Search results for " voltammetry"
showing 10 items of 295 documents
Dialkyl(butadiene)cyclopentadienylmolybdenum(III) Complexes. Synthesis, Characterization, and Reactivity
2000
International audience; Treatment of CpMo(η4-diene)Cl2 (diene = 1,3-butadiene, C4H6, 1‘; isoprene, C5H8, 1‘ ‘; 2,3-dimethyl-1,3-butadiene, C6H10, 1‘ ‘) in diethyl ether at low temperature with 2 equiv of alkylmagnesium RMgX reagents affords the corresponding dialkyl complexes CpMo(η4-1,3-diene)R2 (2, 2‘, 2‘ ‘, R = CH3, a; CH2Ph, b; CH2SiMe3, c). These species are isolable in moderate yields and have been fully characterized by EPR, elemental analyses, and cyclic voltammetry. They all show a reversible reduction process at relatively low potentials and an irreversible oxidation. The structure of 2‘ ‘a was confirmed by single-crystal X-ray diffraction. The mixed complex CpMo(η4-C4H6)Cl(CH3), …
Electrochemical reduction properties of A-frame compounds and crystal structure of Pd2(dppm)2(Me)2(Br)+ dimer
2006
Abstract Two series of A-frame complexes, [Pd2(dppm)2(R)2(μ-X)]+ (R = Me and X = Cl, Br, I, H; R = Mes and X = Br, I), were investigated by cyclic voltammetry (CV). The 2-electron reduction potentials for the first series increase from I (−1.10), Br (−1.17), Cl (−1.25) to H (−1.65 V versus SCE, in CHCl3), as well as in the second series; Br (−1.35) and I (−1.38 V versus SCE, in THF). The nature of the LUMO where the electron reduction takes place is qualitatively addressed by DFT on the corresponding model complexes [Pd2(H2PCH2PH2)2(R)2(μ-X)]+. The LUMO and (LUMO + 1) of the halide derivatives exhibit the presence of Pd d x 2 - y 2 atomic orbitals interacting in an anti-bonding fashion with…
Versatile redox reactivity of triaryl-meso-substituted Ni(ii) porphyrin
2014
The electrochemical oxidation of nickel(II) 5,15-p-ditolyl-10-phenylporphyrin (1-Ni) leads to the formation of different coupling products, with the distribution depending on the nature of the solvent (CH2Cl2–CH3CN, CH2Cl2, DMF), the cell configuration (2 or 3 compartments) and the number of electrons abstracted. In a two compartment configuration (anode and cathode in the same compartment) in a CH2Cl2–CH3CN mixture, nickel(II) 5-chloro-10,20-p-ditolyl-15-phenylporphyrin (1-Ni-Cl) was isolated in good yield and its mechanism of formation is proposed. Switching to the three compartment configuration, the meso-β/meso-β doubly fused dimer (3-Ni) is detected as the major product whereas in pure…
Cobalt-Containing Silicotungstate Sandwich Dimer [{Co3(B-β-SiW9O33(OH))(B-β-SiW8O29(OH)2)}2]22-
2005
The 6-cobalt-substituted [{Co3(B-beta-SiW9O33(OH))(B-beta-SiW8O29(OH)2)}2]22- has been characterized by IR and UV-vis spectroscopy, elemental analysis, magnetic studies, electrochemistry, and gel filtration chromatography. A single-crystal X-ray analysis was carried out on K10Na12[{Co3(B-beta-SiW9O33(OH))(B-beta-SiW8O29(OH)2)}2].49H2O (KNa-1), which crystallizes in the monoclinic system, space group P2(1)/n, with a=19.9466(8) A, b=24.6607(10) A, c=34.0978(13) A, beta=102.175(1) degrees, and Z=2. Polyanion 1 represents a novel class of asymmetric sandwich-type polyanions. It contains three cobalt ions, which are encapsulated between an unprecedented (B-beta-SiW9O34) fragment and a (B-beta-Si…
Electrochemical reduction of graphene oxide and its in situ spectroelectrochemical characterization
2012
The electrochemical properties of self-assembled films of graphene oxide (GO) on mercaptoethylamine (MEA) modified rough Au-surfaces were studied. The film deposition process on MEA primed gold was followed by surface plasmon resonance measurements and the film morphology on 3-aminopropyltriethoxysilane primed Si(100)-surface was studied by atomic force microscopy. The deposited few layer thick GO films on gold were electrochemically reduced by cyclic voltammetry simultaneously as the structural changes in the film were recorded by in situ vibrational spectroscopies. In situ surface enhanced infrared spectroscopy results indicate that the effect of the applied potential on the GO structure …
A comparative evaluation of palladium and platinum nanoparticles as catalysts in proton exchange membrane electrochemical cells
2008
The goal of the present study is the development and comparative characterisation of carbon-supported and nanostructured Pd- and Pt-based electrocatalysts for hydrogen oxidation in Proton Exchange Membrane (PEM) H2/O2(air) fuel cells and proton reduction in PEM water electrolysers. Catalysts have been synthesised in a solution using a combined impregnation/reduction polyol method. They have been characterised using X-ray Diffraction (XRD) analysis, Transmission Electron Microscopy (TEM), Thermogravimetric Analysis (TGA) and cyclic voltammetry. NanoPt, nanoPd and nanoPt-Pd catalysts deposited onto a carbon carrier have been used to prepare Membrane-Electrode Assemblies (MEAs) which, in turn,…
Experimental analysis of materials in proton exchange membrane electrolysis cells
2019
Abstract An accelerated supply and demand of energy has resulted in an increased need for efficient energy storage options, where storing energy in hydrogen gas emerges as one of the most attractive. In this study, a singular proton exchange membrane (PEM) electrolysis cell was designed using adequately low-cost materials, and tested using polarisation curves, cyclic voltammetry and AC impedance. A comparative study of various micro porous layer (MPL) materials was performed in an effort to find suitable options which are able to steadily operate under anodic conditions. The best performance was achieved using carbon cloth, however this material was unstable. Untreated porous titanium and n…
Electrochemical incineration of 1,2-dichloroethane: Effect of the electrode material
2008
The electrochemical incineration of 1,2-dichloroethane (EDC) at Pt, Au, boron-doped diamond (BDD), Ebonex, stainless steel, Ti/IrO2–Ta2O5 and PbO2 has been studied in acid media by cyclic voltammetry and bulk electrolysis. It has been shown that the performances of the process dramatically depend on the anodic material. Higher current efficiencies were obtained at BDD. In particular, at proper values of applied current density, it is possible to obtain the almost complete conversion of EDC to CO2 at BDD with current efficiencies higher than 40%.
Electrochemical reduction and carboxylation of halobenzophenones
2002
Abstract The electrochemical reduction of a series of halogenated benzophenones XC6H4COC6H4Y (1) was studied in aprotic solvents, in the absence and presence of CO2, by cyclic voltammetry (CV) and controlled-potential electrolysis. The mechanism of electroreduction in dimethylformamide (DMF) has been investigated in some detail. Most of the compounds undergo reductive carbonhalogen bond cleavage in the time window of CV. The radical anions derived from difluorobenzophenones (X=Y=4-F; X=2-F, Y=4-F) as well as from the 3-chloro derivative are quite stable with a cleavage rate constant (kc) of the order of 10−2 s−1 or less. With 4-chloro-, 2-chloro-, 4,4′-dichloro- and 2,4′-dichorobenzophen…