For the challenging nature of the zirconium environment analysis, this study consists to analyze the electrochemical behavior of Zirconium in both aqueous and organic media. To that end first the electrolytic media wa...For the challenging nature of the zirconium environment analysis, this study consists to analyze the electrochemical behavior of Zirconium in both aqueous and organic media. To that end first the electrolytic media was selected on the basis of the Pourbaix potential-pH diagram, which provides informations on the predominance of Zr<sup>(IV) </sup> ion and Zr in aqueous media. In aqueous media, analyzes were first carried out in acidic media then in basic media. Studies have thus revealed that the acidic environment is not favourable for the electrochemical analysis of zirconium. Voltammograms obtained in an acidic environment show no zirconium detection signal;this is due to the strong presence of H<sup>+</sup> ions in the solution. We have also observed in acidic media the phenomenon of passivation of the electrode surface. In aqueous alkaline media (pH = 13), we have drawn in reduction several Intensity-Potential curves by fixingsome technical parameterslike scanning speed, rotation speed of the electrode. The obtained voltammograms show cathodic waves, starting from -1.5 V/DHW and attributed to the reduction of Zr<sup> (IV) </sup> to Zr (0). The last phase of this study focused on the electrochemical analysis of zirconium in an organic media. In this media, several intensity-potential curves were plotted in reduction and in cyclic voltammetry with various parameters. Through several reduction analysis, the Zr<sup> (IV) </sup> was reduced to Zr (0) to the potential of -1.5 V/DHW. The electrochemical analysis of zirconium in organic media seems globally easier to achieve thanks to its large solvent window (i.e. dimethylformamide (DMF) solvent window > 6 V).展开更多
Electrochemical detection of 3-methyl-4-nitrophenol (MNP) in direct phenol oxidation occurs at high potentials and generally leads to progressive passivation of the electrochemical sensor. This study describes the use...Electrochemical detection of 3-methyl-4-nitrophenol (MNP) in direct phenol oxidation occurs at high potentials and generally leads to progressive passivation of the electrochemical sensor. This study describes the use of a carbon fiber microelectrode modified with a tetrasulfonated nickel phthalocyanine complex for the detection of MNP at a lower potential than that of direct phenol oxidation. The MNP voltammogram showed the presence of an anodic peak at -0.11 V vs SCE, corresponding to the oxidation of the hydroxylamine group generated after the reduction of the nitro group. The effect of buffer pH on the peak current and SWV parameters such as frequency, scan increment, and pulse amplitude were studied and optimized to have better electrochemical response of the proposed sensor. With these optimal parameters, the calibration curve shows that the peak current varied linearly as a function of MNP concentration, leading to a limit of detection (LoD) of 1.1 μg/L. These results show an appreciable sensitivity of the sensor for detecting the MNP at relatively low potentials, making it possible to avoid passivation phenomena.展开更多
文摘For the challenging nature of the zirconium environment analysis, this study consists to analyze the electrochemical behavior of Zirconium in both aqueous and organic media. To that end first the electrolytic media was selected on the basis of the Pourbaix potential-pH diagram, which provides informations on the predominance of Zr<sup>(IV) </sup> ion and Zr in aqueous media. In aqueous media, analyzes were first carried out in acidic media then in basic media. Studies have thus revealed that the acidic environment is not favourable for the electrochemical analysis of zirconium. Voltammograms obtained in an acidic environment show no zirconium detection signal;this is due to the strong presence of H<sup>+</sup> ions in the solution. We have also observed in acidic media the phenomenon of passivation of the electrode surface. In aqueous alkaline media (pH = 13), we have drawn in reduction several Intensity-Potential curves by fixingsome technical parameterslike scanning speed, rotation speed of the electrode. The obtained voltammograms show cathodic waves, starting from -1.5 V/DHW and attributed to the reduction of Zr<sup> (IV) </sup> to Zr (0). The last phase of this study focused on the electrochemical analysis of zirconium in an organic media. In this media, several intensity-potential curves were plotted in reduction and in cyclic voltammetry with various parameters. Through several reduction analysis, the Zr<sup> (IV) </sup> was reduced to Zr (0) to the potential of -1.5 V/DHW. The electrochemical analysis of zirconium in organic media seems globally easier to achieve thanks to its large solvent window (i.e. dimethylformamide (DMF) solvent window > 6 V).
文摘Electrochemical detection of 3-methyl-4-nitrophenol (MNP) in direct phenol oxidation occurs at high potentials and generally leads to progressive passivation of the electrochemical sensor. This study describes the use of a carbon fiber microelectrode modified with a tetrasulfonated nickel phthalocyanine complex for the detection of MNP at a lower potential than that of direct phenol oxidation. The MNP voltammogram showed the presence of an anodic peak at -0.11 V vs SCE, corresponding to the oxidation of the hydroxylamine group generated after the reduction of the nitro group. The effect of buffer pH on the peak current and SWV parameters such as frequency, scan increment, and pulse amplitude were studied and optimized to have better electrochemical response of the proposed sensor. With these optimal parameters, the calibration curve shows that the peak current varied linearly as a function of MNP concentration, leading to a limit of detection (LoD) of 1.1 μg/L. These results show an appreciable sensitivity of the sensor for detecting the MNP at relatively low potentials, making it possible to avoid passivation phenomena.