate, salinity, arsenic, iron, and
other heavy metals have been reported to exceed the Bureau of Indian Standards (BIS) permissible limits in some
areas of the country. Groundwater contamination by iron was reported from 301 districts across 26 states (Press
Information Bureau, Government of India 2019). The Central Water Commission (CWC) conducted a study from
May 2014 to April 2018 and reported that iron and copper exceeded tolerance limits in 20 river basins of the
Ganga, Yamuna, and Godavari, along with other metals such as nickel, cadmium, chromium, lead, and so on.
Iron and other metal contamination cases are reported from various states of Rajasthan, Uttar Pradesh,
Punjab, and Tamil Nadu. One of the utmost serious environmental issues is heavy metal-induced aquatic con-
tamination. It has extended relatively more importance, because of its toxicity, persistence, and bio-magnification.
The existence of heavy metals in the ecosystem endangers social well-being and harms organisms that live in it
as well as those that consume it (Brennecke et al. 2016; Indracanti & Gunturu 2019). These heavy metals are said
to be hazardous, causing harm to ecosystems as well as human health, including hypothermia, metabolic acido-
sis, stomach upset and ulcer, liver and brain damage, respiratory problems, mental retardation, tissue damage,
and depression. Metal toxicity creates not only health problems but also an adverse effect on materials causing
staining of laundry and plumbing and slimy coating on the piping because of undesirable iron bacteria growth
(Sheeka Subramani et al. 2019). There are several techniques for the extraction or separation of iron from
water and wastewater, namely, reverse-osmosis technique, ion exchange, chemical precipitation, adsorption tech-
nique, and membrane filtration technique (Fu & Wang 2011; Xu et al. 2021). Many of these methods were no
longer sustainable for removal processes. Bioadsorption can be distinguished as the elimination of components
from the arrangement by natural or biological materials (such materials can be inorganic and organic and in gas-
eous/vaporous form, insoluble or soluble/solvent structure). Isotherm adsorption studies were used to predict the

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ability of particular adsorbents to remove contaminants in the affluent approach. The lack of modern water treat-
ment systems and a lack of skilled workers lead to water contamination and a lack of drinkable water. This study
was prompted by the need for low-cost options for water and wastewater treatment. Because traditional or
advanced pollution removal is impossible, low-cost water treatment options are needed for affected areas in sev-
eral developing countries with poor economic conditions. Nowadays, bioadsorption is an emerging technology as
it utilizes the inactive waste biomass (plant-origin biomass such as leaves, steam, seeds, shells, and agricultural
waste) as an adsorbent in the adsorption process and provides maximum efficiency even at lower concentrations
(Anselmo et al. 2022). The use of low-cost or economical products has become necessary in latest years due to the
requirement for safe and economical approaches (De Gisi et al. 2016; Kim & Singh 2022). The requirement for
safe and cost-efficient methods has necessitated the use of low-cost plant -origin biomass like Calabrian pine bark
(Acemioǧlu 2004), tea leaves (Ahluwalia & Goyal 2005), Typha domingensis leaves (Abdel-Ghani et al. 2009),
green clover leaves (Mem 2017), olive leaves (Elsherif 2017), Moringa oleifera seed (Abbas 2018), banana peel
(Shrestha 2018a), pineapple peel (Izzati et al. 2018), and Launea procumbens leaves (Indracanti & Gunturu
2019), and agricultural by-products such as Cajanus cajan husk (Ahalya et al. 2007), pecan nutshell (Vaghetti
et al. 2014), saw dust (Shrestha 2018b), hazelnut hull (Sheibani et al. 2012), and peanut hull (Awad 2017) in
recent years. These are natural assets with a huge bioadsorption capacity for heavy metal expulsion from
water or wastewater (Sharma et al. 2021).
Plants are considered to be an important source of medicine, and many drugs in use are derived from them, e.g.
Ocimum sanctum Linn. (OSL) commonly known as Tulsi. Traditionally, O. sanctum is consumed as fresh leaves,
dried powder, and herbal tea. O. sanctum is said to have a number of medicinal properties. It is a general vitalizer
that improves physical endurance. Several recent studies on these extracts have revealed that they have anti-stress
and anti-inflammatory, antioxidant, and immunemodulatory properties. In ayurvedic medicines, its extracts are
used to treat headache, inflammation, common colds, stomach disorders, heart disease, malaria, and various
forms of poisoning. It has also been proven to have anti-carcinogenic and radioprotective properties (Sreelakshmi
2017; Anitha 2018).
The current study directs to validate the viability of using OSL leaf powder as a bioadsorbent for iron ion elim-
ination from aqueous solutions. The uptake of iron ions by OSL leaf powder was investigated in this study under
various initial conditions (pH, bioadsorbent dose, bioadsorbent time, and metal concentration). To interrelate the
experimental observations and to calculate the parameters of kinetics models such as pseudo-first-order model
(PS1) and pseudo-second-order model (PS2), power function equation or model and Elovich model were applied.
Two-parameter isotherm models like Langmuir, Freundlich, and Temkin; three-parameter isotherm models like
Redlich–Peterson, Sips, and Toth; four-parameter models like Baudu and Fritz–Schlunder; and five-parameter
model like Fritz–Schlunder were employed to study the bioadsorption equilibrium statistics.
Linear regression is the most commonly adopted method to decide the best-fitting model for adsorption iso-
therm and kinetics along with the respective model parameters. However, the error distribution shifts to either
the worst or the best depending on how the isotherm as well as kinetic equations are linearized. Therefore,
many researchers employ the nonlinear regression approach to establish the parameters of bioadsorption
isotherm and kinetic. The reduction of dispensing errors between the experimental observations and the
forecasted isotherm serves as its foundation. The evaluation of isotherm data makes use of a number of
error functions like the sum of square of errors (ERRSQ), the sum of absolute errors (EABS), the average
relative error (ARE), the mean square error (MSE), the root-mean-square error (RMSE), and coefficient of
determination R 2.
The thermodynamic parameters were analysed to study the adsorption process. Hence, the present work
focuses on removal of iron using OSL leaf powder as bioadsorbents.

MATERIALS AND METHODS

Adsorbate preparation
The stock iron solution was prepared by slowly adding 20 ml H2SO4 to 50 ml of distilled water (or di-ionized
water) and then dissolving the 1.404 g of ferrous ammonium sulphate (Fe (NH4)2 (SO4)2.6H2O). After that,
0.1 M potassium permanganate (KMnO4) was added dropwise until a faint pink solution is formed, and then
it was diluted to 1,000 ml using deionized or distilled water (APHA 2017). By diluting the stock iron metal ion
solution, the essential initial concentration solution was prepared.

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Bioadsorbent preparation
Bioadsorbent materials, i.e. OSL leaves in natural form, were washed by using distilled water (three to four times)
to eliminate dust or dirt and any other surface contaminations. They were dried at room temperature in a clean
and neat space. After that, they were dried in an oven at 60–80 °C (Shah et al. 2017). Dried adsorbents were
ground and powdered using mixer and sieved through 180 μm sieve and stored in a container (labelled as
OSL leaf powder) for further experimental use.

Adsorbent characterization
To determine physiochemical characteristics of the OSL, biomass analytical techniques were used. The mor-
phology of OSL leaves biomass was observed using a scanning electronic microscope equipped with an
energy-dispersive spectroscopy (SEM-EDS) analyser on a ZEISS-Sigma IV instrument. The Rigaku miniflex-
600 instrument (having Cu Kα radiation at 40 kV and 30 mA over the range (2θ) of 20–80°, with a scanning
rate at 2° per minute) was utilized to obtain X-ray diffraction (XRD) patterns. Fourier-transform infrared spec-
troscopy (FT-IR) bands of raw and metal-laden biomass were recorded to identify the functionalities being
capable of interacting with iron ions in biomass using 400–4,000/cm spectrum on a Shimadzu IR affinity with
ATR having a resolution of 4/cm.

Optimization of the factors affecting the removal of iron

Ph
To observe the impact of pH (Labindia PICO þ model used to measure pH) on the uptake percentage of iron
through media by OSL leaf powder, aliquots (100 ml) comprising 0.01 g/l of the iron metal ion were shifted to
a set of 250 ml conical flasks having 0.5 g of the OSL leaf powder adsorbent separately. By using 0.1 N HCl
and 0.1 N NaOH solutions, the pH of each flask was adjusted between 2 and 8 and stirred at 150 rpm for
120 min at 25 °C. The biomass was disassociated from the solution by filtration, and the resulting solutions
were analysed for iron by using UV-VIS spectrophotometer (Shimadzu UV1900 model was used) as mentioned
in APHA (2017).
The adsorption percentage or removal efficacy of the metal ion by the OSL leaves powder is calculated from
the following relation:

Removal efficiency ¼ e(%) ¼ [(Co  Ce )=Co ]  100

where Co is the initial concentration of metal ions (mg/l) and Ce is the ¼residual concentration of metal ions (mg/l).

Adsorbent dose
The influence of adsorbent dose, i.e. OSL leaf powder, was calculated, with adsorbent doses varying between 0.1
and 0.6 g/l. The samples were agitated for 120 min at 150 rpm at 25 °C temperature considering predefined pH,
and residual concentration was analysed as mentioned earlier.

Time of contact
For contact time ranging between 15 and 180 min, the consequence of variation in contact time on iron ion
uptake was observed with the predefined pH and bioadsorbent dose (OSL leaf powder) at 150 rpm at 25 °C temp-
erature. The residual concentration was analysed as mentioned earlier.

Initial metal ion concentration

The impact of the initial concentration of the solution of iron metal ions was examined by varying the concen-
tration of the iron ion solution from 0.005 to 0.05 g/l. Predefined iron ion solutions containing varying
concentrations of iron metal ions were diluted from the stock of 0.2 g/l iron standard solution (APHA 2017).
The mixtures were stirred at predefined pH for 120 min at 150 rpm at 25 °C, and residual concentration was ana-
lysed as mentioned earlier.

Temperature
The impact of the temperature on the uptake of iron ions was observed at different temperature ranges varying
from 25 to 50 °C. The 10 mg/l initial concentration iron ion sample was agitated at predefined pH, adsorbent
dose, and contact time at 150 rpm, and residual concentrations were analysed as mentioned earlier.

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Isotherm experiments
Experiments of isotherm were performed in batch approach. A total of 100 ml iron metal ion samples with vary-
ing initial iron ion concentrations of 0.01–0.05 g/l and predefined pH were transferred into 250 ml Erlenmeyer
flasks. To these solutions, predetermined quantities of the OSL leaf powder bioadsorbent were added. The mix-
tures were stirred for 120 min at 150 rpm at 25 °C. The biomass was disassociated from the solution by filtration,
and the resulting solutions were analysed for iron by using UV-VIS spectrophotometer. By using the following
equation, the remaining metal concentration in the sorbent component (i.e. adsorption capability (qe) measured
in mg/g) is determined:

qe ¼ (Co –Ce )V=m

where Co and Ce are the initial and final (equilibrium) metal ion concentrations in solution (mg/l), V is the volume
of sample (l) and m is the adsorbent mass (g).

Kinetics experiments
The time of contact required to attain equilibrium was determined through kinetic experiments. A total of 10 mg/l
initial iron metal ion solutions (100 ml volume) were mixed with 0.2 g of OSL leaf powder adsorbent. Sorption
experiments were conducted (at constant temperature) in flasks placed in an orbital shaker at 150 rpm till equili-
bria were attained. Metal concentrations were determined by collecting samples at predetermined intervals.
(Unless otherwise mentioned, all experimentations were performed in triplicate. The average of results was
taken from replicated tests conducted at the same temperature.)

Modelling
Isotherm modelling
A variety of models are available in the literature to describe sorption equilibrium. The different models are used
in this study: two-, three-, four-, and five-parameter models. The isotherm model’s equations and assumptions are
listed in Table 1.

Kinetic models
A variety of models are mentioned in the literature to describe kinetics. In this work, PS1, PS2, power function
equation or model, and Elovich model were utilized to co-relate statistics. Table 2 summarises the equations and
assumptions of the kinetics models.

Regression analysis and error function

The OriginPro 2022 Software (version 9.9, OriginLab Corporation, MA) was utilized for the kinetic and isotherm
models’ linear and nonlinear regression analyses. ERRSQ, EABS, ARE, MSE, RMSE, and determination coeffi-
cient R 2 were implemented to examine the adequacy of each isotherm and kinetics model quantitatively (using
Excel), in the present study. Table 3 summarises the equations of error functions.

Thermodynamic parameters
The thermodynamic factors like ΔG (Gibb’s free energy), ΔH (Change in enthalpy), and ΔS (Change in entropy)
for bioadsorption of the iron ions by OSL leaf powder were determined by the following equations:

DG ¼ RT ln K
DG ¼ DH  T DS
ln K ¼ (DS=R)–(DH=RT )

where ΔG is Gibb’s free energy (KJ/mol), K ¼ qe/Ce ¼ distribution coefficient for the adsorption (g/l), qe ¼ bio-
sorption capacity at equilibrium (mg/g), Ce is the residual concentration of metal ion at equilibrium (g/l or
mg/l), R is the universal gas constant ¼ 8.314 (J/mol K), T is the absolute temperature (K), ΔH is the change in
enthalpy (KJ /mol), ΔS is the change in entropy (J/mol K).
The experimental data were utilized to calculate the values of Gibbs free energy (ΔG) for various temperatures.
The values of enthalpy change (ΔH) and entropy change (ΔS) were derived using slope and intercept of the graph
of ln K versus 1/T.

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Table 1 | Isotherm models and their assumptions

Sr.
No. Model Equation Remarks/assumptions

1 Two-parameter model
Langmuir isotherm 1=Ce ¼ b þ qmax b1=qe (linear) • Monolayer adsorption over a surface with a
qe ¼ qmax [(b  Ce )=(1 þ b  Ce )](nonlinear) finite number of like sets or sites.
qmax ¼ Capacity of maximum adsorption • Adsorption energy is uniform (Langmuir
Ce ¼ Residual concentration at equilibrium 1917).
b ¼ constant • Constant signifies the affection between
metal ions and bioadsorbent.
Freundlich isotherm logqe ¼ logK þ 1=n log Ce (linear) • It takes surface heterogeneity and multi – layer
qe ¼ K  C 1=n (nonlinear) bioadsorption to the binding sites on the
K ¼ constant for bioadsorption equilibrium sorbent’s surface into account.
n ¼ constant (revealing of bioadsorption • This model does not take biosorbent
intensity) saturation into account (Freundlich 1906).



Temkin isotherm RT RT • The isotherm model is used for the
qe ¼ InAT þ In Ce (linear)
bT bT characterization of the chemisorption system.


RT • It is applied only for a moderate
qe ¼ InAT Ce (nonlinear)
bT concentration range of metal ions (Shahbeig
et al. 2013).
2 Three-parameter model
Redlich–Peterson ln (KRP Ce =qe –1) ¼ gln (Ce ) þ ln (aRP )(linear) • At low metal concentrations, it takes into
isotherm q ¼ (KRP  Ce )=(1 þ aRP  Cb )(nonlinear) account Henry’s law, and at high
kRP, aRP, and b ¼ R–P parameters concentrations, it resembles the Freundlich
isotherm model (Krishna Prasad &
Srivastava 2009).
Sips isotherm bS ln Ce ¼ ln (KS =qe ) þ ln aS (linear) • It combines the Langmuir and Freundlich
qe ¼ KS [CebS =(1 þ aS  CebS )(nonlinear)] models.
KS ¼ Constant for sips isotherm (l/g) • At low adsorbate concentrations, it follows
aS ¼ Constant for sips model (l/mg) the Freundlich isotherm model, whereas at
βS ¼ exponent of sips isotherm higher adsorbate concentrations, it obeys the
Langmuir isotherm model (Saadi et al. 2015).
Toth isotherm In (qe =KT ) ¼ ln(Ce )–1=t ln (aT þ Ce )(linear) • It can be employed for the modelling of
qe ¼ (KT Ce )=(aT þ Ce )(1=t)(nonlinear) numerous heterogeneous and multilayer
KT ¼ Toth constant for equilibrium adsorption systems.
aT ¼ exponent for Toth isotherm • It is commonly used to describe various gas
adsorption processes and the adsorption of
organic compound vapour (Staudt 2005).
Furthermore, the Toth isotherm model
equation can describe data behaviour at high
and low concentrations.
3 Four-parameter model
Fritz–Schlunder qe ¼ (K1 Ce^ a)=(1 þ K2 Ce^ b) • It is a Langmuir–Freundlich type equation that
isotherm K1 and K2 ¼ F-S model constants allows for a broad range of experimental
α and β ¼ F-S model equilibrium constants observations to be incorporated (the isotherm
contains a large number of coefficients)
(Ayawei et al. 2017).
Baudu isotherm qe ¼ qm KCe^(1þxþy) =1 þ KCe^(1þm) • It was discovered that evaluating the
K ¼ Baudu model’s equilibrium constant Langmuir coefficients (b and qm) at various
x and y ¼ Baudu model’s parameters equilibrium concentrations revealed that
these coefficients do not remain constant
over a wide range of concentrations. As a
result, the Langmuir isotherm was reduced to
the Baudu isotherm.
• The range of (1 þ x þ y) , 1 and (1 þ x) , 1
is covered by this isotherm model. The
Freundlich isotherm model replaces this
model when surface coverage is low (Nemr
et al. 2010).

(Continued.)

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Table 1 | Continued

Sr.
No. Model Equation Remarks/assumptions

4 Five-parameter model
Fritz–Schlunder qe ¼ (qm K1 Ce^ a)=(1 þ K2 Ce^ b) • It is an empirical model that can accurately
isotherm K1 and K2 ¼ F-S model constants simulate model variations and be used with a
m and n ¼ F-S model equilibrium constants wide range of equilibrium statictics/data
(Ayawei et al. 2017).
When α and β ¼ 1, Compared to the
Freundlich isotherm model at higher
adsorbate concentrations, this model is
comparable to the Langmuir isotherm.
Note: qe ¼ capacity of adsorption (measured in mg/g).

Table 2 | Kinetics models and their assumptions

Sr.
No. Model Equation Remarks/Assumptions

1 Pseudo-first qt ¼ qe (1  ek 1 t ) • The adsorption rate is corresponding to the number of

order K1 ¼ Rate constant for pseudo-first empty sites by the solutes.
order (/min) • It only appears to work well in areas where the
bioadsorption process takes place quickly (Ho & Chiang
2001).
2 Pseudo-second qt ¼ qe [(qe k2 t)=(1 þ qe k2 t)] • (Ho & McKay 1999) discovered that using the Lagergren
order K2 ¼ Rate constant for pseudo- model to estimate biosorption kinetics is not appropriate
second order (/min) for the complete adsorption period.
3 Power function qt ¼ ktn • It is a quantitative representation of the relationship
equation k and v ¼ adjustment parameters between sorbate mass/unit adsorbent mass of adsorbent
(mg/g/min) and contact time.
4 Elovich’s qt ¼ (1=b)ln (abt þ 1) • The rate of adsorption reduces exponentially as the
equation a and b ¼ constants quantity of adsorbed solute increases.
• The graphical aids in identification of the type of
bioadsorption occurring on the heterogeneous superficies
of the adsorbent, either chemisorption or not (Wu et al.
2009).
Note: qt ¼ capacity of adsorption at time t (mg/g); qe ¼ capacity of adsorption at equilibrium (mg/g).

Table 3 | Error functions and their mathematical expressions

Sr. No. Error function Mathematical expression/formula References

1 ERRSQ Sni¼1 (qec  qem )2i Foo & Hameed (2010)

2 EABS Sni¼1 jqem  qeC j Nebaghe et al. (2016)
 
100 n qem  qec 
3 ARE Si¼1  Nemr et al. (2010)
n qem 
1 X n
4 MSE [qem  qeC ]2 Nemr et al. (2010)
n  1 i¼1
sffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffiffi
5 RMSE 1 X n
Nemr et al. (2010)
[qem  qec ]2
n  1 i¼1

Note: qem ¼ experimentally measured values of bioadsorption capacities (mg/g), qec ¼ computed values of bioadsorption capacities (mg/g), n ¼ no. of data points.

RESULTS
Adsorbent characterization
The SEM-EDS was utilized to explore the OSL leaf powder’s surface morphology. Uneven and micro-porous
structures were noticed in the OSL leaf powder (Figure 1). It signifies that the surface of SL leaf powder is a

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Figure 1 | SEM and EDS results: (a) SEM image of OSL leaf powder before adsorption, (b) SEM image of OSL leaf powder after
adsorption of iron ions, (c) EDS analysis of OSL leaf powder before adsorption, and (d) EDS analysis of OSL leaf powder after
adsorption.

mixture of small and large particles, is heterogeneous, is rough, and has crater-like pores – a structure that was
suggested to be suitable for metal ion bioadsorption (Bhattacharyya & Sharma 2004). It was clearly seen that
there was a considerable modification in morphology of biosorbent after and before iron ions binding, which
was verified by the energy-dispersive spectroscopy (EDS) result (Figure 1(a) and 1(b)). A similar study was carried
out using Tribulus terrestris seed powder for the extraction of iron ions by Sasikala & Muthuraman (2016), and
the morphological changes before and after the adsorption of iron ions were observed.
EDS results of OSL leaf powder revealed the presence of C (53.20%), O (41.50%), Ca (1.85%), Ga (1.57%), Zn
(1.06%), and Fe (0.83%) (as shown in Figure 1(c)). In the EDS spectrum of OSL leaf powder after bioadsorption
(Figure 1(d)), two new peaks of iron were found to have appeared. This demonstrates that iron ions are present on
the surface of OSL leaf powder. In addition, it can be seen that the distribution of the brighter areas is not uni-
form, signifying that only a limited number of functional groups were taking part in the bioadsorption of iron ions.
It was determined from the SEM and EDS results that OSL leaf powder can absorb iron ions.
XRD is the most effective method for obtaining the structure of materials (amorphous and crystalline). The
XRD observations comprised distinct, broad peaks at 2θ ranging from ∼20 to 25° (reflection of (002) graphite
plane) and a weak peak at ∼40 to 45° (reflection of (001) graphite plane). The broad initial peaks concentrated
at ∼22° are associated with a lower reflection compared with graphite, thus revealing a noteworthy level of inter-
layer spacing. The XRD patterns of the OSL biomass before and after the bioadsorption process are presented in
Figure 2. XRD of the biomass showed that it was amorphous (indicating that large surface area and pore volume),
and because of this property, metal ions can simply infiltrate its superficies. In contrast to raw OSL biomass, the
results after the bioadsorption of iron ions indicate variations or fluctuation. This will possibly lead to the precipi-
tation of iron ions in their mineral or hydrolysed forms (Venkata Ramana & Min 2016; Sheeka Subramani et al.
2019).

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Figure 2 | XRD pattern of OSL leaf powder before and after adsorption.

FT-IR analysis comprises the chemical characterization of OSL biomass before and after the bioadsorption pro-
cess as shown in Figure 3.
Table 4 shows the peaks extracted from FT-IR spectra. C-H, O-H, C-O, C ¼ O, and C ≡ O functional groups
were likely to be participating in the bioadsorption process of iron ions on OSL leaf powder. Along with the
said group when OSL leaf powder biomass loaded with iron ions, a significant change in peaks was not observed.
On the basis of FT-IR spectra, we can conclude that the chemical nature of the OSL leaf powder bioadsorbent
remains almost the same after iron adsorption (Nair et al. 2013; Mandal & Bhattacharya 2015; Sakuntala
et al. 2019).

Influence of pH
It is worth noting that hydronation of performing moieties (e.g. carboxyl and amino groups) in biomass and also
metal chemistry, i.e. its solubility, can be influenced by pH. Figure 4(a) shows metal uptake which tends to
increase with an increase in pH. Adsorption capacities accomplished their maximum at pH levels around 5
for OSL leaf powder pH (experimental conditions: bioadsorbent dose ¼ 0.5 g/l, initial concentration ¼ 0.01 g/l,
time of contact ¼ 120 min, temperature ¼ 25 °C, agitation speed ¼ 150 rpm). The removal % of the iron ions
increases when pH increases from 2 (27.62%) to 5 (75.85%). When the pH dropped, proton concentrations
increased, and counteraction for binding the involved effective sites on the biosorbent’s superficies by Hþ and
metal ions has begun. The bind metal could not be bound by protonated active sites. As a result, free ions
remain in the solution. Once the initial pH of the solution was increased above 5, iron ions precipitated
owing to the presence of a greater concentration of hydroxyl anions in the media. Hence, further experimen-
tations were performed at pH 5.

Influence of bioadsorbent dose

The number of biosorption sites available is determined by the amount of adsorbent used. Figure 4(c) depicts the
effectiveness of biosorbent concentration on metal elimination efficacy and adsorption ability. The bioadsorption
of iron ions was perceived to increase (with an increase in the biosorbent quantity, an increase in biomass of

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Figure 3 | FT-IR spectrum of OSL leaf powder before and after adsorption.

Table 4 | FT-IR peaks and their tentative assignments

FT-IR peak positions (/cm)

Biomass Before adsorption After adsorption Tentative assignment

OSL leaf powder 3,332.99 3,332.99 Surface hydroxyl (O-H) stretching bond
2,924.08 2,924.08 C-H (asymmetric) stretching of CH2 of alkane group
2,854.64 2,854.64 Symmetric C-H stretching of CH2 of alkane group
1,612.49 1,612.49 C ¼ O bond stretching of vibration of derivative of amide groups
C ≡ O bond stretching of aromatic groups
1,081.41 1,081.41 Carboxyl (C-O) stretching vibration of secondary alcohols

surface area was observed along with the number of potential binding sites at higher doses) linearly with increas-
ing bioadsorbent concentration up to 0.2 g (removal rate is 97.03%). After this dosage, the removal efficiency
decreases. The adsorption capability (mg/g) of the OSL leaf powder decreases from 89.13 to 8.31 as a dose of
bioadsorbent increases from 0.1 to 0.6 g, which may be due to the unsaturation of the active bioadsorbent
sites during the processes (experimental conditions: pH ¼ 5, initial concentration ¼ 10 mg/l, contact time ¼
2 h, temperature ¼ 25 °C, agitation speed ¼ 150 rpm).

Influence of contact time

The usual bioadsorption kinetics show a quick initial metal uptake followed by a slower process. The extraction
of iron ions increases with an increase in contact time. Figure 4(b) shows that up to 30 min of contact, there was a
rapid extraction of iron ions (65.15%). Finally, the extraction decreases after 120 min. Thus, 120 min contact time
was used for further studies. The maximum removal of 98.91% was observed within the first 120 min for OSL leaf
powder biomass (Figure 4(b)). As contact time increases, the bioadsorption capability (in mg/g) was observed to

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Figure 4 | Influence of variation of parameter on adsorption of iron by OSL leaf powder: (a) pH, (b) contact time, (c) adsorbent
dose, (d) initial metal concentration, and (e) temperature.

increase (from 21.70 to 42.48). The experimental conditions applied were as follows: pH ¼ 5, initial concen-
tration ¼ 0.01 g/l, bioadsorbent dose ¼ 0.2 g/l, temperature ¼ 25 °C, speed of agitation ¼ 150 rpm.

Influence of temperature
The removal efficacy and uptake of iron ions of OSL leaf powder were influenced by temperature (Figure 4(e)).
Both the removal efficiency and adsorption capability decrease with an increase in temperature. The separation
efficiency of OSL leaf powder decreases from 98.76 to 88.23% with an increase in temperature from 25 to 50 °C.
The adsorption efficiency (mg/g) decreases up to 44.11 as the temperature increases to 50 °C.

Kinetics of adsorption
Kinetics models can be utilized to fit experimentation statistics to study the bioadsorption kinetics of iron metal
ions (Figures 5 and 6). To determine the model parameters, kinetic models having diverse reaction orders were
utilized, and linear as well as nonlinear regression fittings were carried out by using origin pro 2022 software.

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Figure 5 | Bioadsorption kinetics of iron ions on OSL leaf powder – linear: (a) pseudo-first order, (b) pseudo-second order,
(c) power function equation, and (d) Elovich model.

Figure 6 | Bioadsorption kinetics of iron ions on OSL leaf powder – nonlinear.

The experimental results for bioadsorption kinetics of iron ions on the OSL leaf powder were linked to kinetic
models, permitting the parameters of these models to be determined as shown in Table 5 (linear and nonlinear).
Co-relation coefficients and error functions agreed to evaluate the model’s co-relation with the experimental data.
The power function equation or model and Elovich model fail to adequately describe the experimental statistics;
the other two models perform better, for defining the iron ion adsorption on OSL leaf powder in both linear and
nonlinear forms.

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Table 5 | Kinetic model parameter obtained by linear and nonlinear regression

Error functions/kinetics model Parameter R2 ERRSQ EABS ARE MSE RMSE

Linear
PS1 Constant K1 (/min) 0.0152 0.99 0.17 1.06 0.15 0.017 0.133
qe,cal (mg/g) 23.87
PS2 Constant K2 (/min) 0.0013 0.98 0.57 1.26 5.59 0.05 0.239
qe,cal (mg/g) 50
Power function equation k 12.28 0.85 12.78 8.09 50.78 1.27 1.13
v 0.264
Elovich model a (mg/g/min) 10 0.88 52.26 10.79 21.44 5.22 2.28
b (g/mg) 0.103
Nonlinear
PS1 Constant K1 (/min) 0.0418 0.9977 0.15 0.83 0.19 0.01 0.12
qe,cal (mg/g) 45.42
PS2 Constant K2 (/min) 0.0011 0.9909 3.68 4.21 0.95 0.36 0.60
qe,cal (mg/g) 51.04
Power function equation k 14.95 0.954 51.59 15.66 3.63 5.15 2.27
v 0.22
Elovich model a (mg/g/min) 9.839 0.968 43.216 14.48 3.32 4.32 2.07
b (g/mg) 0.11

The PS1’s R 2 values were observed to be high, i.e. (.0.99), in the case of linear analysis, while they were low for
the PS2, power function model/equation, and Elovich model. More than the other mentioned kinetic models, the
ERRSQ values confirm the close fitting of the experimental observations with the PS1. Consequently, linear
regression was observed to be the most appropriate method for defining the kinetics of iron adsorption into
OSL leaf powder in the PS1.
The nonlinear forms of all said kinetic models showed higher R 2 values than the linear forms. In addition, the
values of the ERRSQ values were lower compared to the linear forms, across the entire range of experimental
observations. The linear and nonlinear kinetic parameters of the PS1 and the PS2 were observed to vary slightly
(Table 5). However, when the nonlinear equations’ error function values were examined, it was discovered that
they were lower than the linear form’s error function values. The comparability of experimentation results with
model statistics discovered a convincing correlation between the experimental observations and the PS1, which
was confirmed to be the superlative for explaining bioadsorption kinetics of iron ions on the OSL leaf powder.

Isotherm modelling
The inter-relationship among the quantity of the bioadsorbed constituent per bioadsorbent quantity and the con-
centration of this constituent in the solution is represented by bioadsorption isotherms. The estimation of
equilibrium parameters affords important facts and statistics that can be used to design future adsorption struc-
tures or systems.
The established adsorption isotherm models were preferred to apt the experimental figures on iron metal ion
bioadsorption on the superficies of biomass. Because the procedure was multifaceted and included numerous
physical and chemical interactions, the bioadsorption isotherm was characterized by various models
(Figures 7–11).
The experimental statistics was compared with 3 two-parameter, 3 three-parameter, 2 four-parameter, and 1
five-parameter models that described the bioadsorption equilibrium of iron ions on OSL leaf powder are given
in Table 6 (linear) and Table 7 (nonlinear).
Table 6 shows a comparison of the results of the isotherm by the linear method. The close-fitted isotherm is
chosen using error functions based on the error functions that resulted in a lower error between the experimental
and calculated amounts of iron bioadsorbed and a higher correlation coefficient. When the error equations
(ERRSQ, EABS, ARE, MSE, RMSE, and R 2) were taken into consideration, the Langmuir isotherm model
was found to have the lowest error values. In the linear method, the Redlich–Peterson isotherm, Sips and
Toth isotherm, Freundlich isotherm, and Temkin isotherm were followed by those models.

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Figure 7 | Bioadsorption isotherm model fitted by a two-parameter model.

Figure 8 | Bioadsorption isotherm model fitted by a three-parameter model.

Figure 9 | Bioadsorption isotherm model fitted by a four-parameter model.

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Figure 10 | Bioadsorption isotherm model fitted by a five-parameter model.

For the nonlinear method, a computer-operable trial-and-error method was utilized to minimize the error dis-
pensation between the experimental observations and the isotherms studied. The error functions that correspond
to the parameters of the calculated isotherm are shown in Table 7. It demonstrates that the Langmuir isotherm,
followed by the Freundlich–Temkin isotherm (for two-parameter models), was identified as the close-fit isotherm
by the error functions that were correlated to the smallest deviations from the predicted equilibrium data
(Figure 7). It could be found that the Langmuir model very well represents the experimental observations on
the bioadsorption of iron ions onto OSL leaf powder. The Langmuir model has the lowest error values and rela-
tively high R 2. The qmax value (in mg/g) for iron ions was 123.26. In the Freundlich equilibrium, the k constants
for OSL leaf powder were obtained to be 73.75 l/g. The value of n obtained is between 0 and 10, which signifies
that iron ions adsorb relatively strongly on the superficies of the adsorbents. The low correlation coefficients, on
the other hand, showed that this was a unsuitable model for describing this equilibrium. It can be seen that the
error function values produced by the nonlinear method are lower when compared to those produced by the
linear method. The error functions for the nonlinear regression method have not changed except for the
Temkin isotherm model. The great similarity between Temkin model’s linear and nonlinear equation forms
may account for the same.
The equilibrium adsorption statics data can be modelled by the three-parameter isotherm equations, i.e. Red-
lich–Peterson, Sips, and Toth isotherms. The isotherm parameters derived from the linear and nonlinear fitting
analyses are summarized in Tables 6 and 7. The coefficients of determination are very good (R 2 . 0.990) for
all the three models (Table 7). R 2 values for the Redlich–Peterson isotherm model were observed to be 0.99
for both nonlinear and linear model fitting but show lower error values in the case of the nonlinear models. A
superior and comprehensive representation of the experimental data for the bioadsorption isotherms was
observed for the Sips isotherm model (considering values of the error functions). The Sips and Toth model’s
linear and nonlinear trends show a poor fit for the linear model and a strong correlation for the nonlinear
model (by comparing the values of coefficient of determination, i.e. R 2 and other error functions). The exponent
of the Toth model (t) calculated by linear and nonlinear regression falls in the range of 0–1, suggesting a good
resemblance of Toth isotherm with Langmuir isotherm. Adsorption occurred on a heterogeneous surface
when t is less than 1. The close-fitted bioadsorption isotherm models were found to be in the following order
observed using the three-parameter equations: Sips . Toth ¼ Redlich–Peterson. The equilibrium statistics or
data were well described by three-parameter isotherm models than by two-parameter isotherm models, as
shown earlier.
With linear and nonlinear four-parameter isotherm models, the adsorption equilibrium statistics were exam-
ined. The four-parameter isotherm model of the Fritz–Schlunder isotherm and the Baudu isotherm is used to
obtain an accurate fit to the experimental results of bioadsorption isotherms (Figure 9). Fritz–Schlunder isotherm
shows that the coefficients of determination (R 2 . 0.99) are very good and have low values for error function as

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Figure 11 | Bioadsorption isotherm model linear fitting by two- and three-parameter model: (a) Langmuir, (b) Freundlich,
(c) Temkin, (d) Redlich–Peterson, (e) Sips, and (f) Toth.

compared to Baudu (R 2 ¼ 0.86). The adsorption of iron ions on OSL leaf powder appears to be better explained
by Fritz–Schlunder’s equation than the Baudu isotherm. The Baudu isotherm has a lower maximum bioadsorp-
tion capacity than the Langmuir isotherm, while it is greater than the Langmuir isotherm and theoretical values
in the case of the Fritz–Schlunder isotherm.
The nonlinear form of the Fritz–Schlunder five-parameter isotherm model was used to analyse the adsorption
data. The Fritz–Schlunder five-parameter isotherm model provides a satisfactory fit to the bioadsorption iso-
therms’ experimental observations (Figure 10). The Fritz–Schlunder five-parameter models fit better than the
Baudu isotherm model. (The correlation coefficients are very high (.0.99), and the error functions have low
values).

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Table 6 | Isotherm model parameter (linear)

Linear

Isotherm model Parameter R2 ERRSQ EABS ARE MSE RMSE

Langmuir qmax (mg/g) 121.06 0.998 2.43 4.26 34.9 0.24 0.49
a (l/mg) 2.54
Freundlich K (l/mg) 64.71 0.84 69.15 14.82 51.19 6.92 2.63
n 0.251
Temkin A 75.52 0.94 154.79 21.50 4.85 15.48 3.93
B 17.37
Redlich–Peterson a (mg/g/min) 2.70 0.99 2.53 3.98 17.14 0.25 0.50
b (g/mg) 0.98
K 316
Sips Ks (l/g) 234.5 0.962 16.83 11.55 76.04 1.68 1.30
as (l/mg) 0.46
bs 1.24
Toth qm 94.43 0.962 16.83 11.55 76.04 1.68 1.30
K 0.386
t 0.803

Table 7 | Isotherm model parameters (nonlinear)

Nonlinear

Isotherm model Parameter R2 ERRSQ EABS ARE MSE RMSE

Langmuir qmax (mg/g) 123.26 0.996 2.39 4.05 0.41 0.24 0.49
a (l/mg) 2.27
Freundlich K (l/mg) 73.75 0.86 48.06 12.58 1.22 4.81 2.19
n 0.183
Temkin A 77.23 0.94 130.79 20.06 1.71 13.08 3.62
B 17.37
n
Redlich–Peterson a (mg/g/min) 2.57 0.996 2.40 3.71 0.43 0.24 0.49
b (g/mg) 0.98
K 303.3
Sips Ks (l/g) 256.1 0.997 2.01 3.31 0.95 0.20 0.45
as (l/mg) 2.04
Bs 0.90
Toth qm 114.2 0.996 3.27 4.44 0.60 0.33 0.57
K 2.61
t 0.98
F-S A 222.4 0.997 2.62 3.93 0.71 0.26 0.51
B 1.65
m 0.849
n 0.869
Baudu Qm 95.76 0.863 63.49 18.38 1.69 6.35 2.52
K 3.35
A 0.18
B 7.90
F-S qm 14.91 0.997 2.05 3.66 0.47 0.20 0.45
K1 14.91
m 0.84
K2 1.65
n 0.86

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Table 8 compares the biosorption uptake of iron ions by OSL leaf powder and other biosorbents mentioned in
the literature. The adsorbent shows the potential for the separation of iron ions from the aqueous media.

Table 8 | Adsorption capacity of different bioadsorbents

Sr. No. Biomass qmax (mg/g) Reference

1 Azadiracta indica leaves 146.30 Ang et al. (2013)

2 Ocimum sanctum leaves 123.26 Present study
3 Sawdust 116.00 Shrestha (2018a)
4 Spent tea leaves 90.90 Bajpai & Jain (2010)
5 Peanut hull 79.28 Awad (2017)
6 Peacan nutshell 76.59 Vaghetti et al. (2014)
7 Banana peel 33.79 Shrestha (2018c)
8 Launea procumbens leaves 17.00 Indracanti & Gunturu (2019)
9 Lagenaria siceraria peel 11.36 Ahmed et al. (2018)
10 Ananas comosus peel 10.43 Izzati et al. (2018)

Because of differences in surface properties interconnected to the existence of several functional groups, the
sorption abilities of specific biological materials may differ.

Thermodynamics parameters
Table 9 shows the estimated thermodynamic parameters, i.e. ΔG (Gibb’s free energy), ΔH (change in enthalpy)
and ΔS (change in entropy) for bioadsorption, of the iron ions by OSL leaf powder, and Figure 12 depicts the
graph of ln K versus 1/T for the OSL leaf powder.

Table 9 | Thermodynamic parameters for bioadsorption of iron ions on OSL leaf powder

Biomass T (K) ΔG (KJ/mol) ΔH (KJ/mol) ΔS (KJ/mol K)

OCL leaf powder 298 14.04  72.80  0.197

303 13.01
308 11.87
313 11.03
318 9.88
323 9.19

Figure 12 | Thermodynamic plot for the adsorption of iron ions by OSL leaf powder.

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The negative values of change in Gibb’s free energy (ΔG) found for the bioadsorption of iron ions by OSL leaf
powder at various temperatures firm up the feasibility of the reaction and revealed the spontaneous kind of the
bioadsorption processes, which did not involve an external energy source for the system. The negative value of
ΔH (difference in enthalpy) indicates adsorption reaction to be in agreement with the exothermic nature of inter-
actions, and the negative value of ΔS (change in entropy) presented the decreased uncertainty at solid–liquid
interphase throughout the bioadsorption processes of iron ions on the said adsorbent. Negative values of ΔH
and ΔS revealed that no structural changes of the adsorbent supported adsorption of iron ions on the OSL
leaf powder were physical in nature.

CONCLUSION
OSL leaf powder is an environmental friendly and cost-effective biosorbent for heavy metals removal from aqu-
eous stream or media. This study examines the effectiveness of OSL leaf powder for the extraction of iron ions
from aqueous media.
The kinetics and equilibrium of iron ions bioadsorption onto the surface of OSL leaf powder were described
using several mathematical models. The maximum potential of bioadsorption (in mg/g) of 123.26 was calculated
from the Langmuir model for OSL leaf powder, under optimum conditions (pH 5, biomass concentration 0.2 g,
contact time 2 h and speed of agitation 150 rpm at temperature 25 °C). The possible, spontaneous, and exother-
mic nature of the bioadsorption process of iron metal ions on OSL leaf powder was revealed by the
thermodynamic parameters. The OSL leaf powder has been effectual in extracting iron ions from aqueous media.
The outcome of this study shows that, in comparison to linear regression, nonlinear regression is the most effec-
tive method for finding the ideal isotherm and the parameters of the isotherm. The Fritz–Schlünder isotherm,
derived from a comparison of nonlinear isotherms, is the close-fitting model for the bioadsorption of iron ions
on powdered OSL leaves. For the purpose of describing the adsorption equilibrium isotherms of iron ions on
powdered OSL leaves, all of the tested models were categorized as follows: Fritz–Schlunder (five parameters) ¼
Fritz–Schlunder (four parameters) . Sips . Redlich–Peterson . Toth ¼ Langmuir . Temkin . Baudu ¼ Freun-
dlich. According to kinetic experiments, it was observed that the bioadsorption process is quick and attained
equilibrium in a short contact time. The PS1 model (nonlinear) well defined the process’s kinetics of bioadsorp-
tion of iron ions on OSL leaves adsorbents. When nonlinear kinetic equations are transformed into linear forms,
the parameters of the model may be distorted. Furthermore, the nonlinear kinetic equations have the advantage
of not necessitating prior knowledge of qe (experimental) to fit the experimental points. Thus, the adsorption par-
ameters can be primarily obtained using the nonlinear approach. In addition, the ERRSQ approach of error
analysis may be superior to use for the determination of correlation coefficient (R 2) and to identify close-fitting
models. Upscaling and commercialization of the adsorbent on a pilot-scale can be studied, as well as its regen-
eration, reuse, and secure disposal of the laden adsorbent can be addressed in future studies. Furthermore,
research on the bioadsorption of iron may concentrate on the topics like desorption of bioadsorbent, life cycle
assessment of bioadsorbent, analysing the cost associated with a potential large-scale system for industrial appli-
cation, and iron bioadsorption using bionanomaterials from alternate sources.

DATA AVAILABILITY STATEMENT

All relevant data are included in the paper or its Supplementary Information.

CONFLICT OF INTEREST
The authors declare there is no conflict.

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First received 7 February 2023; accepted in revised form 1 July 2023. Available online 18 July 2023

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