Month: September 2021

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The sol-gel polycondensation of tetramethoxysilane has been followed for the first time by functionalization of the oligomeric silane species with a redox active ferrocene. Recording the decrease of the average diffusion coefficient of the mobile species brings information on the sol or gel state, as well as an easy insight of the polycondensation kinetics.

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Reference：
Iron Catalysis in Organic Synthesis | Chemical Reviews,
Iron Catalysis in Organic Synthesis: A Critical Assessment of What It Takes To Make This Base Metal a Multitasking Champion

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Microorganisms exploit extracellular electron transfer (EET) with external minerals during their growth. This process is accompanied by the conversion of chemical energy. Direct electron transfer (DET) from the microorganisms to solid electron acceptors via membrane-bound cytochrome c enzymes or conductive nanowires/pili has been reported. In previous studies, mediated electron transfer (MET) has also been demonstrated to occur through electrochemically active metabolites acting as redox mediators. The microorganisms with EET capabilities have been harnessed for bioelectrochemical systems (BESs) in the bioremediation of environmental contaminants and the production of biofuels and nanomaterials. Electron transfer at the electrode biofilm/solution interface is one of the core phenomena occurring in BESs. The study of the redox reactions occurring in the microenvironment of the biofilm should elucidate the mechanism of microbial EET, which will then help improve the electron transfer efficiency of BESs. The composition of a biofilm is complex and contains many redox secreta and extracellular polymeric substances. Therefore, the specific current generated from the DET or MET pathways cannot be solely detected using classic electrochemical methods. In the present study, the interfacial electron transfer of Shewanella oneidensis MR-1 on an ITO surface was investigated. Cyclic voltammetry (CV) was first applied to study the redox properties of Shewanella and its interaction with ferrocenylmethanol (FcMeOH), which served as an exogenous electron mediator. The cyclic voltammograms showed that the oxidation current of S. oneidensis MR-1 was dramatically enhanced in the presence of 0.01 mmol·L-1 FcMeOH compared to a control, i.e. bacterium-free ITO. This can be explained by the ability of S. oneidensis MR-1 to reduce FcMeOH+ during the positive scan. These results also showed that FcMeOH was a good redox mediator and capable of transferring electrons between the electrode and the bacterial cells. In addition, using the penetration mode in scanning electrochemical microscopy, the current generated from the MET by FcMeOH was collected using a microelectrode. Examination of the approaching curve showed that the current started to increase when the tip was approaching the solution/biofilm interface, providing positive feedback for the FcMeOH-mediated electron transfer between the microelectrode and the bacterial cells. The electrode biofilm/solution microenvironment was also detected, showing the thickness of the solution/biofilm to be 500 mum and the thickness of the biofilm to be 1100 mum. This study indicates that scanning electrochemical microscopy can be used in studying microbial MET. It also provides insight into the electron transfer mechanism of the microbial metabolism from a physical chemistry perspective.

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Reference：
Iron Catalysis in Organic Synthesis | Chemical Reviews,
Iron Catalysis in Organic Synthesis: A Critical Assessment of What It Takes To Make This Base Metal a Multitasking Champion

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A generic amperometric bioassay based on the enzymatic oxidation catalysed by the stable NADH oxidase (NAox) from Thermus thermophilus has been developed for NADH measurements. The NAox uses O2 as its natural electron acceptor and produces H2O2 in a two-electron process. Electrochemical and spectrophotometric experiments showed that the NAox used in this work, presents a very good activity towards its substrate and, in contrary to previously mentioned NADH oxidases, does not require the addition of any exogenous flavin cofactor neither to promote nor to maintain its activity. In addition, the NAox used also works with artificial electron acceptors like ferrocene derivatives. O2 was successfully replaced by redox mediators such as hydroxymethyl ferrocene (FcCH2OH) for the regeneration of the active enzyme. Combining the NAox with the mediator and the horseradish peroxidase we developed an original, high sensitive “redox-flexible” NADH amperometric bioassay working in a large window of applied potentials in both oxidation and reduction modes. The biosensor has a continuous and complementary linearity range permitting to measure NADH concentrations starting from 5 × 10-6 M in reduction until 2 × 103 M in oxidation. This redox-flexibility allows choosing the applied potential in order to avoid electrochemical interferences. The association of the “redox-flexible” concept with NADH dependent enzymes opens a novel strategy for dehydrogenases based bioassays and biosensors. The great number of dehydrogenases available makes the concept applicable for numerous substrates to analyse. Moreover it allows the development of a wide range of biosensors on the basis of a generic platform. This gives several advantages over the previous manufacturing techniques and offers a general and flexible scheme for the fabrication of biosensors presenting high sensitivities, wide calibration ranges and less affected by electrochemical interferences.

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Reference：
Iron Catalysis in Organic Synthesis | Chemical Reviews,
Iron Catalysis in Organic Synthesis: A Critical Assessment of What It Takes To Make This Base Metal a Multitasking Champion

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Autooxidation of ethoxymethylferrocene at 30-50C promoted by the participation of strong and weak carboxylic acids HX is studied. The radical chain mechanism of the process is established, its kinetics characteristics are determined as well as the composition of the products among which other derivatives of ferrocene have been found. Based on the results of the present study and the earlier obtained data on oxidation of hydroxymethylferrocene a mechanism of initiation of the chains general for both metallocomplexes is suggested. It includes the formation of the intermediate CH2OR (R = H, C2H5) and its subsequent oxidative transformations leading to the formation of the peroxide radical C5H 4Fe+?C5H4-CH2O 2 ? and ROH. The role of the approaching and orientation effect in transformations of this intermediate is discussed as well as the mechanism of the investigated reaction in general.

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Reference：
Iron Catalysis in Organic Synthesis | Chemical Reviews,
Iron Catalysis in Organic Synthesis: A Critical Assessment of What It Takes To Make This Base Metal a Multitasking Champion

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The design and synthesis of two new receptors, C20H 19O3BFe and C20H21O3BFe and their anion sensing properties through multiple channels are reported. Both the receptors, having chelating boronic ester Lewis acidic centre as the sole binding site, selectively bind fluoride ion in micromolar concentration. The binding constant of C20H19O3BFe with the fluoride ion has been found to be quite high [K = 106 M -1], whereas it displays a negligible affinity towards other effective competitors, for example acetate and cyanide (K = 10 M-1) and no sensitivity towards other halide ions. Upon selective recognition of F- in acetonitrile, the redox potential of C20H 19O3BFe shifted by DeltaE = 200 mV and the fluorescence emission was quenched drastically. The considerable changes in their absorption spectra are accompanied by the appearance of a new low energy (LE) peak at 566 nm and by a strong colour change from yellow to deep green which allows the prospective for “naked eye” detection of F- anion.

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Reference：
Iron Catalysis in Organic Synthesis | Chemical Reviews,
Iron Catalysis in Organic Synthesis: A Critical Assessment of What It Takes To Make This Base Metal a Multitasking Champion

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The redox potentials of electroactive species are significantly influenced by the solvation characteristics of the medium. This is manifested in the shift of half-peak potentials with the change in the solvent medium. There have been many approaches till date, both experimental and theoretical to understand the role of molecular solvents in the peak potentials of redox species. The electrochemical studies reported here are aimed at understanding the effect of deep eutectic solvents (DESs) which is distinct from conventional solvents in terms of highly concentrated ionic composition, on the half-peak potentials of some standard redox reactions. The redox species selected for this study are distinct either in terms of their charge [Fe(CN)64-/3-, Ru(NH3)62+/3+, and ferrocene methanol, FcMeOH0/+] or their hydrophilic/hydrophobic properties [methyl viologen and ferrocene]. The redox potentials are compared with the values obtained in the aqueous medium which is very well characterized in terms of solvent reorganization energy and free-energy changes. The cyclic voltammetric behavior of the redox species in DES is significantly different from that of aqueous medium. The diffusion coefficients of the redox species in DES measured by EIS and cyclic voltammetry showed significant deviations from that predicted by Stokes-Einstein equation, indicating the dominant effect of Coulombic interactions within the components of DES.

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Reference：
Iron Catalysis in Organic Synthesis | Chemical Reviews,
Iron Catalysis in Organic Synthesis: A Critical Assessment of What It Takes To Make This Base Metal a Multitasking Champion

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Recent developments in bio-fuel cell technology are reviewed. A general introduction to bio-fuel cells, including their operating principles and applications, is provided. New materials and methods for the immobilisation of enzymes and mediators on electrodes, including the use of nanostructured electrodes are considered. Fuel, mediator and enzyme materials (anode and cathode), as well as cell configurations are discussed. A detailed summary of recently developed enzymatic fuel cell systems, including performance measurements, is conveniently provided in tabular form. The current scientific and engineering challenges involved in developing practical bio-fuel cell systems are described, with particular emphasis on a fundamental understanding of the reaction environment, the performance and stability requirements, modularity and scalability. In a companion review (Part II), new developments in microbial fuel cell technologies are reviewed in the context of fuel sources, electron transfer mechanisms, anode materials and enhanced O2 reduction.

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Reference：
Iron Catalysis in Organic Synthesis | Chemical Reviews,
Iron Catalysis in Organic Synthesis: A Critical Assessment of What It Takes To Make This Base Metal a Multitasking Champion

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This work focuses on the investigation of the very early stages of the degradation of coil-coated galvanized steel sheet through swelling and blistering during exposure to chloride-containing aqueous solutions and the possible effect of the zinc-based metallic coating on the degradation at these very early stages. Three types of coil-coated steel whose difference was in the zinc-based metallic coating, namely galvanized, galfan and aluzinc, were considered. Scanning electrochemical microscopy (SECM) operating in the feedback mode was employed to image topographic changes when the samples were left at their spontaneous open circuit potential. Swelling of the coating and nucleation of blisters were observed for all the samples when they were exposed to naturally aerated 0.1 M KCl solution within 24 h exposure. Conversely, featureless and flat surfaces were found when the samples were either exposed to 0.1 M K2SO4 or to 10 mM KCl. For chloride concentrations of 0.1 M and above the chloride ions were observed to promote coating degradation nearly immediately upon immersion in the electrolyte.

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Reference：
Iron Catalysis in Organic Synthesis | Chemical Reviews,
Iron Catalysis in Organic Synthesis: A Critical Assessment of What It Takes To Make This Base Metal a Multitasking Champion

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Abstract?: Results of the studies in the adsorption properties of ??6, ??7, ??8 cucurbituril complexes with inorganic cations (Na+, K+, Cs+), cation of 3,3′-diethyltiocarbocyanine iodide organic dye and neutral organic compounds: adamantanol-1 and ferrocene at the electrode/solution interfaces are summarized. Effects of different factors on the adsorption behavior of the studied supramolecular complexes are analyzed.

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Reference：
Iron Catalysis in Organic Synthesis | Chemical Reviews,
Iron Catalysis in Organic Synthesis: A Critical Assessment of What It Takes To Make This Base Metal a Multitasking Champion

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Cholesterol oxidase (ChOx) has been immobilized by direct adsorption on gold electrodes. The resulting ChOx monolayers have been characterized using atomic force microscopy (AFM) under liquid conditions and quartz crystal microbalance (QCM) techniques. The immobilized enzyme retains its catalytic activity, thus spatially resolved mapping of enzymatic activity has been carried out using scanning electrochemical microscopy (SECM). The replacement, in the enzymatic reaction, of the natural electron acceptor (O2) by an artificial mediator has been also evaluated, in particular, hydroxymethylferrocene (HMF), thionin, nile blue and azure A, have been studied as electron acceptors for reduced ChOx. In addition, the influence of the low cholesterol solubility on the experimental conditions using redox mediators was also discussed. Finally, the response of the enzymatic electrode to varying cholesterol concentrations has been obtained by measuring directly the H2O2 generated in the enzymatic reaction. Cholesterol can be determined amperometrically at +0.5 V (versus SSCE) with a detection limit of 60 muM and a sensitivity of 0.13 muA mM-1.

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Reference：
Iron Catalysis in Organic Synthesis | Chemical Reviews,
Iron Catalysis in Organic Synthesis: A Critical Assessment of What It Takes To Make This Base Metal a Multitasking Champion