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Electrochemistry of Polynitrocalix-[4]-arenes
Liška, Alan ; Ludvík, Jiří
Calix[4]arene is a suitable inert and stable frame for building "smart" molecules and supramolecular assemblies. Polynitrocalix[4]arenes where reducible nitro groups are located at the upper rim are promising precursors for aimed development of sensors. In this work a series of mono-, di-, tri- and tetra nitroderivatives was reduced, the sequence of individual steps was described and the mechanism discussed. It was found that in this molecule with several redox centers all nitro groups are electronically isolated and thus are reduced independently yielding poly-radical ions. Two different couples of equivalent nitro groups were proved in tetranitro derivatives. The experimental results were confirmed by quantum chemical calculations.
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New Characterisation Approaches for Carbon Ionic Liquid Electrodes (CILES)
Mikysek, T. ; Stočes, M. ; Švancara, I. ; Vytřas, K. ; Ludvík, Jiří
Within this study, some new approaches to characterize the carbon paste mixtures and the respective carbon ionic liquid electrodes (CILEs) are presented and their properties discussed. Particular attention has been paid to the changes of the resistivity, relative to the dependence on composition of the CILE. Three types of carbon ionic liquid pastes were examined, and for the interpretation of experimental data, the results were compared with those of "classic" carbon paste electrode (CPE) based on graphite powder. Some problems connected with homogeneity and stability of carbon pastes are also discussed.
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Optimization of a Flow Rate for a Hyphenation of Voltammetry with Electrospray Ionization Mass Spectrometry
Jaklová Dytrtová, Jana ; Jakl, M. ; Norková, Renáta ; Navrátil, Tomáš
The hyphenation of an electrochemical cell prior to mass spectrometer with electrospray ionization allows studying of products and/or of intermediates of electrode reactions. The measurement is realized in a flowing system. The flow rate of the sample markedly influences the MS signal intensity of the product. The calculated optimum value for the electrochemical cell with the sweep volume 0.72 μL is in the range from 0.4 to 0.5 mL h -1 . The experimental optimal value is 0.45 mL h -1 . The optimization of the flow rate has to be provided individually for each product, because the intensity also depends on the rate of the electrode reaction and product stability.
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(Strept)avidin-biotin interactions at amalgam electrodes covered by thiol monolayer
Josypčuk, Bohdan ; Mareček, Vladimír ; Yosypchuk, O.
Carboxylic group of 11-mercaptoundecanoic acid (MUA) can be used to creat a peptide bond with species containing amino group, e.g., peptides, and proteins. By the help of EDC-NHS technology, streptavidin or avidin was covalently bonded with MUA-monolayer at a silver solid amalgam electrode. Such prepared electrode was used for detecting biotin and biotinylated albumin in the supporting electrolyte (0.15 M NaCl, 0.05 M TRIS, pH 7.0). Electrochemical impendance spectroscopy was performed for the biosensor response monitored by impedance spectroscopy. Binding of biotin or biotinylated albumin with (strept)avidin a change in the resistance of the sensor in the concentration range of 0.5-20 μg mL-1. Electrochemical regeneration of the amalgam electrode permits simply to renew its surface and to create the new biosensor.
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Electrochemistry of Potential Eu MRI Complexes
Gál, Miroslav ; Sokolová, Romana ; Kielar, P.
Properties of the several potential contrast agents for magnetic resonance imaging (MRI) with Eu(III)/Eu(II) redox couple were investigated by means of the electrochemical methods. Cyclic voltammetry, phase sensitive AC voltammetry, and DC polarography were utilized to elucidate the mechanism of the reduction/oxidation of Eu ion in the presence of these compounds. Moreover, the stability constants of the Eu(II)-MRI agent complexes were also determined. Some suggestions on the chemical structure of the potential contrast agents for MRI are also made.
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FOX-7 - Study of Reduction Products of Spectroelectrochemical Methods
Šimková, Ludmila ; Dmitrieva, E. ; Klíma, Jiří ; Dunsch, L. ; Ludvík, Jiří
A new energetic material 2,2-dinitroethene-1,1-diamine (FOX-7) is recently broadly tested because of its high performance and very low sensitivity. On the other hand, its electrochemical and redox properties have not been studied yet. Our results show that FOX-7 is reduced in aprotic solvents only by two one-electron steps up to -2.9 V. The color changes during reduction of FOX-7 and reversibility of the redox process indicate the presence of radical intermediates. Therefore in situ UV-vis-NIR and ESR spectroelectrochemical investigations were performed. The products after exhaustive electrolyses were separated by HPLC and are identified by mass spectrometry. The possible formation of gaseous products was followed online EC-GC.
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Assessment of Potential Risk Connected with the Use of Mercury and Mercury Electrodes
Navrátil, Tomáš ; Švancara, I. ; Mrázová, K. ; Nováková, Kateřina ; Chýlková, J. ; Pelclová, D.
This contribution tries to asses critically the danger connected with utilization of mercury in different branches of human activites. The main attention was devoted to electrochemistry, mainly to voltammetry and polarography. However, to other branches were characterized as well: dentistry, in battery production, mining industry, and a few others. The most toxic and contarily almost nontoxic forms of mercury and of its compounds were characterized. Some interesting cases of exposure to mercury, according to the database of the Czech Toxicological Information Centre (TIC) (from years 1995-2011), have been reported,
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Use of Copper Solid Amalgam Electrode for Determination of Triazolic Fungicide Tebuvonazole
Nováková, Kateřina ; Navrátil, Tomáš ; Jaklová Dytrtová, Jana ; Chýlková, J.
With the use newly developed mercury meniscus-modified copper solid amalgam electrode (inner diamter 1.5 mm), the voltammetric behavior of fungicide tebuconazole was researched by differential pulse voltammetry (DPV) and cyclic voltammetry (CV). Applying CV and elimination voltammetry with linear scan (EVLS), the reaction mechanism was investigated. The optimum conditions for DPV determination of this triazolic fungucude were identified in Britton-Robinson buffer/methanol (1:1, v/v) of pH 6.3 DPV with optimized parameters (Ein = +400 mV vs. Ag/AgCl/3M KCl, scan rate 20 mV s-1) was used for determination of determination of tebuconazole in analyzed solutions. Application the prolonged time (60 s), the limit of detection 2.10-7 molL-1. The applicability of the developed method was verified on the analysis of the real soil solution sample.
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Investigation of Complexes of Tebuconazole with Zinc
Jakl, M. ; Norková, Renáta ; Navrátil, Tomáš ; Jaklová Dytrtová, Jana ; Balík, J.
Tebuconazole is one of the most utilized triazole pesticides in agriculture. Its stability is highly affected by complexation with metals. Moreover, it creates more or less stable complexes with essential elements that become unavailable to plants. In the system with overbundant tebuconazole, an inert (very stable) complex with Zn was found. Elimination voltammetry wit linear scan was used for revealing of the electrode processes on the mercury surface. The relatively slow kinetically controlled step in tebuconazole/Zn complex formation indication indicates the great ability of Zn-tebuconazole system to react with more ligans. Therefore, multiligand Zn-tebuconazole complexes with other ligands are expected in the nature.
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