Analytica Chimica Acta 530 (2005) 61–67
Miniaturised stripping-based carbon modified sensor for in
field analysis of heavy metals
Ilaria Palchetti
∗
, Serena Laschi, Marco Mascini
Department of Chemistry, University of Florence, Via della Lastruccia 3, 50019 Sesto Fiorentino, FI, Italy
Received 4 June 2004; received in revised form 16 August 2004; accepted 16 August 2004
Available online 7 December 2004
Abstract
A new miniaturised electrochemical carbon modified sensor for on-site stripping analysis of trace heavy metals is described. The graphite
working electrode is modified with a cellulose-derivative mercury coating. A detailed description of the construction of the system as well as
the systematic laboratory test carried out to optimise its performance is reported. Coupling this sensor with square wave (SW) anodic stripping
analysis, detection limits of 0.3, 1 and 0.5 gl
-1
were found for lead(II), cadmium(II) and copper(II), respectively. Deoxygenation of sample
solution is not required. The entire analysis time is shorter than 4 min.
Examples of on-site environmental applications are given. In particular, on-site analysis of heavy metals was performed at a contaminated
site. For this purpose, the sensor was coupled with a portable commercial electroanalytical instrumentation.
© 2004 Elsevier B.V. All rights reserved.
Keywords: Stripping voltammetry; Screen-printed electrodes; Mercury-coating; Heavy metals; On-site analysis; Soil; Sediments; Wastewater
1. Introduction
Stripping analysis is considered to be the most sensitive
electroanalytical technique and to be highly suitable for the
task of field monitoring of toxic metals. The sensitivity of
stripping analysis is attributed to its preconcentration step, in
which trace metals are accumulated onto the working elec-
trode surface [1,2]. This is then followed by the measurement
step, in which the metals are stripped away from the electrode
during an appropriate potential scan. Stripping analysis can
provide useful information on the total metal content, as well
as characterisation of its chemical forms (e.g. labile fraction,
etc.) [3].
Various advances in stripping analysis should accelerate
the realisation of on-site environmental testing of toxic met-
als. New sensor technology has thus replaced the traditional
laboratory-based mercury electrodes and associated cum-
bersome applications (oxygen removal, cell cleaning, etc.)
∗
Corresponding author. Tel.: +39 0554573323; fax: +39 0554573397.
E-mail address: ilaria.palchetti@unifi.it (I. Palchetti).
[4–11]. Portable and compact (hand-held) battery operated
stripping analysers are currently being commercialised for
controlling these field-deployable devices [5,12].
As reported in literature [4], the use of screen-printed elec-
trodes (SPE) is a great simplification in the design and oper-
ation of heavy metal determination, in accordance with the
requirements of a decentralised assay. Screen-printed elec-
trodes are miniaturised devices, based on different layers of
inks printed on an inert plastic or ceramic substrate. More-
over, since they are mass-produced at low cost, they can be
used as disposable. Applications of these devices in the field
of heavy metal detection are extensively reviewed in [11,13].
In this paper, the use of mercury-coated screen-printed
sensors, prepared beforehand in the lab and ready to use
on-site, is proposed. In this way, the handling, the trans-
port and disposal of toxic mercury(II) solutions during de-
centralised measurements is avoided, since the coating is
pre-deposited on the electrode surface. Similar approaches
have been reported in literature: a Nafion
®
-mercury acetate
membrane cast onto a glassy carbon electrode coupled with
classical bulky reference and counter electrodes is reported in
0003-2670/$ – see front matter © 2004 Elsevier B.V. All rights reserved.
doi:10.1016/j.aca.2004.08.065