We report a simple, facile, and reproducible
method for the fabrication
of electrochemically reduced graphene oxide (ERGO) films on glassy
carbon electrode (GCE) by the self-assembly method. The graphene precursor,
graphene oxide (GO), was self-assembled on GCE through a diamine linker
which was preassembled on GCE by electrostatic interaction between
the positively charged amine and the negatively charged layers of
graphene oxide (GO). The oxygen functional groups present on the surface
of GO were electrochemically reduced to retain the aromatic backbone
of graphene. The attachment of GO followed by its electrochemical
reduction was confirmed by ATR-FT-IR spectroscopy, Raman spectroscopy,
X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), atomic
force microscopy (AFM), and scanning electron microscopy (SEM). Raman
spectra show that the intensity ratio of D and G bands was increased
after the electrochemical reduction of GO. XPS results reveal that
the carbon-to-oxygen ratio was increased after the electrochemical
reduction of electrostatically assembled GO. Further, Raman and XPS
results confirm the removal of oxygen functional groups present on
the surface of GO after electrochemical reduction. Impedance spectral
studies show that the electron transfer reaction was facile at ERGO
modified GCE. Finally, the electrocatalytic activity of ERGO was examined
by studying the oxidations of ascorbic acid (AA), dopamine (DA), and
uric acid (UA). It enhanced the oxidation currents of AA, DA, and
UA when compared to bare GCE. The electrocatalytic activity of the
present modified electrode was highly stable.
The
attachment of nitrogen-doped graphene (NG) on glassy carbon
electrode (GCE) followed by electrodeposition of copper nanostructures
(CuNSs) is described in this paper. Nitrogen-doped graphene oxide
(N-GO) was prepared by intercalating melamine into graphene oxide
(GO) by sonication. The doping of nitrogen was confirmed from the
characteristic peaks at 285.3 and 399 eV in the XPS corresponding
to the C–N bond and nitrogen, respectively. The presence of
amine groups on the N-GO was exploited to attach them on GCE via Michael’s
reaction. Subsequently, N-GO was electrochemically reduced to form
NG by reducing the oxygen functionalities present on the N-GO. Then,
the CuNSs on the NG modified electrode was prepared by electrodeposition
at various applied potentials with different deposition times. The
homogeneous deposition of cubic, spherical, quasidendritic, and dendritic
NS at the applied potentials of 0, −0.10, −0.30, and
−0.40 V, respectively, was evidenced from scanning electron
microscopy (SEM) studies. The surface energy of the system can be
reduced by the intercalated nitrogen in the graphene layer via doping.
Hence, the NG layers with large surface area act as a robust scaffold
for the homogeneous deposition of CuNSs. Further, the electrocatalytic
activity of the NG-CuNSs modified GCE toward glucose oxidation was
studied. In a comparison with NG and CuNSs, the NG-CuNSs exhibited
2-fold higher oxidation current. Further, it was found that the electrocatalytic
activity of the composite electrode depends on the shape of the CuNSs.
Among the different CuNSs, the NG-dendritic CuNSs electrode exhibited
higher electrocatalytic activity. Finally, the practical applicability
of the present sensor was demonstrated by fabricating NG-dendritic
CuNSs on screen printed carbon electrode for the determination of
glucose in human blood serum and urine samples.
In this paper, electrochemically reduced graphene oxide-gold nanoparticles (ERGO-AuNPs) composite film was fabricated on glassy carbon electrode (GCE) by a simple electroless deposition method using a solution containing HAuCl 4 and NH 2 OH. The deposition of AuNPs on ERGO film was achieved via two different approaches. First approach involves the electroless deposition of AuNPs on graphene oxide (GO) modified GCE followed by the electrochemical reduction. The second approach is the electroless 10 deposition of AuNPs on ERGO film modified GCE which was fabricated by self-assembling GO on 1,6hexadiamine modified GCE followed by the electrochemical reduction. The particle coverage estimated from cyclic voltammetry (CV) showed that the particle coverage of AuNPs deposited on ERGO film (22 %) was higher than that of GO film (17 %) and bare GCE (7%) under identical conditions. The obtained higher coverage is attributed ERGO film's ability to spontaneously reduce Au 3+ ions. Although AuNPs 15 deposition was observed at ERGO surface in the absence of NH 2 OH, the particle coverage was much less (2 %) and hence the electroless deposition was carried out in the presence of NH 2 OH. SEM and CV studies showed that the particle coverage and density of AuNPs were increased while increasing the electroless deposition time. 65 modified GCE. The electrochemically reduced graphene oxide (ERGO) film was fabricated on GCE by self-assembly method 31 and it was used to anchor the deposited AuNPs. The term 'electroless deposition' was coined by Brenner and Riddell and it is described as the spontaneous reduction of metal 70 ions to the metallic state in the absence of external source of
The study reports synthesis of poly-(melamine) film on the surface of edge plane pyrolytic graphite (EPPG) followed by its characterization using cyclic voltammetry, square wave voltammetry, field emission scanning electron microscopy (FE-SEM), Horizontal Attenuated Total Reflectance-infrared spectroscopy (HATR-IR) and electrochemical impedance spectroscopy (EIS). The p-(melamine) film coated EPPG has been used as a highly sensitive electrochemical sensor for the determination of propranolol, a β-blocker. The p-(melamine)/EPPG sensor showed excellent electrocatalytic activity for the oxidation of propranolol by significant increment in the peak current and shift in the peak potential toward less positive potential. The fabricated sensor exhibited linear increase in the oxidation peak current with the increasing propranolol concentration in the range 0.1–800 μM with the L.O.D. and L.O.Q. as 9 nM and 30 nM, respectively. The effect of interferents on the peak current response has been studied and it is observed that the common metabolites present in the biological fluid matrix did not interfere in the determination. The p-(melamine)/ EPPG sensor displayed advantages such as simple preparation, high sensitivity, excellent selectivity and good reproducibility toward determination of propranolol. To ensure the analytical applicability of the fabricated sensor, the method has been successfully demonstrated by determining propranolol in the commercial pharmaceutical formulations, human urine and plasma samples.
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