Monitoring of pesticide residues in food, beverages, and the environment requires fast, versatile, and sensitive analyzing methods. Direct electrochemical detection of pesticides could represent an efficient solution. Adequate electrode material, electrochemical technique, and optimal operation parameters define the detection method for practical application. In this study, cyclic voltammetric and differential pulse voltammetric techniques were used in order to individually and simultaneously detect two pesticides, i.e., carbaryl (CR) and paraquat (PQ), from an acetate buffer solution and also from natural apple juice. A graphene-modified boron-doped diamond electrode, denoted BDDGR, was obtained and successfully applied in the simultaneous detection of CR and PQ pesticides, using the differential pulse voltammetric technique with remarkable electroanalytical parameters in terms of sensitivity: 33.27 μA μM−1 cm−2 for CR and 31.83 μA μM−1 cm−2 for PQ. These outstanding results obtained in the acetate buffer supporting electrolyte allowed us to simultaneously detect the targeted pesticides in natural apple juice.
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.
Zinc chromite (ZnCr2O4) has been synthesized by the thermolysis of a new Zn(II)-Cr(III) oxalate coordination compound, namely [Cr2Zn(C2O4)4(OH2)6]·4H2O. The coordination compound has been characterized by chemical analysis, infrared spectroscopy (IR), and thermal analysis. The zinc chromite obtained after a heating treatment of the coordination compound at 450 °C for 1 h has been investigated by XRD, FE-SEM, TEM/HR-TEM coupled with selected area electron diffraction (SAED) measurements. The photocatalytic performance of nanosized zinc chromite was assessed for the degradation and mineralization of humic acid (HA) from a drinking water source, envisaging the development of the advanced oxidation process for drinking water treatment technology. A mineralization efficiency of 60% was achieved after 180 min of 50 mg L−1 HA photocatalysis using zinc chromite under UV irradiation, in comparison with 7% efficiency reached by photolysis.
This work reported new voltammetric/amperometric-based protocols using a commercial boron-doped diamond (BDD) electrode for simple and fast simultaneous detection of sulfide and nitrite from water. Square-wave voltammetry operated under the optimized working conditions of 0.01 V step potential, 0.5 V modulation amplitude and 10 Hz frequency allowed achieving the best electroanalytical parameters for the simultaneous detection of nitrite and sulfide. For practical in-field detection applications, the multiple-pulsed amperometry technique was operated under optimized conditions, i.e., −0.5 V/SCE for a duration of 0.3 s as conditioning step, +0.85 V/SCE for a duration of 3 s that assure the sulfide oxidation and +1.25 V/SCE for a duration of 0.3 s, where the nitrite oxidation occurred, which allowed the simultaneously detection of sulfide and nitrite without interference between them. Good accuracy was found for this protocol in comparison with standardized methods for each anion. Also, no interference effect was found for the cation and anion species, which are common in the water matrix.
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.
1 March 2018 in International Journal of Electrochemical Science