No (6906)
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6906
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Spectroelectrochemical Devices for Monitoring of Intermediates and Products on Carbonbased Composite Electrodes
Vaněčková, Eva; Šikula, M.; Hrdlička, Vojtěch; Sebechlebská, Táňa; Kolivoška, Viliam
2024 - English
Spectroelectrochemistry (SEC), as an interdisciplinary field, provides us with more comprehensive information about electroactive molecules involved in charge transfer reactions. Commercially\navailable SEC cells most often have an incorporated platinum working electrode, which can limit the range of the usable potential window and, in addition, can complicate the analysis due to the\nabsorption phenomenon. In this work, we designed and manufactured two types of custom-made SEC cells employing optically transparent carbon-based working electrodes for UV-Vis monitoring of reactants and electrogenerated intermediates and products. The first SEC cell is entirely manufactured by 3D printing using fused deposition modeling (FDM) by combining optically transparent (PET) and electrically conductive (PLA-CB) filaments. The second SEC cell employs pencil graphite (PG) rods as the working electrode (PGE) and its body is manually assembled from quartz slides. The functionality of the FDM 3D printed SEC cell and manually assembled quartz SEC cell were verified by cyclic voltammetry with in situ UV-Vis spectroscopic absorption monitoring of ruthenium(III) acetylacetonate (Ru(ac)3) redox-active probe dissolved in an aqueous or non-aqueous deaerated solvent, respectively. Both presented cells enable complete redox reversible conversion and strictly oxygen-free conditions.
Keywords:
pencil graphite electrode; spectroelectrochemistry; 3D printed electrode
Available on request at various institutes of the ASCR
Spectroelectrochemical Devices for Monitoring of Intermediates and Products on Carbonbased Composite Electrodes
Spectroelectrochemistry (SEC), as an interdisciplinary field, provides us with more comprehensive information about electroactive molecules involved in charge transfer reactions. ...
Basic characteristics of sulfide catalysts for the direct decomposition of H2S
Bonnet, Florian; Kaluža, Luděk
2024 - English
Sulfide catalysts are crucial in the hydrodesulfurization (HDS) of petroleum fractions, facilitating the hydrogenolysis of carbon-sulfur bonds. This process generates significant volumes of hydrogen sulfide (H2S), which is typically processed in the Claus unit. However, excess H2S can overwhelm the Claus process, creating both operational and environmental challenges. Researchers are now exploring sulfide catalysts for the direct thermo-catalytic decomposition of H2S to address this issue. Supported catalysts, like Mo/Al2O3, and commercial catalysts, considered typical monolayer-type well-dispersed catalysts, show the highest O2 uptake, ranging from 41.29 μmol/g for MoS2/Al2O3 (KLO) to 58.70 μmol/g for the commercial 715. Unsupported multilayer catalysts, such as Ni/MoWS2 (KKP), exhibit lower O2 uptake at 2.54 μmol/g, though it demonstrates high HDS activity with thiophene. Moreover, O2 uptake effectively describes the sintering of the Mo monolayer phase during the thermocatalytic reaction of H2S at 800°C. These O2 uptakes clearly correlate with the XRD patterns, where the MoS2 phase is X-ray amorphous with an O2 uptake of about 19.04 μmol/g, while the MoS2 phase in the spent catalyst shows certain crystallinity exhibiting an average particle size by Scherrer equation of about 6 nm and the O2 uptake of 1.63 μmol/g. O2 chemisorption thus serves as a valuable measure of the dispersion of Mo sulfides. The results obtain with the study of CoMo/Al2O3 (KJJ-family catalysts), highlight the correlation between the increasing amount of adsorbed O2 with the increasing nominal loading of MoO3 and the increasing rate constant of thiophene kTH. This research reveals the potential of these catalysts in hydrocarbon refining. The findings underline the connection between catalytic chemistry, process engineering, and environmental sustainability, with the objective to enhance industrial refining processes.
Keywords:
sulfide catalyst; O2 chemisorption; H2S decomposition
Available at various institutes of the ASCR
Basic characteristics of sulfide catalysts for the direct decomposition of H2S
Sulfide catalysts are crucial in the hydrodesulfurization (HDS) of petroleum fractions, facilitating the hydrogenolysis of carbon-sulfur bonds. This process generates significant volumes of hydrogen ...
Electrochemistry of Acetaminophen
Mikysek, T.; Ludvík, Jiří
2024 - English
The contribution is focused on electrochemical oxidation of acetaminophen mainly in non-aqueous media. The influence of various organic solvents as well as the pH effect is described herein. The redox properties of acetaminophen were studied by means of cyclic voltammetry, and rotating-disk voltammetry. We found that the protonation/deprotonation of acetaminophen acts as a ratedetermining step, where the stability of phenoxy radical intermediate plays an important role.
Keywords:
acetaminophen; phenacetine; voltammetry
Available on request at various institutes of the ASCR
Electrochemistry of Acetaminophen
The contribution is focused on electrochemical oxidation of acetaminophen mainly in non-aqueous media. The influence of various organic solvents as well as the pH effect is described herein. The redox ...
A New Approach to Determining the Drug Guaifenesin Using Voltammetric and Flow Injection Analysis
Kelíšková, P.; Matvieiev, O.; Sokolová, Romana; Janíková, L.; Behúl, M.; Šelešovská, R.
2024 - English
This study presents a new method for detecting guaifenesin (GFE) in pharmaceutical samples. We employed screen-printed sensors with a boron-doped diamond electrode (BDDE) to develop and validate both voltammetric and flow amperometric methods. These approaches were effectively used to analyze model solutions, pharmaceutical preparations, and serum samples spiked with GFE, producing accurate results comparable to those obtained with HPLC/DAD analysis. The developed methods provide straightforward, sensitive, and selective means for determining GFE in various sample matrices, underscoring the potential of SP/BDDE in electrochemical analysis.
Keywords:
guaifenesin; screen-printed sensor; boron-doped diamond electrode
Available on request at various institutes of the ASCR
A New Approach to Determining the Drug Guaifenesin Using Voltammetric and Flow Injection Analysis
This study presents a new method for detecting guaifenesin (GFE) in pharmaceutical samples. We employed screen-printed sensors with a boron-doped diamond electrode (BDDE) to develop and validate both ...
Optimization of Parameters Used in the Application of Elimination Voltammetry with Linear Scan
Navrátil, Tomáš; Trnková, L.; Hrdlička, Vojtěch; Li, X.
2024 - English
Elimination Voltammetry with Linear Scan (EVLS) is a well-established mathematical method that aids in understanding an analyzed electrochemical system. In almost 30 years since its derivation, it has become a “black-box” technique that is applied automatically (in most cases due to its incorporation into a voltammetric software) without thinking about its fundamentals. However, the choice of optimum parameters under which DC voltammetric data (from which elimination curves are calculated) is crucial. This contribution deals with revealing the optimum ratio of applied scan rates and their absolute values (i.e., times of recording) in dependence on the character of the investigated system (diffusion-controlled process, adsorption-controlled process, etc.).
Keywords:
elimination voltammetry with linear scan; optimization; adsorption
Available on request at various institutes of the ASCR
Optimization of Parameters Used in the Application of Elimination Voltammetry with Linear Scan
Elimination Voltammetry with Linear Scan (EVLS) is a well-established mathematical method that aids in understanding an analyzed electrochemical system. In almost 30 years since its derivation, it has ...
Fenotypování jarního ječmene na odolnost vůči suchu
Klem, Karel; Findurová, Hana; Panzarová, K.; Pytela, J.; Trtílek, M.; Holub, Petr
2024 - Czech
Odolnost rostlin/plodin vůči suchu představuje komplex vlastností, které se různě uplatňují v závislosti na typu, závažnosti a načasování sucha. Proto je nutné poměrně komplexní hodnocení morfologické a fyziologické fenotypové reakce na sucho. Tato metodika se zaměřuje na vývoj postupů a vyhodnocení komplexní fenotypové odezvy genotypů jarního ječmene na sucho pomocí neinvazivně měřených parametrů založených na červeno-zeleno-modrém (RGB) zobrazování, termálním infračerveném zobrazování a zobrazovací fluorescence chlorofylu měřených v rámci automatizované fenotypovací platformy. Vývoj metodiky byl založen na experimentu, ve kterém byly sledovány dynamické změny odezvy šesti genotypů ječmene, reprezentujících širokou škálu tolerance k suchu (od genotypu velmi citlivého až po genotyp velmi tolerantní), na kontinuální vysychání až k bodu vadnutí a následné opětovné zavlažení. Byly identifikovány tři kritické termíny v průběhu sucha a opětovného zavlažení, klíčové pro identifikaci odolnosti jarního ječmene vůči suchu: i) dosažení 50% hladiny dostupné půdní vody, ii) dosažení bodu vadnutí, iii) úplná regenerace rostlin po opětovném zavlažení. Jednotlivé sledované parametry založené na zobrazovacích metodách ovšem ukázaly potenciál pro hodnocení citlivosti na sucho v různých termínech od počátku vysychání či regenerace. Korelace s relativní odezvou výnosu se postupně zvyšovala u projekční listové plochy hodnocené ze strany (SPA) a dosáhla maxima v bodě úplné regenerace po opětovném zvlažení. Aktuální kvantový výtěžek fotosystému II (ΦPSII) vykazoval nejvyšší korelaci s relativním výnosem zrna kolem bodu vadnutí. Naproti tomu relativní rozdíl teploty listů vůči teplotě okolního vzduchu (Tdiff) vykazoval vysokou korelaci s výnosovou odezvou na sucho dříve, a to již při dosažení 50% úrovně dostupné vody pro rostliny v půdě. Nejvyšší korelace s relativní výnosovou odezvou byly získány u barevné analýzy RGB v bodě vadnutí a po regeneraci, zejména u relativního podílu khaki, béžového, tmavě zeleného a olivově zeleného odstínu. Vícenásobná regrese s parametry poskytujícími Pearsonův korelační koeficient R > 0,5 mírně zlepšila odhad relativní odezvy výnosu na sucho, ale zajistila především významné zlepšení odhadu absolutního výnosu zrna při stresu suchem, přičemž přesnost odhadu se v obou případech pohybovala okolo 90 %. Tato metodika ukazuje, že použití kombinace fenotypovacích metod charakterizujících různé morfologické a fyziologické znaky umožňuje nejen hodnocení tolerance k suchu (na základě relativní výnosové reakce na sucho), které je klíčové pro výběr genetických zdrojů pro následný šlechtitelský proces, ale také umožňuje testovat výnosovou výkonnost nových genotypů při stresu suchem. Drought tolerance is a complex of traits that vary depending on the type, severity, and timing of drought. Therefore, a relatively comprehensive assessment of the morphological and physiological phenotypic response to drought is necessary. This methodology focuses on the development of procedures and evaluation of the complex phenotypic response of spring barley genotypes to drought using non-invasively measured parameters based on red-green-blue (RGB) imaging, thermal infrared imaging, and chlorophyll fluorescence imaging measured within an automated phenotyping platform. The development of the methodology was based on an experiment in which the dynamic changes in the response of six barley genotypes, representing a wide range of drought tolerance (from a very sensitive to a very tolerant genotype), to continuous drying until the point of wilting and subsequent re-watering were monitored. Three critical time points during drought and re-watering were identified, key for detecting drought tolerance: i) reaching 50% of available soil water, ii) reaching wilting point, iii) full plant recovery after re-watering. However, the different imaging-based parameters monitored showed potential for assessing drought sensitivity at different time points from the onset of drying or recovery. The correlation with relative yield response increased progressively for the side projected leaf area (SPA) and reached a maximum at the point of complete recovery after re-watering. The actual quantum yield of photosystem II (ΦPSII) showed the highest correlation with relative grain yield around the wilting point. In contrast, the relative difference of leaf temperature to ambient air temperature (Tdiff) showed a high correlation with yield response to drought earlier, as early as at the point of reaching 50% of the level of soil water available to plants. The highest correlations with relative yield response were obtained for RGB colour analysis at the wilting point and after recovery, especially for the relative proportion of khaki, beige, dark green, and olive-green hues. Multiple regression with parameters providing a Pearson correlation coefficient R > 0.5 slightly improved the estimation of the relative yield response to drought, but mainly provided a significant improvement in the estimation of absolute grain yield under drought stress, with an estimation accuracy of around 90% in both cases. This methodology shows that the use of a combination of phenotyping methods in characterising different morphological and physiological traits not only allows the assessment of drought tolerance (based on relative yield response to drought), which is crucial for the selection of genetic resources for subsequent breeding, but also allows the testing of the yield performance of new genotypes under drought stress.
Keywords:
spring barley; drought; drought tolerance; phenotyping; rgb imaging; chlorophyll fluorescence imaging; thermal infrared imaging; yield
Available at various institutes of the ASCR
Fenotypování jarního ječmene na odolnost vůči suchu
Odolnost rostlin/plodin vůči suchu představuje komplex vlastností, které se různě uplatňují v závislosti na typu, závažnosti a načasování sucha. Proto je nutné poměrně komplexní hodnocení morfologické ...
Application of In situ TR Spectroelectrochemical Techniques in Determination of Redox Mechanism of Bioactive Compounds
Sokolová, Romana; Jiroušková, Eliška; Degano, I.; Wantulok, J.; Nycz, J.
2023 - English
The electron transfer reactions play an important role in many natural processes. Reactions such as \ndissociation, protonation, and reactions with water and other small molecules often occur in \nbiotransformation. The reaction schemes involving these chemical reactions coupled to the \nelectron transfer can be determined by cyclic voltammetry. Additionally, in \nsitu spectroelectrochemistry can efficiently contribute to the determination of oxidation or \nreduction mechanism. This technique provides information about the electroactive chromophore during \nthe redox process allowing to identification the first reaction intermediates. The final reaction \nproducts were identified by chromatographic techniques. This study represents a key role of TR \nspectroelectrochemistry in the determination of reaction intermediates in the case of \n1,10- phenanthroline derivative substituted by bioactive phenothiazine unit and \ndrug 3- fluorophenmetrazine (2-(3-fluorophenyl)-3-methylmorpholine, 3-FPM). Co pound 3-FPM\nhave recently appeared as the new psychoactive substance in the drug market.\n
Keywords:
IR spectroelectrochemistry; psychoactive substances; oxidation mechanism
Available on request at various institutes of the ASCR
Application of In situ TR Spectroelectrochemical Techniques in Determination of Redox Mechanism of Bioactive Compounds
The electron transfer reactions play an important role in many natural processes. Reactions such as \ndissociation, protonation, and reactions with water and other small molecules often occur in ...
A polarizable reference electrode
Mareček, Vladimír
2023 - English
New concept of a reference electrode for electrochemical systems resolves a problem of a poor \npotential stability of refence electrodes based on the distribution of a strongly \nhydrophobic common cation between two immiscible electrolyte solutions (TTTES). The use of a \npolarizable metal electrode instead of a classical reference electrode is demonstrated in \n a modified conventional four-electrode cell with TTTES. A simple battery operated potentiostat \ncontrols the working electrode potential in a three-electrode configuration. The working metal \nelectrode then serves as a polarizable reference organic solvent electrode in a four-electrode \nsystem for the polarization of the water/organic solvent interface.\n\n
Keywords:
reference electrode; liquid/liquid interface; chloride extraction
Available on request at various institutes of the ASCR
A polarizable reference electrode
New concept of a reference electrode for electrochemical systems resolves a problem of a poor \npotential stability of refence electrodes based on the distribution of a strongly ...
Elektrochemické studium pH závislých redoxních vlastností komplexů mědi s aza-makrocyklickými ligandy
Koláčná, Lucie; Maďar, M.; Kubíček, V.; Ludvík, Jiří
2023 - Czech
Molekulární elektronika je progresivní směr moderní materiálové chemie. Zabývá se vývojem\nelektronických prvků na úrovni jedné molekuly. Nejdůmyslnější molekulární elektroniku\nnajdeme v přírodě v podobě metaloenzymů. Jedním ze směrů výzkumu jejich modelů jsou\nkomplexy různě substituovaných azamakrocyklů. Předností těchto molekul je jejich stabilita a\ndobře definovaná syntéza. Investigated Cu(II) complexes are based on plain or cross-bridged cyclam. The\nelectrochemically inactive cyclam was modified by carboxylate, phosphonate, or phenolate\npendant arms. Cu(II) represents the main redox center of the complexes. Modification of the\nligand causes a changed pattern of complex redox response in buffered aqueous solution.\nIrreversible Cu(II) reduction results in complex decomposition to amalgamated copper and\nligand in excess. After Cu(0) electrochemical in situ re-oxidation, copper and ligand are recomplexed.\nComplexes undergo isomerization, accelerated by increasing the temperature. The\ninfluence of pH on complex isomerization and the reversibility of its reduction was described.
Keywords:
cyclam; Cu(II) complexes; pendant arms
Available on request at various institutes of the ASCR
Elektrochemické studium pH závislých redoxních vlastností komplexů mědi s aza-makrocyklickými ligandy
Molekulární elektronika je progresivní směr moderní materiálové chemie. Zabývá se vývojem\nelektronických prvků na úrovni jedné molekuly. Nejdůmyslnější molekulární elektroniku\nnajdeme v přírodě v ...
Determination of Selected Natural Psychoactive Substances in Organic Matrices at 3D Printed Electrodes
Choińska-Mlynarczyk, Marta; Šestáková, Ivana; Navrátil, Tomáš
2023 - English
Psilocybin and its derivative psilocin are popular psychoactive substances both as experimental\ntreatments in clinical trials and as illicit drugs. Their potential ability to influence the human\nbrain entails the need for a fast, inexpensive, selective, and sensitive method of their\ndetermination. The aim of our study was the development of new 3D-printed electrodes which\nfulfill these demands and are useful for medical, toxicological, and forensic purposes.\nSuccessful development allows determining in real matrices (human plasma and dried\nmushrooms) concentrations of the order of 1 μmol dm-3.\n
Keywords:
natural psychoactive substances; 3D-printed electrodes; psilocin; psilocybin
Available on request at various institutes of the ASCR
Determination of Selected Natural Psychoactive Substances in Organic Matrices at 3D Printed Electrodes
Psilocybin and its derivative psilocin are popular psychoactive substances both as experimental\ntreatments in clinical trials and as illicit drugs. Their potential ability to influence the ...
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