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Potentiometric extractive sensing of lead ions over

Published on 15 September 2020. Downloaded by University of Delhi on 10/13/2020 5:41:28 PM.

Cite this: Dalton Trans., 2020, 49,

a nickel oxide intercalated chitosan-grafted-
13862 polyaniline composite†
Chandra Shekhar Kushwaha and S. K. Shukla *

Received 31st July 2020,
Accepted 15th September 2020
DOI: 10.1039/d0dt02687e
rsc.li/dalton
The present research paper reports the extractive potentiometric sensing of lead ions over a chemically
functionalized ternary nanocomposite of nickel oxide intercalated chitosan grafted polyaniline (NiO-in-
CHIT-g-PANI) prepared by the in situ chemical polymerization and composite formation technique under
optimized conditions. The structural, morphological, and physical properties of the composite material
were investigated by Fourier transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), scanning
electron microscopy (SEM), and other suitable ASTM methods. The obtained analytical result suggests the
formation of a porous hybrid composite matrix with better electrical conductivity ∼ 5.25 × 10−3 S cm−1,
free interactive carbonyl sites, and evolved aligned crystallinity. Furthermore, a film of the synthesized
composite was cast on ITO coated glass by the spin coating technique for potentiometric sensing and
the recovery of adsorbed Pb2+ ions from natural and artificial water solutions. Under optimum conditions
of ∼pH = 7.0 and a temperature of 25 °C, the electrode exhibited potential responses for Pb2+ ions in
concentrations ranging from 1.0 × 10−6 M to 1 × 10−3 M along with a sensitivity of 0.2379 mV µM−1 cm−2,
response time of 40 s, recovery time of 10 s, and stability for 64 days. The adsorbed Pb2+ ions were recov-
ered at a rate of 84% after applying an optimized reverse voltage on the above-used electrodes. The
adsorption and desorption mechanism has been explained based on the induced potential due to the
electrochemical surface interaction between Pb2+ and the NiO-in-CHIT-g-PANI based electrode. The
analytical application of the fabricated electrode in the real sample was also explored for the sensing and
recovery of the respective metal ions in wastewater samples along with the possibility of optimization of
the required metal concentrations.

Introduction purification, and precipitation sensing, have been developed

Synergism between potentiometry, size confinements, and
materials sciences has produced several innovative features for
its holistic application in the analysis and preparation of in-
organic and organic materials present in water, biological
fluids, and effluents. The advances in the above-referred inte-
gration have significantly improved the potentiometric tech-
niques, selective precipitation, electrodialysis, and water purifi-
cation. In the early 1960s, Rastogi et al. reported the intimate
relationship between phase transformation and electrical
potential difference, particularly the precipitation and dis-
solution of several inorganic compounds with great potential
in a wide range of applications.1 In this regard, several poten-
tiometric applications, including electrochemical coating,
Department of Polymer Science, Bhaskaracharya College of Applied Sciences,
University of Delhi, Delhi-110075, India. E-mail: sarojshukla2003@yahoo.co.in;
Fax: +91-11-25081015; Tel: +91-11-25087597
† Electronic supplementary information (ESI) available. See DOI: 10.1039/
D0DT02687E
with precise parameters.2 Currently, potentiometric sensors
have been efficiently used in the monitoring of anions, organic
molecules, and cations like lead, copper, mercury, and
cadmium in water, edible products, clinics, environmental
waste, and effluents.3,4 Among the different heavy metals, lead
is a highly cumulative toxicant and causes multiple problems
in the brain, liver, kidneys, and bones. Furthermore, lead is
also an industrially important metal for use in energy devices,
electronic devices, shielding materials, different advanced
materials and for making different alloys.5 Thus, the industrial
importance of lead and its exponential use is leading to
increasing and continuous pollution in both aquatic and non-
aquatic systems. Nowadays, the presence of residual lead is
also reported in drinking water, fruit juices, vegetables, and
other edible products.6 Thus, the precise monitoring of lead in
drinking water, effluents, and consumable items is very impor-
tant to standardize its applications.7
In this regard, different analytical methods are used for the
effective detection of lead, and these are atomic absorption
spectroscopy, inductively coupled plasma atomic emission

13862 | Dalton Trans., 2020, 49, 13862–13871 This journal is © The Royal Society of Chemistry 2020