DOI: 10.1002/elan.201900432
EffectsofHumidity,TemperatureandBismuth
ElectrodepositiononElectroanalyticalPerformancesof
Nafion-coatedPrintedElectrodesforCd
2 +
andPb
2 +
Detection
Noemi Colozza,
[a]
Ilaria Cacciotti,
[b]
Danila Moscone,
[a]
and Fabiana Arduini*
[a]
Abstract: The synergistic use of Nafion polymeric mem-
brane and in situ electrodeposited bismuth film is a
worthwhile strategy to develop electrochemical sensors
for the detection of Cd
2 +
and Pb
2 +
. However, Nafion thin
films morphological and conductivity properties have a
strong dependence on the environmental conditions, such
as relative humidity and temperature, while the bismuth
in situ electroplating can affect the repeatability of
measurements. With the aim to overcome these draw-
backs, the effects of the storage environmental conditions
were investigated to improve the morphological stability
and electroanalytical performances of Nafion film-based
sensor for the detection of Cd
2 +
and Pb
2 +
. Nafion-coated
graphite-based screen-printed electrodes were stored at
different humidity and temperature conditions and char-
acterised by using square wave anodic stripping voltam-
metry, cyclic voltammetry, electrochemical impedance
spectroscopy, and scanning electron microscopy. Signifi-
cant differences were observed at the varying of humidity
conditions, with an enhancement of sensor electrochem-
ical performances at lower humidity. Furthermore, differ-
ent approaches for bismuth in situ electrodeposition on
Nafion-coated screen-printed electrodes were compared
by using overlap or removal approach. This study
disclosed considerable differences in the electrochemical
performances and morphology of the resulting bismuth-
sensor, obtaining an enhancement of the working stability
for the removal approach.
Keywords: heavy metals · lead · cadmium · stripping analysis · in situ electroplated
1Introduction
The combined use of Nafion and bismuth for the design
of sensitive and sustainable electrochemical sensors for
heavy metals detection has gained increasing attention
during the last decades. Indeed, the need to replace the
mercury-based sensors has boosted the research in the
development of more eco-friendly sensors. In literature, a
variety of studies have demonstrated the suitability of
combining the advantages of electrochemical sensors,
such as their cost-effectiveness and their easiness to use,
with the properties of Nafion and bismuth, delivering
analytical devices which can represent a worthy alterna-
tive to reference methods (e.g. inductively coupled
plasma mass spectrometry) for heavy metal detection,
thanks to competitive detection limits.
In details, Nafion is a sulfonated tetrafluoroethylen-
based copolymer, which can be used to modify the surface
of an electrochemical sensors to improve its mechanical
resistance and to provide protection from fouling by
organic compounds and surfactants [1–3]. It is known as a
benchmark material among the solid polymer electrolytes
with proton exchange capacity [4,5], and is typically
employed for fuel cells. Although the most robust
applications of Nafion involve its use in the form of a
free-standing membrane (thickness > 25 μm), the possibil-
ity of using thin films (usually with a thickness between
100 nm and 1 μm) is also of great interest, particularly for
electrochemical applications.
However, it is well known that the Nafion thin films
physical properties and polymeric structure are strongly
influenced by the environmental conditions [6–9]. In
particular, the Nafion proton conductivity is remarkably
affected by the environmental conditions to which it is
exposed, such as temperature [10] and relative humidity
(RH%) [9–13]. These RH%-dependent properties should
rely on the peculiar Nafion polymeric structure and its
strong tendency for water uptake. Basing on the Cluster-
Network model, proposed by Gierke et al. [14], Nafion
structure is characterised by a network of water nano-
channels which branch out among ionic domains
[12,13,15]. The ionic domains are normally deprotonated
[a] N. Colozza, D. Moscone, F. Arduini
Department of Chemical Science and Technologies, University
of Rome Tor Vergata, Via della Ricerca Scientifica 1, 00133
Rome, Italy
E-mail: fabiana.arduini@uniroma2.it
[b] I. Cacciotti
Department of Engineering, University of Rome “Niccolò
Cusano”, Via Don Carlo Gnocchi 3, 00166, Rome, Italy
Supporting information for this article is available on the
WWW under https://doi.org/10.1002/elan.201900432
Full Paper
www.electroanalysis.wiley-vch.de © 2019 Wiley-VCH Verlag GmbH & Co. KGaA, Weinheim Electroanalysis 2019, 31, 1 – 14 1
These are not the final page numbers!
��