Materials Today: Proceedings xxx (xxxx) xxx

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Removal of heavy metals (Cu & Ni) from wastewater using rice husk and
orange peel as adsorbents
R. Lakshmana Naik a,⇑, M. Rupas Kumar b, T. Bala Narsaiah c
a
Department of Chemical Engineering, RGUKT-RK Valley, Kadapa, Andhra Pradesh, India
b
Department of Civil Engineering, RGUKT-Ongole, Ongole, Andhra Pradesh, India
c
Department of Chemical Engineering, JNTUA CE, Anantapuram, Andhra Pradesh, India

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

Article history: Recent industrial growth in India has caused large quantities of heavy metals including mercury, lead,
Available online xxxx zinc, copper, nickel, cadmium, and chromium to be released into the environment. As heavy metals are
extremely toxic and non-biodegradable, it is extremely difficult to separate them from the atmo-
Keywords: sphere. Many research studies attempted to address the ability of the non-conventional absorbents in
Adsorption removing different types of wastewater pollutants. As a cost-effective alternative to conventional effluent
Adsorbents treatment methods, Bio-sorption technology utilizes natural and agricultural waste materials as absor-
Agricultural wastes
bents, which are relatively cheaper, sustainable, and abundant. The study concentrates on the capacity
Waste water
Heavy metals (Cu and Ni)
of rice husk and orange peel in extracting heavy metals from waste water. Adsorption tests has been car-
Redlich-Peterson Isotherm ried out for different combinations of rice-husk and orange peel varying dosage, contact time, pH and
mixing speed and optimal levels resulting in maximum removal efficiency levels are ascertained. To
determine the efficiency of the adsorbents, Redlich-Peterson isotherms were constructed using different
combinations of orange peel and rice-husk under varying conditions.
Copyright Ó 2022 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of the International Confer-
ence on ‘‘Novel Materials and Technologies for Energy and Environment Applications (NMTEEA-2022)”.

1. Introduction causing serious health disorders. Water contaminated with

heavy-metal ions can cause environmental problems even at very
Inorganic effluents from the industries such as plating of metals, low concentrations, highlighting the need for materials that are
mining activities, and industries related to tannery, smelting, capable of complexing these metal ions effectively [4].
alloys and batteries contain toxic metal ions that accumulate in Heavy metals can be removed from wastewater in several ways,
food chain. The adsorption process has found to be an effective including membrane processing, chemical precipitation, ion
method for separating hazardous metals from wastewater [1]. As exchange, filtration, reverse osmosis, electrochemical treatment
a cost-effective alternative to conventional effluent treatment and adsorption. Research attempts made on effluent processing
methods, Bio-sorption technology utilizes natural and agricultural containing heavy-metals has demonstrated that adsorption is a
waste materials as absorbents, which are relatively cheaper, sus- highly efficient method of removing heavy metals from wastewa-
tainable, and abundant [2]. Chemically processed plant residues ter stream [5]. Fundamentally, Adsorption is a method in which
have been reported to have better adsorption capabilities than one or both of the materials of a mixture are selectively condensed
unmodified versions [3]. This is due to the use of a wide range of or retained on a solid surface. The solid that adsorbs is adsorbent
chemicals such as oxidizing agents, mineral and organic acids, and the component adsorbed is adsorbate. Despite the fact that
bases, organic compounds, and so on. Because heavy metal ions several industrial adsorbents, such as silica gel and activated alu-
are extremely soluble in water, they can be absorbed by living mina are available, [6] activated carbon is extensively used. Acti-
creatures. The entry of the heavy-metal ions into the food chain vated carbon remains a costly resource given its widespread use
leads to accumulation in large concentrations in the human body for the water and wastewater treatment industries. The research
attempts made in the recent past calls for the need for safe and
⇑ Corresponding author. inexpensive methods such as usage of low-cost agricultural waste
E-mail address: [email protected] (R. Lakshmana Naik).
products to remove heavy metals from polluted waters [7].

https://doi.org/10.1016/j.matpr.2022.06.112
2214-7853/Copyright Ó 2022 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of the International Conference on ‘‘Novel Materials and Technologies for Energy and Environment
Applications (NMTEEA-2022)”.

Please cite this article as: R. Lakshmana Naik, M. Rupas Kumar and T. Bala Narsaiah, Removal of heavy metals (Cu & Ni) from wastewater using rice husk
and orange peel as adsorbents, Materials Today: Proceedings, https://doi.org/10.1016/j.matpr.2022.06.112
R. Lakshmana Naik, M. Rupas Kumar and T. Bala Narsaiah Materials Today: Proceedings xxx (xxxx) xxx

Agricultural products include proteins, polysaccharides and lignin accumulation in biological materials, making it an efficient
that can be correlated to functional groups of metal ion adsorption. adsorbent.
Agricultural wastes are viable alternatives to synthetic adsorbents
because of their abundance of natural occurrences and large 2.2. Experiment
amount of useful surface groups. Recent years have seen a lot of
research on the removal of heavy metals from soil using agricul- The adsorption of metal ions by low cost adsorbents has been
tural by-products that include ash, banana pith, pine bark, peanut, investigated under many situations such as heavy metal concen-
soybean hulls, eggs, rice husk, orange peel, shell of hazelnut, saw- tration, pH, mixing speed, and adsorbent dosage. Adsorption is per-
dust, and compost [8]. The adsorption of heavy metal is monitored formed batch wise and the following steps are involved: Pre-
considering various conditions of contact time, adsorbent dose, treatment, Synthetic waste water preparation, Addition of adsor-
RPM and pH [9] to evaluate the best conditions of the activity. bents, Stirring using magnetic stirrer, Centrifugation and Measur-
The adsorption tests are performed with batch wise industrial ing absorbance using spectrophotometer. Calibration curve is
effluent. Batch-wise adsorption, centrifugation to extract the drawn before conducting the batch wise adsorption experiment.
adsorbate from the residual sample and spectrophotometer to Calibration curve is drawn by choosing different concentrations
quantify the final metal strength in the residual sample are the of 1, 2, 3, 4, 5 gm/100 ml of copper sulfate and nickel nitrate sep-
steps involved in the experiment. Chemical precipitation, Mem- arately in distilled water and calculating absorbance using spec-
brane processing filtration, and Ion exchange are the unit processes trophotometer as shown in Fig. 1.
involved in the heavy metal removal from industrial waste water,
which are highly cost effective and thus making them less usable. i. Pretreatment of orange peel and rice husk
Adsorption is not only an effective technique but also economical
Orange fruit peel was obtained from a local fruit market located
for the heavy metals removal from wastewater. The adsorption iso-
in Andhra Pradesh, India. In order to remove any physical impurity
therm is the standard depiction of the adsorbate concentration and
on the surface, peels were washed with distilled water after a thor-
amount of material adsorbed, which is represented by a graph cre-
ough washing with tap water; around 72 °C, it was then oven-dried
ated between the adsorbed quantity and the equilibrium concen-
until it received a constant weight. It was eventually grounded and
tration at a certain temperature. The isotherm shape was used in
sieved.
the current investigation to identify the nature of the interaction
The raw material was rice husk collected from a rice mill in
between adsorbate and adsorbent.
Andhra Pradesh, India. The rice husk was properly washed with
purified water to eliminate a sticking soil and then dried in air at
2. Experimental section 100 °C in an oven for 24 h. The husk of rice was milled and then
passed through various sieves. For further procedures, the particle
2.1. Materials: rice husk and orange peel size of 80 lm was picked.

Rice husk is a type of agricultural waste that is produced during ii. Synthetic waste water preparation
paddy cultivation. Organic matter content in dry rice husk is
between 70 and 85 percent which includes cellulose, lignin, hemi Metal solutions (Cu, Ni) were formed by dissolving nickel
celluloses in high proportions and silica present in the cellular nitrate (NiNO3)26H2O, copper sulfate (CuSO45H2O) separately in
membrane. Because of its granular form, insoluble in water, chem- distilled water to produce the necessary metal ion concentrations
ical stability, high mechanical strength, and abundant availability and synthetic wastewater. To carry out adsorption tests, 2 gm of
at a low cost, rice husk has become a preferred adsorbent [10]. copper sulphate and nickel nitrate are applied to 100 ml of distilled
Orange peel consists significant proportions of pectin, cellulose, water.
hemicelluloses, limonene and various low molecular weight com-
pounds. Some of the recent studies have proved the usage of iii. Addition of adsorbents
orange peel in cadmium removal from aqueous solutions employ-
ing adsorption technique [11,12]. Orange peel contains carboxyl The synthetic waste water adsorbents are applied to the syn-
and hydroxyl groups, which are key functional groups for metal thetic wastewater after the preparation. For rice husk and combi-

(a) (b)

Fig. 1. a) Calibration curve for copper b) Calibration curve for Nickel.

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R. Lakshmana Naik, M. Rupas Kumar and T. Bala Narsaiah Materials Today: Proceedings xxx (xxxx) xxx

nation of rice husk and orange peel, adsorption experiments were increase in the absorbent volume. For varied doses of 1, 2, 3, 4, 5,
performed. Adsorption is done by adding 5gm of adsorbent (2.5gm 6, 7, 9, 11 g/100 ml, the removal of Cu and Ni ions by mixing rice
orange peel + 2.5gm rice husk) to evaluate the effect of pH, contact husk and orange peel in equal amounts is shown in Fig. 2(a) and
time, and stirring velocity effect. To find out the effect of adsorbent (b). Cu and Ni removal ratios using rice husk and orange peel are
dose different doses were added i.e., 1, 2, 3, 4, 5, 6, 7, 9, 11 increased from 20.65% to 99.10% and from 7.50% to 99.36% with
gm/100 ml. the increase in adsorbent amount In the case of a combined form
of adsorbent, the removal ratios are more compared to the ratios
iv. Stirring when using a single adsorbent.

On a magnetic stirrer, adsorbents are applied to the synthetic

waste water stirring. Stirring speed is held at 200 RPM to assess 3.2. Effect of contact time
the effect of adsorbent dosage, pH effect and contact time effect.
To find the impact of RPM, various speeds, i.e. 50, 100, 200, 250, The adsorbate concentration and contact time between adsor-
300, 350, 400 RPMs, will be maintained. For all adsorption checks, bent and adsorbate species plays a significant role throughout
room temperature is maintained. the process of removing contaminants from wastewater at a speci-
fic temperature and pH. The ability of an adsorbent to absorb con-
v. Centrifugation taminants quickly and achieve equilibrium in a short amount of
time suggests its suitability for use in wastewater treatment. In
Centrifugation is done to separate the residual solution from the addition, the contact time at the solid solution interface is one of
adsorbents. Upon stirring in the centrifuge tubes, residual sample the reasons for the creation of surface charges. Adsorption analysis
is obtained. Centrifugation takes place for 6 min at 4000 RPM. was performed at various times between 15 and 120 min. The
Supernatant is obtained from the centrifuge tubes before the spec- adsorbents took two hours to remove the metal ions from the
trophotometer is used to measure the absorption of metal ion in wastewater completely. When Rice husk is used a single adsorbent,
residual solution. Cu’s removal ratios increased from 6% to 76.5% between the time
period 15–120 min and for Ni, the same adsorbent resulted in
vi. Measuring absorbance of metal ion present in residual the removal ratios from 1.5% to 69.35% under the same change in
solution time period. When rice husk and orange peel as a single adsorbent,
the removal ratios of Cu varied from 17% to 97.8% for 15–120 min
Centrifuged samples are stored in sample collections for spec- and for Ni the removal efficiency ranged from 6 to 98.75 percent
trophotometer absorbance analysis. Copper sulfate solution will for the same time period variance shown in in Fig. 3(a) and (b).
provide the absorption directly, but 0.5% DMG (Di methylene gly-
oxide) solution is added for nickel solution. DMG solution is pre-
pared by adding 0.5gm of DMG to 100 ml of ethanol. Using Beer 3.3. Effect of RPM
Lamberts law, absorbance from spectrophotometer concentration
is measured in residual solution. The removal of heavy metals from aqueous solution by adsorp-
tion was determined by the stirrer’s RPM. Adsorption experiments
3. Results and discussion have been performed for different RPMs, i.e.
50,100,200,250,300,350,400. Best removal rates for low RPM have
3.1. Effect of adsorbent dose been found. The removal ratios of Cu when the rice husk is a single
adsorbent are 61 per cent and 6 per cent respectively for 50 and
The effect of the volume of adsorbent on rice husk removal of 400 rpm and for Ni respectively 77.3 per cent and 9.25 per cent
Cu ions is shown for varying 1, 2, 3, 4, 5, 6, 7, 9, 11 g/100 ml adsor- for 50 and 400 rpm. Cu removal ratios when rice husk and orange
bent doses. Cu and Ni removal using rice husk is increased respec- peel are combined as a single adsorbent are 98 per cent and 10.5
tively from 4.50% to 62.42% and from 0.30% to 65.49% with an per cent respectively for 50 and 400 rpm and 97% and 24 per cent

(a) (b)

Fig. 2. a) Effect of adsorbent dose on Cu removal b) Effect of adsorbent dose on Ni removal.

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R. Lakshmana Naik, M. Rupas Kumar and T. Bala Narsaiah Materials Today: Proceedings xxx (xxxx) xxx

Fig. 3. a) Effect of Contact time on Cu removal b) Effect of Contact time on Ni removal.

for 50 and 400 rpm respectively for Ni as shown in in Fig. 4(a) and 3.5. The Redlich-Peterson isotherm
(b).
The Langmuir and Freundlich isotherms are combined to form
the Redlich-Peterson isotherm. The numerator is derived
from the Langmuir isotherm, which has the advantage of
3.4. Effect of pH
approaching the Henry zone at infinite dilution [13]. This
isotherm model incorporates three parameters and is empirical
The removing of metal ions from aqueous solutions by adsorp-
in nature. It incorporates elements from both the Langmuir
tion was pH dependent, as it altered the adsorbent surface load,
and Freundlich equations, hence the adsorption mechanism is a
the degree of ionization of the functional groups, and metal ion spe-
mix and does not follow ideal monolayer adsorption [14]. The
ciation. Most researchers concluded that with various metal ions,
following expression describes this model:
the optimum pH varies. H+ ions contend with metal cations for
exchangeable sites in the system at lower pH levels, releasing some
AC e
of the latter. Under intense acidic conditions, heavy metal cations Qe ¼
are not completely adsorbed. To find the appropriate pH for effective 1 þ BC be
adsorption of Cu and Ni ions, experiments with different pH values,
i.e. 4, 7, 10, were conducted. Maximum adsorption occurs at a pH of where A is the Redlich-Peterson isotherm constant (L/g), B is the
10 as shown in in Fig. 5(a) and (b). Minimum adsorption at pH 4 may constant (L/mg), and b is an exponent between 0 and 1. Ce denotes
be owing to the large concentrations and mobility of the adsorbent’s equilibrium liquid phase concentration (mg/l), and
H+ ions, h+ ions are preferable adsorbed compared to Cu and Ni ions. Qe denotes the adsorbent’s equilibrium adsorbate loading (mg/g).

Fig. 4. a) Effect of RPM on Cu removal b) Effect of RPM on Ni removal.

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R. Lakshmana Naik, M. Rupas Kumar and T. Bala Narsaiah Materials Today: Proceedings xxx (xxxx) xxx

Fig. 5. a) Effect of pH on Cu removal b) Effect of pH on Ni removal.

Fig. 6. Redlich-Peterson Isotherm a) Cu (Rice Husk) b) Cu (Risk husk with orange peels). (For interpretation of the references to colour in this figure legend, the reader is
referred to the web version of this article.)

Fig. 7. Redlich-Peterson Isotherm a) Nickel (Rice Husk) b) Nickel (Risk husk with orange peels). (For interpretation of the references to colour in this figure legend, the reader
is referred to the web version of this article.)

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R. Lakshmana Naik, M. Rupas Kumar and T. Bala Narsaiah Materials Today: Proceedings xxx (xxxx) xxx

Table 1
Redlich-Peterson Isotherm constants and correlation coefficients (R2) for the adsorption of Cu and Ni ions unto adsorbent.

Redlich isotherm constants Cu (rice husk) Cu (rice husk + Orange peel) Ni (Rice husk) Ni (Rice husk + Orange peel)
A 0.1283 0.2682 0.11158 0.18231
Β 1.257 0.858 2.688 1.033
R2 0.905 0.933 0.632 0.980

At high adsorbate liquid-phase concentrations, [15] simplifies to the Declaration of Competing Interest
Freundlich equation:
The authors declare that they have no known competing finan-
A cial interests or personal relationships that could have appeared
Q e ¼ C 1b
B e to influence the work reported in this paper.
In the Freundlich isotherm model, A/B = KF and (1  b) = 1/n.
When b = 1, the equation is reduced to the Langmuir equation with
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