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DOI: 10.1039/C9RA00356H (Paper) RSC Adv. , 2019, 9, 7890-7902

Removal of Pb(II) and Cd(II) from wastewater using arginine cross-linked chitosan–

carboxymethyl cellulose beads as green adsorbent

Kaiser Manzoor a, Mudasir Ahmadb, Suhail Ahmada and Saiqa Ikram *a

a Biopolymer Research Laboratory, Department of Chemistry, Jamia Millia Islamia, New Delhi, India. E-

mail: [email protected]
b Applied Chemistry, School of Natural & Applied Science, Northwestern Polytechnical University, P. R.

China

Received 15th January 2019 , Accepted 28th February 2019

First published on 11th March 2019

Abstract
A one pot approach has been explored to synthesize crosslinked beads from chitosan (CS) and
carboxymethyl cellulose (CM) using arginine (ag) as a crosslinker. The synthesized beads were
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FTIR, SEM, EDX, XRD, TGA and XPS analysis. The results showed that CS and CM
were
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uses cookies and the obtained
and similar technologies material
to store and retrieve(beads) was analyzed for adsorption of
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information about your use of this website. This information helps us to provide,
Cd(II) and Pb(II) by using batch adsorption experiments; parameters such as temperature,
analyse and improve our services, which may include personalised content or
contact time,
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initial ion concentration
information were
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thermodynamic models were used to check the best fit of the adsorption data. The results
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revealed
'Cookie thatlink.
settings' the kinetics data of the adsorption of Pb(II) and Cd(II) ions shows the best fit with
the pseudo second order model whereas the thermodynamics data shows the best fit with the
 Langmuir isotherm with maximum adsorption capacities of 182.5 mg g−1 and 168.5 mg g−1 for
Pb(II) ions Cd(II) ions, respectively. For the recovery and the regeneration after the one use of the
beads, several adsorption–desorption cycles were carried out to check the reusability and
recovery of both the metal ion and the adsorbent without the loss of maximum adsorption
efficiency.

Introduction

Industrialization and advancement in other technologies such as fertilizers for agriculture, antibiotics
for healthcare and the setup of various industries on the banks of water bodies have led to increased
discharge of pollutants into water bodies. 1,2 These pollutants range from dyes from textile industries,
to heavy metal ions from tanning, paint manufacturing, and electroplating industries. 3,4 Exposure to

heavy metal ions can cause serious complications in all living creatures, especially in humans. WHO
have rightly proposed that some of the prominent chemical concerns of public health are due to heavy
metals including cadmium, lead, and mercury. Toxicity due to these three heavy metals often proves
fatal and they are also probable human carcinogens. 5–7 In children overexposure to lead causes

swelling of the optic nerve (papilledema), ataxia, brain damage (encephalopathy), convulsions,
seizures, and impaired consciousness whereas in adults it causes high blood pressure, damage to the
reproductive organs, fever, headaches, fatigue, vomiting, anorexia, abdominal pain, constipation, joint
pain, incoordination, insomnia, irritability, altered consciousness, and hallucinations. Exposure to
cadmium leads to headaches, fatigue, vomiting, nausea, diarrhea, abdominal cramps, emphysema,
pulmonary edema, low levels of iron within the red blood and breathlessness (dyspnea). 8,9
There have been continuous efforts from researchers throughout the world on the removal of heavy
metal ions through physical and chemical methods. 10 A large number of techniques such as chemical
precipitation, flocculation, reverse osmosis, electrodialysis, membrane filtration, and adsorption have
been introduced for remediation of heavy metal ion containing wastewater. 11–14 Among all these
This siteadsorption
techniques uses cookies
is most efficient and advanced method for being cost efficient and environment
friendly. Adsorption
This website of the
uses cookies andheavy
similar metal ions using
technologies to storerenewable
and retrieve biopolymers and their modified forms is
information about your use of this website. This information helps us to provide,
one of the most advancement in adsorption methodology. 15–18 Biopolymers for being environment
analyse and improve our services, which may include personalised content or
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friendly, We may share and
biocompatible this information with Google
biodegradable and other
resources havethird parties. been evaluated for their adsorption
recently
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characteristics due
optional. You can to presence
review of ample
and configure number
your cookie ofbyNclicking
settings and O oncontaining
the functional groups which in turn
'Cookie
have settings'
higher link.for heavy metal ions. Chitosan and its derivatives have been extensively studied for
affinity
adsorption of heavy metal ions from wastewater. Different ways are being proposed for modification of
the biopolymers to enhance their adsorption efficiency, cost efficiency, environment friendliness and as
well as their reusability. Graft copolymerization of the biopolymers, composites with inorganic/organic
hybrid materials and direct functionalization of the polymeric backbone have been used for syntheses
of different adsorbent material. 19–26 The important aspect for the adsorption application are:
selectivity, capacity, regeneration ability, kinetics, thermodynamics, and the cost efficiency. The use of
biopolymers as adsorbents is common, but the increase in surface area, mechanical properties, and
decrease in the swelling is still a challenge.
With the above goal, we have synthesized beads from CS and CM using arginine as crosslinker.
Arginine has guanidine moiety which has very high affinity for metal ions due to presence of large
number of amine groups. Incorporation of arginine into chitosan/carboxymethyl cellulose increases the
adsorption of these macromolecules enormously. The synthesized beads with large surface area and
less swelling, showing high removal efficiency demonstrated excellent reusability for removal of these
metal ions from aqueous solution. The beads were further evaluated for the soil degradability and
began to decompose within five weeks from burying under the soil. The synthesized beads of CS-ag-CM
can prove highly efficient adsorbent for removal of Pb(II) and Cd(II) from wastewater.

Material and methods

General remarks

All the chemicals and solvents were purchased from Himedia and Fischer Scientific New Delhi, India
Limited. Chitosan (degree of deacetylation ≥ 75%) and carboxymethyl cellulose (low viscosity) were
used. Double distilled water was used throughout the experiment. FTIR was recorded on Bruker Tensor
37 Spectrophotometer (Central Instrumentation Facility, Jamia Millia Islamia New Delhi, India) by
scanning the product in the wavelength range from 4000 cm−1 to 500 cm−1. SEM imaging was carried

out using FEI Quanta 200 FESEM (50–50k×) University Sophisticated Instruments Facility (USIF) and TGA
was performed on TG-A6300 instrument (SII Nano Technology Inc. Tokyo, Japan) Department of
Chemistry, Aligarh Muslim University Aligarh, India. XRD analysis was done on D8 Advance
diffractometer (Bruker) (Central Instrumentation Facility, Jamia Millia Islamia New Delhi, India) with Cu
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target λ = 0.154 nm at 40 kV, and 2θ was 10°–80°. Batch adsorption was used to carry out the adsorption
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studies. XPS about
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(Omicron Nanotechnology,
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radiation hν = 1486.7 eV) at Materials Research Centre Malviya National Institute of Technology JLN
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SomeJaipur,
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Preparation of arginine crosslinked CS/CM adsorbent
Chitosan solution was prepared by dissolving 3 g (6 × 10−3 moles) of CS in 0.01 M acetic acid solution.

CMC solution was prepared by dissolving 1.57 g (6 × 10−3 moles) and arginine solution was prepared by

dissolving 2 g (1.2 × 10−2 moles) in double distilled water. Chitosan solution was added simultaneously

to flask containing CM and arginine solutions. On the dropwise addition of the chitosan solution the
solid bead structures are formed while the mixture was continuously stirred at 110–120 °C for 1 h. The
resultant product was obtained as bead like structures, washed with distilled water till solution
stabilises at neutral pH. Ethanol was added to remove the water and left for drying in oven at 40 °C for
24 h.

Procedure for metal ion adsorption

Metal ion solutions of Pb(II) and Cd(II) ion were prepared by dissolving desired amount of salts of these
metal ions in double distilled water. Batch adsorption method was used for analyzing the effect of
dosage, pH, initial ion concentration, contact time and temperature on the adsorption of the metal ions
onto CS-ag-CM. All the batch adsorption methods to study the kinetics and thermodynamics of
adsorption of Pb(II) and Cd(II) ions from aqueous solution were performed thrice in order to obtain the
precise values for different adsorption quantities. The amount of metal ion adsorbed on the adsorbent
was obtained by using eqn (1)

(1)

where q is the adsorption capacity in mg g−1, Co and Ce (mg L−1) are the initial and final metal ion

concentrations respectively, V (L) is the volume of the solution taken and m (g) is the mass of the
adsorbent spent.

Procedure for metal ion desorption

The metal ion adsorbed CS-ag-CM was placed in the volumetric conical flasks containing 0.01 M EDTA
solution and was stirred in an orbital shaker for about one hour and readings were noted down every 10
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min untilsite uses cookies
desorption was complete. The beads were washed with water and dried in oven for their
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Swelling studies
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The swelling
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can review CS,configure
CM, andyour
CS-ag-CM were by
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theacidic, neutral and alkaline solutions

at 'Cookie
298 K. settings' link.
The extent of swelling was obtained by using equation
 (2)

where ws is the swollen weight of the material whereas w is the dry weight of the material.

Results and discussions

Preparation of arginine crosslinked chitosan/carboxymethyl cellulose beads

The covalent bonding of arginine with both CS and CM requires esterification or amidation of the
carboxyl group of ag or CM with the amine group on CS and ag. 27 Esterification although less

dominant than amidation due to its reversible nature is favored at lower temperature however amide
bond is formed at higher temperature because of the initial protonation of the –NH2 group. The product
CS-ag-CM obtained consists of both ester and amide linkages as can be shown from the FTIR spectrum
of the product ( Scheme 1 ).

Scheme 1 Reaction pathway.

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Characterization of CS-ag-CM
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our services, which andpersonalised
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content or was characterized by FTIR, XRD,
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SEM. The FTIR Wespectrum
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Fig. 1 shows bandand
at other third parties.
3600–3300 cm−1 which can be assigned to –N–H
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stretching vibration
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and configure O–H
your stretch,
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carbonyl group of amino acetyl moiety and –N–H bending vibrations respectively. 28 The spectrum of

CM shows the characteristic bands at 3400 cm−1, 1590 cm−1, 1405 cm−1 which are assigned to O–H
bending, C O stretching of carboxyl and C–H bending respectively. 29 The crosslinked adsorbent CS-

ag-CM shows characteristic peak at 1746 cm−1 and 1650 cm−1 which can be assigned to the C O

stretching frequencies of ester and amide carbonyls, respectively. Furthermore, the bands appearing at
1152 cm−1 and 899 cm−1 are characteristic of glycosidic bridge of the amide bond. The absorption band

appearing at 1372 cm−1 is due to C–N stretching vibrations. 30–32

Fig. 1 FTIR spectrum of (a) CS, (b) CM, (c) ag and (d) CS-ag-CM.

XRD patterns of the CS, CM, and CS-ag-CM are shown in Fig. 2 . The less intense broad peaks of CS
and CM at 2θ = 20° are the characteristic of the amorphous nature of these polymers. However, the
sharp and intense peat at 2θ = 20° of CS-ag-CM shows the transformation towards more crystalline
nature of the CS-ag-CM which is typically attributed to the crosslinking of the two polymeric backbones
by arginine.
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 Fig. 2 XRD patterns of (a) CS, (b) CM, (c) ag and (d) CS-ag-CM.

SEM micrographs of CS, CM, CS-ag-CM and M-CS-ag-CM [M = Cd(II), Pb(II)] are shown in Fig. 3(a–e) .
As predictable from the SEM images ( Fig. 3a and b ) of both CS and CM, their surfaces are smooth and
non-porous, their XRD data revealing their amorphous structure. The XRD pattern of pure arginine (ag)
shows the absolute crystalline structure with distinct peaks. The surface morphology of the adsorbent
( Fig. 3c ) CS-ag-CM shows the porous surface with large number grooves and increased surface area.
The surface of CS-ag-CM after adsorption of Pb(II) ions white spots ( Fig. 3e and f ) can be seen on the
surface of adsorbent. On increasing the magnification of the Pb(II) ion adsorbed surface further,
covered surface of CN-ag-CM is clearly indicative of Pb(II) covered surface.

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 Fig. 3 SEM micrographs of (a) CS, (b) CM, (c) CS-ag-CM, (d) Pb(II)/Cd(II)-CS-ag-CM (e) Pb(II)/Cd(II)-CS-
ag-CM and EDX spectrum of (f) CS-ag-CM and (g) Pb(II)/Cd(II)-CS-ag-CM.

Thermal analysis

Thermal analysis of all the raw material and the final product were carried out in order to evaluate the
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thermal stability of the adsorbent as shown in Fig. 4 . It was observed that the adsorbent CS-ag-CM was
This website uses cookies and similar technologies to store and retrieve
thermally more
information stable
about than
your use both
of this CS and
website. ThisCM. The amount
information oftothe
helps us residual CS-ag-CM is much larger than
provide,
analyse and improve our services, which may include personalised content or
the CS and CM at 600 °C which is approximately 45%, is the strong evidence for the crosslinking of CS
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 Fig. 4 TGA of CS, CM and CS-ag-CM.

XPS analysis

XPS analyses shows the evidence of the adsorption of Pb(II) and Cd(II) on to CS-ag-CM as shown in Fig.
5 . The adsorption of Pb species with the appearance of new peaks in the range of 136 and 410 eV
correspond to Pb 4p and Pb 4d respectively. The spin–orbit components (Δmetal = 4.9 eV) in the Pd 4f
region with binding energy of Pb 4f7/2 138.9 eV are characteristic of Pb(II) species. Similarly, the peaks at

406 and 643 eV correspond to Cd 3d and Cd 3p species of Cd(II) respectively. These results confer that (i)
both Pb(II) ions and Cd(II) ions are not reduced to metallic forms upon contact with the CS-ag-CM
beads, and (ii) the adsorption results from the coordination of Pb(II) and Cd(II) species by the guanidine
moiety of the crosslinker arginine. 33,34

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 Fig. 5 XPS of CS-ag-CM before and after adsorption of Pb(II) and Cd(II).

Adsorption studies

Adsorption parameters were calculated using equilibrium batch adsorption method. A series of 50 ppm,
100 ppm, 150 ppm and 200 ppm concentration solutions of Pb(II) and Cd(II) ions from their respective
salts were prepared and effect of different parameters on adsorption process such as temperature,
contact time, pH, initial ion concentration were observed, and relative conclusions were made on
comparing the obtained quantities. It was observed that the adsorption capacity for uptake of Pb(II)
ions was 182.5 mg g−1 and that for Cd(II) ions was 168.5 mg g−1 from the aqueous solution.
Effect of temperature. In order to study the effect of temperature on adsorption of Pb(II) and
Cd(II) 50 ppm solution of both these metal ions was taken in two different flasks, 100 mg of adsorbent
was added to both the flasks and left in orbital shaker for 1 h each at 303 K. The solutions were filtered,
and the remaining concentration was determined by titration, similar procedure was repeated at
temperatures. From the plot of qe vs. T Fig. 6(a) , it was observed that initially the adsorption increased
on increasing with temperature with maximum adsorption at 310 K for Cd(II) and 315 K for Pb(II) ions
and there on decreases with further increase in temperature. This can be attributed to the fact that
initially when temperature increases the thermal energy of the metal ions also increases which in turn
increase the probability of contact between the vacant sites of the adsorbent and the metal ions.
However, on increasing the temperature further the thermal vibration of metal ions become much
faster than the adsorbent–metal ion interaction resulting in the release of metal ions back into the

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solution.

Fig. 6 Effect of (a) temperature, (b) pH, (c) contact time and (d) initial ion concentration on the
adsorption of Pb(II) and Cd(II) onto CS-ag-CM.

Effect of pH. Effect of pH on adsorption of Cd(II) and Pb(II) onto CS-ag-CM was studied by
preparing 50 ppm solution of metal ions with different pH and were subjected to shaking in orbital
shaker for 1 h at temperatures 310 K for Cd(II) and 315 K for Pb(II) ions. The resultant solutions were
filtered after 1 h and the remaining concentration was determined by titration. The graph of qe vs. pH
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( Fig. 6(b) ) shows that initially the amount of Cd(II) and Pb(II) adsorbed onto CS-ag-CM increases with
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increase in the
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use maxima
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ions improve
onto our services,
adsorbent does which
notmay includebecause
increase personalised content
of the or
formation of metal hydroxides in alkaline
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medium. At lower
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competes with Cd(II) and Pb(II) ion adsorption onto CS-ag-CM. 35,36
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Effect of contact time. Contact time between the adsorbent surface and the adsorbate molecules
has a profound effect on the adsorption capacity. Initially when all the adsorbent sites are vacant, the
adsorbate molecule adhere to the vacant sites as soon as the metal ions come in contact with them
thereby showing a gradual increase in the adsorption with time till a maximum is attained at 40 min as
shown in Fig. 6(c) . Thereafter no further increase in adsorption is seen which occurs due to fact that
when all the adsorbent sites are occupied a dynamic equilibrium is attained in which the number of
molecules being adsorbed equals the number of adsorbate molecules being desorbed. 37,38
Effect of initial concentration. Initial concentration of the adsorbate molecules affects the rate
of adsorption to a great extent as depicted in Fig. 6(d) . At the lower initial adsorbate concentration
lesser number of collisions occur between the adsorbate molecules and the adsorbent which increase
with increase in the initial adsorbate concentration and shows sharp increase in the adsorption
capacity up to initial concentration of 300 mg L−1 for Cd(II) ion and 325 mg L−1 for Pb(II) ion. There is no
further increase in adsorption with increasing initial ion concentration due to attainment of the
dynamic equilibrium between free adsorbate ions in solution and adsorbed metal ions. 39
Adsorption kinetics. In order to determine the rate of adsorption of Pb(II) and Cd(II) onto
adsorbent, three different kinetic models were used, pseudo first order, pseudo second order and
intraparticle diffusion model. 39–44 The linear forms of these models are given below:

ln(qe − qt) = ln qe − k1t (3)

(4)

qt = Kidt1/2 + C (5)

where qe and qt are adsorption capacities at equilibrium and at time t respectively, k1, k2 and Kid are
first order, second order and intraparticle diffusion rate constants respectively. On comparing the R2
values of the plots obtained from these equations as shown in Fig. 7(a–c) , it was observed that pseudo
first order plot with R2 = 0.990 (Pb) and 0.944 (Cd) and could not explain the adsorption phenomena.
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However, pseudo second order model could establish a much better relation in the adsorption kinetics
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with R2 values
information corresponding
about your use of thisto 0.999 This
website. for both Pb(II)helps
information and us
Cd(II) ions which has much been used to
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describe the kinetics of divalent metal ions onto peat. The intraparticle diffusion plot shows
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multilinearity
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arethe adsorption
necessary of bothtoPb(II)
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different pathways. The first step corresponds to boundary layer diffusion of Pb(II) and Cd(II) ions on to
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CS-ag-CM while as the second step corresponds to the gradual sorption of these ions onto adsorbent.
The intraparticle diffusion of Pb(II) and Cd(II) ions in the second step slows down due to low leftover
concentration of these ions in the solution the similar adsorption behaviour shown in the adsorption of
Pb(II) ions onto sawdust and polyacrylamide zirconium(IV) iodate ( Table 1 ). 45

Fig. 7 Plots of (a) pseudo first-order kinetics, (b) pseudo second order kinetics and (c) intraparticle
diffusion model.

Table 1 Kinetic parameters of pseudo first order, pseudo second order and intraparticle diffusion model
forThis
adsorption of Pb(II)
site uses and Cd(II) onto CS-ag-CM
cookies
Pseudo
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uses order
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store andsecond
retrieve order Intraparticle diffusio
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k1 and
analyse (g mg −1 min−1) q (mg g−1) R2
improve our services,
m which may includekpersonalised
−1
2 (g mg min
−1) q (mg g−1)
content orm R2 Kid (mg g−1 min1/2) C
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Pb(II) 0.070 185.236 0.990 0.003
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181.159 0.999 11.021 10
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Cd(II) 0.03998 123.993 0.94464 0.0037 164.744 0.999 5.0281 10
'Cookie settings' link.
 
 Adsorption isotherms. Adsorption isotherms are used to establish the relation between the
amount of adsorbate adsorbed and the unadsorbed adsorbate. There are a number of adsorption
isotherms but most important being Langmuir isotherm, Freundlich isotherm, and Temkin isotherm
and their linear forms as shown below: 46

(6)

(7)

(8)

where Ce (mg L−1), qm (mg g−1) and qe (mg g−1) are the equilibrium concentration, equilibrium
adsorption capacity, maximum adsorption capacity respectively. KL and KF are Langmuir and
Freundlich constants respectively, R (8.314 J K−1 mol−1) is gas constant and T (K) is temperature. AT (L
g−1) and bT (J mol−1) are Temkin constants associated with the heat of adsorption.
The Langmuir model ( eqn (6) ) is usually used to describe the monolayer adsorption of adsorbate at
the surface of adsorbent considering the similar types of adsorbent vacant sides and similar adhesive
forces that bind the adsorbate molecules to the adsorbent surface neglecting the interactions between
the adsorbate molecules.
Freundlich isotherm ( eqn (7) ) gives information about the adsorption on heterogeneous surfaces
with the possibility of multilayer adsorption while as Temkin isotherm model ( eqn (8) ) takes in
consideration the adsorbate–adsorbent interactions assuming linearity in the evolution of adsorption
energy and the surface coverage of the adsorbent.
Langmuir isotherm assumes monolayer coverage on a homogeneous surface with identical
adsorption sites studied for gas adsorption on solid surface. However, in solution–solid systems, a lot of
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factors come into play such as hydration forces, mass transfer etc. which makes it more complicated,
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and obeyingabout
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isotherm adequacy can be seriously affected by the experimental conditions, the range of
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concentration of the
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properlyBoth Langmuir
and others are and Freundlich isotherms might
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adequately describe the same set of liquid–solid adsorption data at certain concentration ranges,
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particularly if the concentration is small and the adsorption capacity of the solid is large enough to
make both isotherm equations approach a linear form.
 The plots obtained for the three isotherm models for adsorption of Pb(II) and Cd(II) onto CS-AG-CM
are shown in Fig. 8(a–c) . All the three models fit the adsorption process of Pb(II) and Cd(II) onto CS-ag-
CM to different extent from good to best. The Freundlich model with R2 values 0.985 for Pb(II) and 0.984

for Cd(II) is less suitable for explaining the adsorption process as compared to Langmuir plot with R2
0.988 for Pb(II) and 0.989 for Cd(II) which shows the best fit with the adsorption of Pb(II) and Cd(II) onto
CS-ag-CM. The isotherm parameters and the regression coefficients of different isotherm models are
shown in Table 2 . It is clear from the correlation coefficients that Langmuir model best correlates the
adsorption of Pb(II) and Cd(II) onto CS-ag-CM with maximum adsorption capacities 185.5 mg g−1 for
Pb(II) and 169.7 mg g−1 for Cd(II) ions obtained from the slope of the plot which is higher than any of the
previously synthesized adsorbent for removal of Pb(II) and Cd(II) as shown in Table 3 . Furthermore, the
higher values of bT for Pb(II) and Cd(II) suggest the stronger adhesion of these metal ions onto
adsorbent surface.

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Fig. 8 Isotherm plots of (a) Langmuir isotherm, (b) Freundlich isotherm and (c) Temkin isotherm.
Table 2 Parameters of various isotherm models for adsorption of Pb(II) and Cd(II) onto CS-ag-CM

Langmuir Freundlich Temkin

KL (L mg−1) qm (mg g−1) R2 KF n R2 AT bT R2

Pb(II) 6.92 × 10−2 185.5 0.988 67.49 5.24 0.985 11.23 115.90 0.766

Cd(II) 5.91 × 10−2 169.7 0.989 53.94 4.64 0.984 21.72 147.92 0.765

Table 3 Comparison of the adsorption capacities of various adsorbents for adsorption of Pb(II) and
Cd(II) ions from wastewater

Metal Ion Adsorbent Q (mg g−1) Reference

Pb2+ Chitosan beads 34.98 47

Epichlorohydrin-crosslinked chitosan 34.13 48

Carboxymethylated cellulose 24.59 49

Chitosan–GLA beads 14.24 47

Chitosan–GLA–citric acid (C-Gch) flake 76.75 at 20 °C 50

101.7 at 30 °C

103.6 at 40 °C

γ-Fe2O3 nanoparticles 69.0 51

Chitosan coated calcium alginate 106.9 52

CS-ag-CM beads 182.5 Present study

Cd2+ Amino functionalized mesoporous silica 18.3 53

Nano-alumina 83.3 54

Amino functionalized magnetic graphenes composite 27.8 55

Polyvinyl alcohol/polyacrylic acid double network gel 115.9 56

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CS-ag-CM beads 168.5 Present study
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Recycling studies through successive adsorption–desorption cycles
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The reusability and stability of the adsorbent was evaluated by subjecting it to several adsorption–
desorption cycles. The solutions of 100 ppm each of Pb(II) and Cd(II) were used for adsorption by CS-
ag-CM by shaking these solutions in orbital agitator at 213 K for 30 min. Thereafter the adsorbent with
Pb(II) and Cd(II) adsorbed on its surface was dried and treated with 0.1 M HCl solutions and shaked for
30 min. Six successive adsorption–desorption cycles were repeated until all the metal ions were
recovered from the adsorbent. The remaining concentrations were determined by AAS and it was
observed that 96% of the dissolved metal ions were recovered ( Table 4 and Fig. 9 ).

Table 4 Adsorption–desorption parameters for evaluating the reusability of CS-ag-CM

(%) Adsorbed (%) Desorbed
No. of cycles 1 2 3 4 5 6 1 2 3 4 5 6
Pb(II) 92.5 92.8 93.8 94.2 94.6 95.3 97.5 96.8 98.2 99.0 98.5 98.8

Cd(II) 91.5 91.9 92.2 92.6 93.0 93.5 96.5 96.2 96.7 97.0 97.2 96.6

Fig. 9 Percent recovery/regeneration of (a) Pb(II) and (b) Cd(II) from the CS-ag-CM.

Soil degradability test

ToThis
analyze theuses
site biodegradability
cookies of the used adsorbent in the environment, the CS-ag-CM was buried
under the soiluses
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as to study its self-decomposition.
and similar The
technologies to store and SEM images in Fig. 10(a and b) shows the
retrieve
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morphology of this website.
a sample before This
andinformation helpsFig.
after burial us to10(a
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and b) , respectively. The
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 Fig. 10 Soil degradation of the adsorbent before burial (a) CS-ag-CM, (b) CS-ag-CM after burial of five
weeks under the soil, and (c) graph showing weight loss of CS-ag-CM for 5 weeks.

Conclusion

The increase in the release of toxic heavy metal ions into the environment is a serious threat to
biological life and hence their removal from water is major concern worldwide. In the current work, we
have decreased the hydrophilic property of chitosan together with the higher affinity of the guanidine
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group of the arginine for metal ions for synthesizing the beads for removal of Pb(II) and Cd(II) from
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observed that the synthesized beads were able to remove Pb(II) and Cd(II) from aqueous solution with
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removal efficiency of 95.3% for Pb(II) and 93.5% for Cd(II) which is higher than the adsorbents. The
regeneration and the recovery of the crosslinked beads is evaluated first time with the constant
adsorption efficiency up to 6 adsorption–desorption cycles. This factor makes the CS-ag-CM as good
adsorbent for the adsorption of Pb(II) and Cd(II), as the process need low operational cost and
environmentally friendly.

Conflicts of interest

There are no conflicts to declare.

Acknowledgements

Authors acknowledge Central Instrumental Facility and Centre for Nanoscience and Nanotechnology
Jamia Millia Islamia New Delhi for providing FTIR and XRD facilities, Indraprastha University New Delhi
for providing SEM facility and Aligarh Muslim University for providing EDX and TGA facility. Author also
acknowledges MNIT Jaipur for providing XPS facility. Furthermore, the authors declare no financial
interests from any funding source.

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