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3D Printed Microfluidic Cell for Spectroelectrochemical Analysis
Šikula, M. ; Vaněčková, Eva ; Hromadová, Magdaléna ; Kolivoška, Viliam
Recent advances in fused deposition modeling 3D printing (FDM 3DP) enabled \nthe manufacture of customized spectroelectrochemical (SEC) devices. Despite significant progress, \nreported designs still rely on conventional optical components (windows and cuvettes). In this \nwork, we apply bi-material FDM 3DP combining electrically conductive and optically \ntranslucent filaments to manufacture a fully integrated microfluidic SEC device. Employing cyclic \nvoltammetric measurements with redox probes, we demonstrate that the platform allows SEC sensing of \nreactants, intermediates, and products of charge transfer reactions in an oxygen- free \nenvironment. Developed approaches pave the way for SEC d vices with dramatically\nreduced costs compared to currently available commercial platforms.\n
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(Spectro) Electrochemical Study of Cibalackrot Derivatives – Potential Chromophores for Singlet Fission\n
Šimková, Ludmila ; Lušpai, Karol ; Klíma, Jiří ; Ludvík, Jiří
Recently, substantial attention has been paid to the search for suitable chromophores for singlet fission. This photophysical effect promises to increase the maximum of theoretical efficiency of solar cells. One type of candidates are derivatives of cibalackrot. Redox properties are critical for their use. Our electrochemical work is focused on the study of oxidation and reduction of a series of substituted cibalackrot derivatives using classic voltammetric techniques and their combination with in situ UV-vis and EPR spectroscopy. The results show the reversible formation of the radical anion (cation) in the first reduction (oxidation) step enabling determination of ´´electrochemical´´ HOMO-LUMO gap.
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UV-Vis and IR Spectroelectrocbemistry of Copper Complexes and Bioactive Compounds
Sokolová, Romana ; Obluková, Michaela ; Sýs, M. ; Mikysek, T. ; Wantulok, J. ; Nycz, J. E. ; Degano, I.
The interpretation of the change of absorption spectrum of an oxidized and reduced molecule\nrecorded during the electron transfer is an efficient tool for the determination of oxidation or\nreduction mechanism. This technique provides the information about the electroactive\nchromophore and is performed in two regimes of electrochemical measurement, cyclic\nvoltammetry and chronoamperometry, respectively. This approach was successfully applied to\nstudy the fundamental electrochemical behavior of recently synthesized copper complexes\nproviding biomimetic activity, ofpolyphenolic bioactive compounds, and also for the reduction\nof halogenated phenanthrolines. The identification of redox products was done by\nchromatographic techniques as HPLC-DAD and HPLC-ESI-MS/MS.
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Preparation and characterization of nanomaterials for electrochemical energy storage
Bouša, Milan
Graphene research is nowadays one of the worldwide most prominent fields of interest in material science due to many extraordinary properties of graphene and related materials. However, the different techniques of synthesis and subsequent handling and/or treatment have a substantial impact on the properties of the graphene and thus a lot of efforts have been focused on developing of the advanced methods for graphene preparation and characterization. Graphene can be easily produced by oxidation and consequent exfoliation of the bulk graphite; however, resulting graphene oxide needs to be reduced back to graphene-like structure due to partial restoration of sp2 network. Herein, a detailed study of the structural evolution of the graphene oxide during electrochemical treatment has been performed using X-ray photoelectron, Raman and infrared spectroscopies and the results were compared with non-oxidized graphene nano-platelets. Additionally, graphene oxide in composite with LiFePO4 olivine material, which is electrochemically almost inactive in a freshly made state, has been tested by repeated electrochemical cycling. Using various electrochemical methods, the progressive electrochemical activity enhancement has been observed and spontaneous graphene reduction was identified as responsible for this...
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Spectroelectrochemical study of porphyrin derivatives in non-aqueous solvents
Povišer, Martin ; Dian, Juraj (advisor) ; Pšenčík, Jakub (referee)
Porphyrins and their derivatives constitute an important group of com- pounds taking part in vital biological processes such as transport of oxygen in blood and in photosynthesis. Electrochemical experiments such as cyclic volta- mmetry allow to examine the energetic balance of oxidation and reduction pro- cesses of particles under study. In spectroelectrochemical studies, the experiment is extended with optical characterization of the arising oxidized or reduced spe- cies. These are means to study of electronic structure of species and available electron transitions. Such studies are especially interesting in case of porphyrins due to possible elucidation of electron transfer in photosynthetic chains. This work presents: (a) an elementary theoretical treatment of electrode reactions fun- damental for electrochemical experiments, (b) description of the experimental realization of spectroelectrochemical study of porphyrins and derivatives in non- aqueous solvents, and (c) results of original spectroelectrochemical measurements on protoporphyrin IX in medium dimethylformamide. 1
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Transparent boron-doped diamond electrode (t-BDDE) for spectroelectrochemistry
Lušpai, K. ; Keszeliová, D. ; Barlog, M. ; Petrák, Václav
In this work we have studied the properties of high quality boron-doped diamond layers prepared on transparent substrate and their use as working electrode for EPR/UV-VIS-NIR spectroelectrochemistry. Final goal of this work is to benefit from the wide potential window of boron-doped diamond electrodes even in the field of the EPR/UV-VIS-NIR spectroelectrochemistry. The studied electrodes are compatiable with UV-VIS-NIR measurements. Spectral background is stable within the whole electrochemical window. Some of the electrodes, with lower doping level, are also compatible with EPR spectroscopy. In this work, the electrodes and their properties are presented and usability is demonstrate by the spectrochemistry on real sample.
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Transparent boron-doped diamond electrode (t-BDDE) for spectroelectrochemistry
Lušpai, K. ; Keszeliová, D. ; Barlog, M. ; Petrák, Václav
In this work we have studied the properties of high quality boron-doped diamond layers prepared on transparent substrate and their use as working electrode for EPR/UV-VIS-NIR spectroelectrochemistry. Final goal of this work is to benefit from the wide potential window of boron-doped diamond electrodes even in the field of the EPR/UV-VIS-NIR spectroelectrochemistry. The studied electrodes are compatiable with UV-VIS-NIR measurements. Spectral background is stable within the whole electrochemical window. Some of the electrodes, with lower doping level, are also compatible with EPR spectroscopy. In this work, the electrodes and their properties are presented and usability is demonstrate by the spectrochemistry on real sample.
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On UV-Vis Spectroelectrochemistry of Luteolin-7-O-Glucoside
Castano, A. ; Sokolová, Romana ; Degano, I.
The UV-Vis spectroelectrochemical cell containing an optically transparent platinum net used as the working electrode was tested in two regimes of electrochemical measurement, cyclic voltammetry and chronoamperometry, respectively. A three electrode setup used silver quasi reference electrode and platinum electrode serving as a counter electrode. The calibration of the spectroelectrochemical cell was performed for one-electron oxidation processes as well as for two-electron oxidations. The spectral changes during the oxidation of luteolin-7-O-Glucoside gave the information about the electroactive chromophores in molecule. Resulted spectra were compared with luteolin. The identification of products of oxidation was done by complementary analytical techniques HPLC-DAD and HPLC-ESI-MS/MS.
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Redox Properties of Fluorinated Derivativers of 1,3-Diphenylisobenzofuran-Chromophores for Singlet Fission
Šimková, Ludmila ; Ludvík, Jiří
Derivatives of 1,3-diphenylisobenzofuran attract interest because they should be efficient as the molecules for singlet fission. The understanding of singlet fission in isolated molecules might be advantageous for use as solar cell sensitizers. This study is focused on fluorinated derivatives of 1,3-diphenylisobenzofuran and the effect of the position of fluorine atoms on their redox properties. For characterization of the redox properties standard electrochemical methods, and in situ UV-vis and EPR spectroscopy techniques were used.
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Preparation and characterization of nanomaterials for electrochemical energy storage
Bouša, Milan
Graphene research is nowadays one of the worldwide most prominent fields of interest in material science due to many extraordinary properties of graphene and related materials. However, the different techniques of synthesis and subsequent handling and/or treatment have a substantial impact on the properties of the graphene and thus a lot of efforts have been focused on developing of the advanced methods for graphene preparation and characterization. Graphene can be easily produced by oxidation and consequent exfoliation of the bulk graphite; however, resulting graphene oxide needs to be reduced back to graphene-like structure due to partial restoration of sp2 network. Herein, a detailed study of the structural evolution of the graphene oxide during electrochemical treatment has been performed using X-ray photoelectron, Raman and infrared spectroscopies and the results were compared with non-oxidized graphene nano-platelets. Additionally, graphene oxide in composite with LiFePO4 olivine material, which is electrochemically almost inactive in a freshly made state, has been tested by repeated electrochemical cycling. Using various electrochemical methods, the progressive electrochemical activity enhancement has been observed and spontaneous graphene reduction was identified as responsible for this...
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