The aim of this study is to prepare and characterize two types of silver-functionalized carbon nanofiber (CNF) composite electrodes, i.e., silver-decorated CNF-epoxy and silver-modified natural zeolite-CNF-epoxy composite electrodes suitable for ibuprofen detection in aqueous solution. Ag carbon nanotube composite electrode exhibited the best electroanalytical parameters through applying preconcentration/differential-pulsed voltammetry scheme.
In this study, the detection protocols for the individual, selective, and simultaneous determination of ibuprofen (IBP) and diclofenac (DCF) in aqueous solutions have been developed using HKUST-1 metal-organic framework-carbon nanofiber composite (HKUST-CNF) electrode. The morphological and electrical characterization of modified composite electrode prepared by film casting was studied by scanning electronic microscopy and four-point-probe methods. The electrochemical characterization of the electrode by cyclic voltammetry (CV) was considered the reference basis for the optimization of the operating conditions for chronoamperometry (CA) and multiple-pulsed amperometry (MPA). This electrode exhibited the possibility to selectively detect IBP and DCF by simple switching the detection potential using CA. However, the MPA operated under optimum working conditions of four potential levels selected based on CV shape in relation to the potential value, pulse time, and potential level number, and order allowed the selective/simultaneous detection of IBP and DCF characterized by the enhanced detection performance. For this application, the HKUST-CNF electrode exhibited a good stability and reproducibility of the results was achieved.
The requirements of the Water Framework Directive to monitor diclofenac (DCF) concentration in surface water impose the need to find advanced fast and simple analysis methods. Direct voltammetric/amperometric methods could represent efficient and practical solutions. Fullerene–carbon nanofibers in paraffin oil as a paste electrode (F–CNF) was easily obtained by simple mixing and tested for DCF detection using voltammetric and amperometric techniques. The lowest limit of detection of 0.9 nM was achieved by applying square-wave voltammetry operated under step potential (SP) of 2 mV, modulation amplitude (MA) of 10 mV, and frequency of 25 Hz, and the best sensitivity was achieved by four-level multiple pulsed amperometry (MPA) that allowed in situ reactivation of the F–CNF electrode. The selection of the method must take into account the environmental quality standard (EQS), imposed through the “watchlist” of the Water Framework Directive as 0.1 µg·L−1 DCF. A good improvement of the electroanalytical parameters for DCF detection on the F–CNF electrode was achieved by applying the preconcentration step for 30 min before the detection step, which assured about 30 times better sensitivity, recommending its application for the monitoring of trace levels of DCF. The electrochemical behavior of F–CNF as a pseudomicroelectrode array makes it suitable for practical application in the in situ and real-time monitoring of DCF concentrations in water.
The synthesis, as well as the mesomorphic and electrochemical properties, of a hetero-bimetallic coordination complex able to self-assemble into a columnar liquid crystalline phase is reported herein. The mesomorphic properties were investigated by polarized optical microscopy (POM), differential scanning calorimetry (DSC) and Powder X-ray diffraction (PXRD) analysis. Electrochemical properties were explored by cyclic voltammetry (CV), relating the hetero-bimetallic complex behaviour to previously reported analogous monometallic Zn(II) compounds. The obtained results highlight how the presence of the second metal centre and the supramolecular arrangement in the condensed state pilot the function and properties of the new hetero-bimetallic Zn/Fe coordination complex.
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