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Pozzolanic Activity of Silicon Dioxide
Barek, Jaroslav ; Žižková, Nikol (referee) ; Rovnaníková, Pavla (advisor)
The aim of this bachelor's thesis is to investigate and identify the present status of resources with dominant amorphous silicon dioxide content and summarize feasible test methods to assess pozzolanic activity. The use of pozzolan as a partial replacement of Portland cement reduces the carbon dioxide emitted per tonne of product and can also improve various physical properties of the resulting cementitious composites. Assessment of the pozzolanic activity of cement replacement materials is increasingly important because of the economic sustainability of cementing materials. The pozzolanic activity of wheat straw ash, silica fume, nanosilica, two diatomites, glass powder and expanded perlite have been investigated and compared using the strength activity index test, the modified Chapelle test and the pozzolanicity test in accordance with the European Standard EN 196-5. From an experimental investigation of seven different pozzolans, the following main conclusions can be drawn. In the case of an acid-base titration (determination of [OH–], the procedure specified in EN 196-5) is better to use Tashiro (mixed indicator) instead of required methyl orange, Tashiro changes color at the endpoint of a titration distinctly. Strength activity index: the procedure used was based on EN 450-1. In its current form, this procedure is misleading because of two other significant properties of the pozzolan, namely its density and its water-reducing/increasing capabilities. Based on the results of our experimental investigation, the current testing procedure is evaluated against an alternative in which the 25% pozzolan replacement for cement is performed on a volumetric basis and the volume fraction of water is held constant.
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Effect of colloidal silicon dioxide on selected properties of cement pastes and mortars
Barek, Jaroslav ; Žižková, Nikol (referee) ; Rovnaníková, Pavla (advisor)
The presented diploma thesis deals with the potential use of colloidal silica in cement composites. Investigation is focused primarily on selected properties of cement pastes and mortars with colloidal silica content. Two selected types of colloidal silica (particles with average size of 14 nm) have been used as a cement addition and partial replacement of cement, respectively. The experimental program for cement pastes with colloidal silica included tests for isothermal calorimetry (the study of cement hydration) and thermal analysis (determining the portlandite content). Hardened cement pastes have been studied through measurements of compressive strength. The microstructure was examined by scanning electron microscopy. Hardened mortars with colloidal silica have been studied through measurements of compressive strength, flexural strength, modulus of elasticity and fracture mechanics parameters. Fracture mechanics tests show that 5 % and 20 % addition of colloidal silica can enhance after 28 days of curing fracture energy up to 18,4 % and 32,7 %, respectively. For the compressive strength enhancing effect of colloidal silica, it was found to be more pronounced in the early age, while rate of strength gain can be lower than the control in the later ages. Our investigations revealed that the silica sol will coagulate immediately when the cement is mixed into the water containing sol. The ionic composition of pore fluid significantly influences the stability of colloidal silica and lead to their aggregation. After additional tests it has been found that small addition of calcium hydroxide greatly improved the compressive strength of the resulting cement pastes with colloidal silica content. Addition of calcium hydroxide in conjunction with modified cement paste preparation can enhance compressive strength after 3 days of curing up to 64,4 % in comparison with the blank paste.
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Electrochemical biosensors with spatially separated enzymatic and detection parts for selective analysis in flow-through arrangement
Tvorynska, Sofiia ; Barek, Jiří (advisor) ; Labuda, Ján (referee) ; Korecká, Lucie (referee)
This dissertation thesis presents the newly developed four highly reusable, stable as well as simple, and cost-effective electrochemical (bi)enzymatic biosensors for the selective and reliable determination of choline, acetylcholine, uric acid, and L-lactic acid in flow injection analysis. All biosensors are based on the concept of the spatial separation of the biorecognition part from detection one and amperometric monitoring of the enzymatically consumed oxygen via its four-electron reduction at the highly negative detection potential. In this way, the design of the biosensors includes an easily replaceable enzymatic mini-reactor(s) connected upstream to the flow cell that contains the appropriate silver amalgam-based transducer. The enzymatic mini-reactor based on choline oxidase, uricase, or lactate oxidase was used for choline, uric acid, or L-lactic acid biosensors, respectively. The acetylcholine bienzymatic biosensor includes the consequently connected choline oxidase- and acetylcholinesterase-based mini-reactors. The first part of this thesis focuses on the construction of two different silver amalgam-based electrodes. Specifically, this section discusses the fabrication of a silver solid amalgam electrode covered by mercury film operating in a wall-jet cell and also highlights the...
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An Enzymatic Biosensor with Amperometric Detection in a Flow Injection Analysis for the Determination of L-lactic Acid: Development and Application
Tvorynska, Sofiia ; Barek, J. ; Josypčuk, Bohdan
An amperometric biosensor consisting of an enzymatic mini-reactor (lactate oxidase covalently\nattached to −NH2 functionalized mesoporous silica powder SBA−15 using glutaraldehyde) and\na silver amalgam-based screen-printed electrode acting as a transducer was developed for the\ndetermination of L-lactic acid (LA) in FIA. The detection potential of −0.9 V vs. Ag pseudoreference\nelectrode was applied for cathodic detection of enzymatically consumed oxygen.\nUnder the optimized conditions, the constructed biosensor enabled selective determination of\nLA with a micromolar limit of detection. Importantly, the proposed biosensor represented\nexcellent operational stability after ≥350 measurements. Finally, it was successfully applied to\nreal sample analysis.
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Continuous monitoring of anthraquinone-based anticancer drugs by amperometric technique
Skalová, Štěpánka ; Fischer, J. ; Barek, J. ; Navrátil, Tomáš ; Krejčí, J. ; Kučerová, R. ; Vyskočil, V.
This contribution is focused on the development of electroanalytical methods for the monitoring of anthraquinone-based anticancer drugs in physiological solution by combination of liquid-flow system and dialysis catheter, possibly inserted into blood circulation of patients. For this purpose, amperometric detection with dual glassy carbon electrode was developed and derivate of these drugs, anthraquinone-2-sulphonate, was used as a model compound. Two different flow rates of carrier solution (physiological solution) were tested (specifically, 1 and 5 mu L min(-1)) and the dependence of peak currents of anthraquinone-2-sulphonate on its concentration was verified
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A comparative study of covalent glucose oxidase and laccase immobilization techniques at powdered supports for biosensors fabrication
Tvorynska, Sofiia ; Barek, J. ; Josypčuk, Bohdan ; Nesměrák, K.
In order to develop the optimal strategy and to deepen the knowledge in the field of enzyme immobilization, three different techniques of covalent binding for two enzymes (glucose oxidase and laccase) at powdered surfaces were compared. Immobilization protocol was optimized by changing supports (two mesoporous silica powders (SBA−15, MCM−41) and a cellulose powder), the functionalized\ngroups introduced at support surfaces (−NH and −COOH), and the methods of activation (glutaraldehyde and carbodiimide). Amino and carboxyl functionalized mesoporous silica and cellulose powders\nwere prepared by silanization using (3-aminopropyl)triethoxysilane and carboxyethylsilanetriol, respectively. It was found that coupling of both enzymes by their –NH groups through glutaraldehyde to -NH functionalized supports, in particular SBA15−NH and cellulose−NH for glucose oxidase, MCM41−NH for laccase, showed the highest activity and the best stability.
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Development of electrochemical methods for study of antibacterial compounds in small volumes
Gajdár, Július ; Barek, Jiří (advisor) ; Šiškanova, Tatiana (referee) ; Labuda, Ján (referee)
Main goal of this Ph.D. thesis is to develop voltammetric methods for the electrochemical study of novel antimycobacterial compounds hydroxynaphthalene- carboxamides. Firstly, this study was focused on the miniaturization of voltammetric methods and construction of an electrochemical microcell due to usually small volume of samples that are associated with an analysis of biologically active compounds in biological matrices. Therefore, all aspects of the voltammetric procedure were studied in a relation to miniaturization. Microcells were based on commercially available electrodes: glassy carbon electrode as a reliable electrode material with well-described characteristics and a novel silver solid amalgam electrode. This study was carried out with analytes 4-nitrophenol, pesticide difenzoquat, and 1-hydroxy-N-(4-nitrophenyl)naphthalene-2-carboxamide. Attention was paid especially to the optimization of oxygen removal procedures in the drop of a solution. Developed miniaturized methods had the same parameters for the determination of studied compounds as in bigger volumes. The proposed electrochemical microcell can be generally used for voltammetric analysis of those samples of biological or environmental origin that are usually available in very limited volumes. Second part of the thesis was focused...
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Determination of heavy metal poisoning antidote 2,3-dimercapto-1-propanesulfonic acid using silver solid amalgam electrode
Choińska-Mlynarczyk, Marta ; Hrdlička, Vojtěch ; Redondo, B. R. ; Barek, J. ; Navrátil, Tomáš
2,3-Dimercapto-1-propane-sulfonic acid (DMPS) was investigated using direct current voltammetry (DCV), differential pulse cathodic stripping voltammetry (DPCSV), differential pulse anodic stripping voltammetry (DPASV), and elimination voltammetry with linear scan (EVLS) at a polished (p-AgSAE)and at a meniscus modified silver solid amalgam electrode (m-AgSAE). EVLS confirmed two consecutive reductions with coupled proton/electron transfer. Voltammetric titrations of DMPS with Pb2+ proved complex formation, with limits of quantification (LOQs) and detection (LODs) 0.3 and 0.1 mu mol L-1 at m-AgSAE and 0.8 and 0.3 mu mol L-1 at p-AgSAE, respectively. Determination of DMPS in commercial drug Dimaval and human urine samples confirmed practical applicability of the developed method.
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Comparison of the Covalent Laccase Immobilization at Amino- and Carboxylfunctionalized Mesoporous Silica, Glassy Carbon, and Graphite Powders using Different Coupling Agents for Optimal Biosensor Preparation
Tvorynska, Sofiia ; Barek, J. ; Josypčuk, Bohdan
In order to find the most suitable immobilization protocol, a comparison of three strategies\nbased on the application of –NH2 and –COOH functionalized supports with the different\nactivation agents (glutaraldehyde and carbodiimide) have been conducted for the covalent\nenzyme (laccase) attachment. Two kinds of the supports, namely mesoporous silica (SBA−15,\nMCM−41) and carbonaceous (glassy carbon, graphite) powders, have been used. It was found\nthat a biosensor consisted of tubular detector of silver solid amalgam as a working electrode\nand the enzymatic mini-reactor with laccase covalently attached to glutaraldehyde activated\n–NH2 functionalized MCM−41 shows the best results regarding sensitivity and stability for\ndopamine detection.
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Construction and application of the amperometric uric acid biosensors based on the covalent immobilization of uricase by different strategies
Tvorynska, Sofiia ; Barek, J. ; Josypčuk, Bohdan
In this work, a promising combination of a biosensor based on the\nenzymatic mini-reactor with the detection principle of four-electron\nreduction of the consumed oxygen at highly negative potential has\nbeen developed for uric acid determination using flow injection\nanalysis. The construction of the biosensor provides a spatial\nsegregation of the biorecognition (uricase-based mini-reactor) and\ndetection (tubular detector of silver solid amalgam (TD-p-AgSA))\nparts. To find out the most appropriate enzyme immobilization\nprotocol, three different strategies of the covalent attachment for\nuricase from Bacillus fastidiosus have been compared. It was found\nthat the biosensor with the mini-reactor based on the covalent\nattachment of uricase via glutaraldehyde to -NH2 functionalized\nmesoporous silica powder MCM-41 showed extremely high stability\n(>1 year) and reusability (at least 600 measurements) The biosensor's\npractical applicability was confirmed by successful determination\nof uric acid in human urine.
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