Electrocatalytic Oxidation of Paracetamol on Ni and NiCu Alloy Modified Glassy Carbon Electrode

In this study we investigated the electrocatalytic oxidation of anti‐inflammatory drug (paracetamol) on Nickel and Nickel–copper alloy modified glassy carbon electrodes (GC/Ni and GC/NiCu) in alkaline solution. These electrodes prepared by galvanostatic method and different electrochemical techniques such as cyclic voltammetry and chronoamperometry were used to track the oxidation process and its kinetics. From Voltammetric studies we concluded that in the presence of drugs the anodic peak current of low valences Nickel species increased, followed by a decrease in the corresponding cathodic current peak. This indicates that drugs were oxidized on the redox mediator which was immobilized on the electrode surface via an electrocatalytic mechanism. Using Laviron's equation, the values of α and k_s for the immobilized redox species were determined. The anodic peak currents show linear dependency with the square root of scan rate. This behavior is the characteristic of a diffusion controlled process. Under the CA regime the reaction followed a Cottrellian behavior and the diffusion coefficient of paracetamol was found in agreement with the values obtained from CV measurements.     

On-column N-dearylation of 2-azetidinones by silica-supported ceric ammonium nitrate

A modified traditional preparative chromatographic column can be used to achieve quantitative N-dearylation of N-(alkoxyphenyl), N-(alkoxynaphthyl), and N-(alkoxybenzyl)-2-azetidinones under mild conditions. Starting materials are charged on top of the column and the pure N-unsubstituted 2-azetidinones leave the column minutes later without need for other purifications. The yields are good-to-excellent and the reaction condition is mild, easy, efficient, and cheap.     

Thickness dependent activity of nanostructured TiO2/α-Fe2O3 photocatalyst thin films

The effect of thickness of TiO₂ coating on synergistic photocatalytic activity of TiO₂ (anatase)/α-Fe₂O₃/glass thin films as photocatalysts for degradation of Escherichia coli bacteria in a low-concentration H₂O₂ solution and under visible light irradiation was investigated. Nanograined α-Fe₂O₃ films with optical band-gap of 2.06 eV were fabricated by post-annealing of thermal evaporated iron oxide thin films at 400 °C in air. Increase in thickness of the Fe₂O₃ thin film (here, up to 200 nm) resulted in a slight reduction of the optical band-gap energy and an increase in the photoinactivation of the bacteria. Sol-gel TiO₂ coatings were deposited on the α-Fe₂O₃ (200 nm)/glass films, and then, they were annealed at 400 °C in air for crystallization of the TiO₂ and formation of TiO₂/Fe₂O₃ heterojunction. For the TiO₂ coatings with thicknesses ≤50 nm, the antibacterial activity of the TiO₂/α-Fe₂O₃ (200 nm) was found to be better than the activity of the bare α-Fe₂O₃ film. The optimum thickness of the TiO₂ coating was found to be 10 nm, resulting in about 70 and 250% improvement in visible light photo-induced antibacterial activity of the TiO₂/α-Fe₂O₃ thin film as compared to the corresponding activity of the bare α-Fe₂O₃ and TiO₂ thin films, respectively. The improvement in the photoinactivation of bacteria on surface of TiO₂/α-Fe₂O₃ was assigned to formation of Ti-O-Fe bond at the interface.     

Dispersive solid phase extraction of lead(II) using a silica nanoparticle-based ionic liquid ferrofluid

We demonstrate the application of an ionic liquid-based ferrofluid to the dispersive solid phase extraction of lead(II) using PAN as the chelator. The ionic liquid contains silica nanoparticles with a magnetic core as the dispersion medium, and its use results in improved stability of the colloidal dispersion and a complete extraction of lead(II) within a few seconds. In addition, there is no need for centrifugation. Specifically, the effect of different variables on the extraction of lead(II) was studied using an experimental design. Lead(II) was quantified by AAS. Under optimized conditions, the calibration graph for lead(II) is linear in the range from 5 to 372 μg L^?1, the relative standard deviation is 1.34 % (for n?=?7), the limit of detection is 1.66 μg L^?1, and the enrichment factor is 200. The maximum adsorption capacity of sorbent was calculated to be 10.7 mg g^?1, and adsorption follows a Langmuir isotherm. Figure

A schematic view of D-SPE experimental set up. We demonstrate the application of an ionic liquid-based ferrofluid to the dispersive solid phase extraction of lead(II) using PAN as the chelator. The ionic liquid contains silica nanoparticles with a magnetic core as the dispersion medium     

A novel water-soluble NHC-Pd polymer: an efficient and recyclable catalyst for the Suzuki coupling of aryl chlorides in water at room temperature

A novel water-soluble NHC-Pd polymer with triethylene glycol legs was developed as a water soluble and highly recyclable catalyst that shows high catalytic activity in the Suzuki-Miyaura coupling of aryl chlorides in high yields in water at room temperature.     

A study on applications of N-substituted main-chain NHC-palladium polymers as recyclable self-supported catalysts for the Suzuki-Miyaura coupling of aryl chlorides in water

The preparation and characterization of a number of main-chain organometallic polymers (NHC-Pd MCOP) with different N-alkyl substituted groups such as benzyl (3a), n-hexyl (3b), and n-dodecyl (3c) are described. Among these polymers, 3c bearing the more lipophilic group n-dodecyl was found to be a more reactive and recoverable catalytic system in the Suzuki-Miyaura cross-coupling reaction of chloroarenes, including both deactivated and hindered aryl chlorides with different types of arylboronic acids under aqueous conditions. While the catalysts seem to be highly recyclable, on the contrary, we have provided much compelling evidence, such as kinetic monitoring, poisoning experiments, and average molecular weight determination before and after catalysis, that shows that the described organometallic polymers might be indeed the source of production of active soluble Pd species in the form of either Pd nanoparticles or fragmented NHC-Pd complexes. Our studies showed that in order to assess whether the catalysts are functioning in a heterogeneous pathway or they are simply a source of production of active Pd species, it is crucial to devise a suitable and highly efficient poison that could capture essentially soluble catalytic species. In this regard, we interestingly found that among a variety of well-known catalyst poisons such as Hg(0), SBA-15-PrSH, and cross-linked poly(4-vinylpyridine) (PVP), only PVP could efficiently quench catalysis, thus providing clear evidence of the formation soluble Pd species in our protocol. In addition, several experiments such as bright-field microscopy, dynamic light scattering (DLS) of the reaction mixture, and kinetic monitoring of the reaction at an early stage confirm not only that the described organometallic polymers could be a source of production of trace amounts of Pd nanoparticles but the capsular structures of these lipophilic polymers in water provides a means of entrapment of nanoclusters in a hydrophobic region, thus accelerating the reaction in pure water in the absence of any co-organic solvent.     

Competitive transport of seven metal cations through bulk liquid membrane using 5,12-di(phenoxymethyl)-1,4-dioxa-7, 10-dithiacyclododecane-2,3-dione as carrier

The competitive metal ion transport of copper(II), cobalt(II), zinc(II), cadmium(II), silver(I), chromium(III) and lead(II) with a S-O donor compound was examined. Competitive transport experiments involving the metal cations from an aqueous source phase through an organic membrane into an aqueous receiving phase have been carried out using 5,12-di(phenoxymethyl)-1,4-dioxa-7,10-dithiacyclododecane-2,3-dione as the ionophore present in the organic phase. Fluxes and selectivities for competitive metal cations transport across bulk liquid membranes have been determined in a variety of chlorinated hydrocarbon and aromatic hydrocarbon solvents. The membrane solvents include: dichloromethane (DCM), chloroform (CHCl₃), 1,2-dichloroethane (1,2-DCE), and nitrobenzene (NB) and also in chloroform-dichloromethane (CHCl₃-DCM) and chloroform-nitrobenzene (CHCl₃-NB) binary mixtures. Although the selectivity for silver(I) cation in all of these organic solvents is fundamentally similar, but the most transport rate for Ag(I) was obtained in dichloromethane. The sequence of transport rate for silver ion in organic solvents was: DCM > CHCl₃ > 1,2-DCE > NB. A linear relationship was observed between the transport rate of silver ion and the composition of CHCl₃-DCM, but a non-linear behavior was observed in the case of CHCl₃-NB binary solution. The influence of the stearic, palmetic and oleic acids as surfactant in the membrane phase on the transport of the metal cations was also investigated.     

In situ formation of silver nanoparticles in PMMA via reduction of silver ions by butylated hydroxytoluene

Silver nanoparticles (Ag NPs) were efficiently generated by in situ reduction of silver ions via butylated hydroxytoluene (BHT), in poly(methyl methacrylate). The characterization of Ag/PMMA by TEM, SEM, XRD, and FTIR indicated that Ag NPs with a face center cubic (fcc) crystal structure and a mean diameter of about 30 nm were dispersed in PMMA matrix with a relatively uniform distribution. In addition, the results of UV–Vis spectroscopy indicated that optical properties of the nanocomposite appeared mainly dependent on the reaction time and temperature. Increasing the reaction time and temperature make higher yield of Ag NPs. A provisional reduction mechanism was also proposed for the formation of the Ag NPs.