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Contributions to Volatile Compound Generation of Arsenic, Silver and Gold by Tetrahydroborate Reaction for Atomic Absorption Spectrometry
Musil, Stanislav ; Rychlovský, Petr (advisor) ; Kanický, Viktor (referee) ; Spěváčková, Věra (referee)
(EN) The presented dissertation thesis summarizes the results contained in five original research papers that were published in prestigious international scientific journals in the field of analytical chemistry and atomic spectrometry. It is devoted to the method of generation of volatile compounds using a tetrahydroborate reaction and detection in a quartz multiatomizer by atomic absorption spectrometry. The thesis can be divided into two thematic parts - speciation analysis of arsenic based on hydride generation technique with collection and separation in a cryogenic trap and generation of volatile species of transition metals. In the first thematic part pre-reduction of pentavalent inorganic and methylated arsenicals has been studied. A simple setup for on-line pre-reduction employing thioglycolic acid as a fast pre-reductant has been developed, connected with a current hydride generator and applied/verified to oxidation state specific arsenic speciation analysis of human urine samples. In the same method the possibility of drying the gaseous phase from water vapor has been investigated to avoid incidental blocking the cryogenic trap by frozen water and to decrease fluctuations of signal baseline. Pronounced losses of methylated species have been discovered on Nafion tube dryer currently used in...
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Speciation analysis of arsenic based on volatile species generation and dielectric barrier discharge plasma atomization
Plecháč, Matěj ; Kratzer, Jan (advisor) ; Kaňa, Antonín (referee)
SPECIATION ANALYSIS OF ARSENIC BASED ON VOLATILE SPECIES GENERATION AND DIELECTRIC BARRIER DISCHARGE PLASMA ATOMIZATION Bc. Matěj Plecháč 2024 Abstract Volatile species generation (VSG) comprises a group of techniques based on analyte derivatization in order to form a volatile compound prior to spectrometric detection. Selective analyte conversion from liquid to gas phase results in enhanced analyte introduction efficiency, but also in matrix separation and reduced risk of interferences. Moreover, VSG step can be utilized during speciation analysis or analyte preconcentration. The most frequent atomizers of volatile species are externally heated quartz tubes (QTA). Dielectric barrier discharge (DBD) atomizers have proved to be alternative hydride atomizers to QTA. The significant difference in toxicity of various species of the same element leads to the urgent need to develop new strategies for speciation analysis. Various approaches to speciation analysis of toxicologically relevant arsenic species including inorganic iAsIII and iAsV , monomethylarsonic acid (MMA), dimethylarsinic acid (DMA) and trimethylarsine oxide (TMAsO) by hydride generation atomic absorption spectrometry (HG-AAS) were investigated in this work. All these species can be converted to volatile compounds. i.e. arsane and its methylated...
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Arsenic and arsenic species cycle in environment
Ševčíková, Kateřina ; Sommer, Lumír (referee) ; Dočekalová, Hana (advisor)
This bachelor thesis, based mostly on literature retrieval, deals with monitoring of individual arsenic compounds in the environment and is also reviewing methods used for their analysis. The experimental part is focused on determination of various arsenic in the Oncorhynchus mykiss tissue by HPLC-UV-HG-AFS. Obtained results showed that the arsenic was present in the tissue of the Oncorhynchus mykiss in form of arsenobetaine, which is common for fishes and other aquatic animals and is not toxic even for consuments.
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The issue of alkylderivatives of mercury in biotic matrices
Zajícová, Markéta ; Doležalová Weissmannová, Helena (referee) ; Vávrová, Milada (advisor)
Alkyl derivatives of mercury, especially methylmercury, bring a significant risk to the environment and the human population. Methylmercury is highly toxic compound, which have the potential to bioaccumulate and biomagnify in tissues of aquatic organisms. This diploma thesis deals with issues of alkyl derivatives of mercury in biotic matrices. The goal of this thesis was to analyze fish tissues. Fish were caught from the river Svratka at the inflow and at the outflow of wastewater treatment plant. Methylmercury was determined in fish muscles and skin. Total mercury was determined in fish muscles. The extraction based on acidic digestion in hydrochloric acid and subsequent extraction with toluene was used for isolation of methylmercury from fish tissues. There was used gas chromatography with electron capture microdetector for determination of methylmercury. Total mercury was determined by special analyzer AMA 254.
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Modification of Diffusive Gradient in Thin Films Technique for Characterization of Environmental Systems
Gregušová, Michaela ; Sommer, Lumír (referee) ; Janoš, Pavel (referee) ; Dočekal, Bohumil (advisor)
Diffusive gradient in thin film technique (DGT) represents a relatively new approach for in situ determinations of labile metal-species in aquatic systems. The DGT device passively accumulates labile species from the solution while deployed in situ, and therefore contamination problems associated with conventional collection and filtration procedures are eliminated. This study deals with a possible modification of DGT technique. The key of using DGT technique for speciation analysis of metals is to find out suitable binding phase and diffusion layer. The new resin gel based on Spheron Oxin (5 sulphophenyl-azo-8-hydroxyquinoline) ion exchanger with a higher selectivity to trace metals than Chelex 100 could potentially provide more information on metals speciation in aquatic systems. The performance of this new binding phase was tested for the determination of Cd, Cu, Ni, Pb and U under laboratory conditions. The hydrogel layer based on poly(2-hydroxyethyl methacrylate) was synthesized and tested as a new diffusion gel for application in DGT technique.
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Speciation analysis of selenium in selenized yeast
Motlová, Tereza ; Vitoulová, Eva (referee) ; Diviš, Pavel (advisor)
The aim of the theses was determination of selenium species in yeast Saccharomyces cerevisiae cultivated in medium with added inorganic form of selenium (Sodium Selenite). Concentrations of Sodium Selenite in cultivation medium were 0,1; 1; 10 and 100 mg.l-1. Cultivation was undertaken in fermenting tub for period of 72 hours. Cultivated yeasts were extracted by use of enzymes and subsequently the species of selenium in particular parts of yeasts were determined. In order to determine selenium species, the method of high-performance liquid chromatography in combination with atomic fluorescent spectrometer and technique of hydride generation was used. Having analysed different fractions of the yeasts Saccharomyces cerevisiae it was ascertained that during cultivation the sorption of selenium occurred in form of Se4+ in cell membranes while in cytoplasm no inorganic forms of selenium were found. Furthermore, it was stated that yeasts Saccharomyces cerevisiae are able to metabolically change inorganic forms of selenium to organic forms (selenomethionine), while these forms are present in cytoplasm and they are likely to be bound to proteinic structures of cell membranes. An increase of concentration of Se4+ in cell membranes could be observed as a result of increasing concentration of Sodium Selenite in cultivation medium. In proteinic structures the concentration of organic selenium forms increased only to concentration 10 mg.l-1 of Sodium Selenite in cultivation medium.
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Speciation analysis employing hydride generation
Matoušek, Tomáš
The lecture presented employing of different ways of hydride generation- selective generation, postcolumn generation and cryotrapping- useful of element speciation analysis. Examples from our laboratory covered applications from the field of clinical, food and natural water analysis.
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UV-photochemical generation of volatile species of tellurium and other transition metals
Jeníková, Eva
This dissertation thesis is focused on UV-photochemical generation of volatile species of tellurium, ruthenium, rhenium and iridium coupled to methods of atomic spectrometry. In the first part, attention was paid to the optimization of parameters of UV-photochemical generation of volatile tellurium species and its application for speciation analysis of Te(IV) and Te(VI) in water samples. UV-photochemical generation was carried out in a UV-photoreactor, which consisted of a low-pressure mercury lamp wrapped with a polytetrafluoroethylene reaction coil that served as a reactor. Atomic absorption spectrometry with a continuum source of radiation and high resolution and atomization in a miniature diffusion flame were used to optimize the conditions of generation, which included the composition of the reaction medium, irradiation time and the addition of transition metals as modifiers. In order to achieve a higher sensitivity of determination, the generator was coupled to a triple quadrupole inductively coupled plasma mass spectrometer. Since efficient UV-photochemical generation of volatile species was achieved only from Te(IV), with no response from Te(VI), the feasibility of this technique for simple "non-chromatographic" speciation analysis was tested and a method for determination of Te(IV) and...
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UV-photochemical generation of volatile species of tellurium and other transition metals
Jeníková, Eva ; Hraníček, Jakub (advisor) ; Šíma, Jan (referee) ; Kanický, Viktor (referee)
This dissertation thesis is focused on UV-photochemical generation of volatile species of tellurium, ruthenium, rhenium and iridium coupled to methods of atomic spectrometry. In the first part, attention was paid to the optimization of parameters of UV-photochemical generation of volatile tellurium species and its application for speciation analysis of Te(IV) and Te(VI) in water samples. UV-photochemical generation was carried out in a UV-photoreactor, which consisted of a low-pressure mercury lamp wrapped with a polytetrafluoroethylene reaction coil that served as a reactor. Atomic absorption spectrometry with a continuum source of radiation and high resolution and atomization in a miniature diffusion flame were used to optimize the conditions of generation, which included the composition of the reaction medium, irradiation time and the addition of transition metals as modifiers. In order to achieve a higher sensitivity of determination, the generator was coupled to a triple quadrupole inductively coupled plasma mass spectrometer. Since efficient UV-photochemical generation of volatile species was achieved only from Te(IV), with no response from Te(VI), the feasibility of this technique for simple "non-chromatographic" speciation analysis was tested and a method for determination of Te(IV) and...
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