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Interferences in determination of antimony by electrochemical generation of volatile compounds and atomic fluorescence spectrometry
Kostúrová, Dominika ; Červený, Václav (advisor) ; Nováková, Eliška (referee)
Antimony is a highly toxic element that enters the environment through natural processes and human activities as well. It is necessary to determine its ultra-trace amounts in various materials such as water, soil and biological samples. Due to the heterogeneity of sample matrices, the determination of antimony is problematic because of frequent interactions. The aim of this work was to investigate the effects of various interferents on the determination of antimony by electrochemical generation of volatile compounds and atomic fluorescence spectrometry. In total, 18 interference dependencies were measured in the determination of Sb(III) and Sb(V). The following ions were selected for the interference study: SO4 2- , Cl- , NO3 - , NO2 - , Fe3+ , Fe2+ , As3+ , Se4+ and Bi3+ . The As3+ ion had the most interesting course of all the interferents and could be used as a suitable additive to increase the sensitivity of antimony determination.
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Interferences in determination of antimony by UV-photochemical generation of volatile compounds and atomic fluorescence spectrometry
Kračmarová, Aneta ; Červený, Václav (advisor) ; Hraníček, Jakub (referee)
This work is focused on the study of interferents of selected elements during UV-photochemical generation of volatile antimony compounds. The interferents included transition metals, halides, hydride-forming elements and salts of mineral acids. Detection was performed by atomic fluorescence spectrometry. Some of the tested added substances proved to be potential reaction modifiers; in their presence, an increase in responses was observed. The best results were obtained using Fe3+ for the determination of Sb3+ and SO4 2- had the best results for the determination of Sb5+ . The largest interferent, i.e. the substance causing the most significant decrease in signal, was for both antimony ions Se4+ .
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UV-photochemical generation of volatile compounds of selenium and tellurium
Nováková, Eliška
The presented thesis deals with UV-photochemical generation of volatile compounds of Se and Te from various species. The aim of the project was to expand the current state of knowledge by the application of photocatalytic reduction of higher oxidation states of Se and Te for the speciation analysis based on UV-photochemical generation of volatile compounds. The first step of the study was the assembly of the apparatus for the photocatalysed UV-photochemical generation of volatile compounds. The material of reactor and the whole experimental set-up were based on literature survey and previous research done in our research group. Experiments were directed towards finding the optimum conditions for generation of volatile compounds of selected model elements Se and Te. Se was studied as the element most commonly determined by the UV-photochemical generation of volatile compounds. Conversely, Te was selected as a model analyte representing elements forming less stable volatile compounds. The second part was the application of the optimised method of photocatalysed UV- photochemical generation of volatile Se compound to the determination of Se in water matrices, liquid certified reference materials and also samples of dietary supplements. TiO2/UV-photochemical generation was also successfully modified to...
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Study of properties of UV-photochemical generation of volatile compounds od antimony
Adámková, Dominika ; Červený, Václav (advisor) ; Hraníček, Jakub (referee)
The master thesis deals with comparison of atomic fluorescence spektrometry and high resolution continuum source atomic absorption spektrometry for three methods generation of volatile compounds Antimony. In both methods of atomic antimony detection, it compares the most common chemical generation of volatile compounds (hydrides) with two alternative methods - electrochemical and UV - photochemical. The values of performance parameters for the determination of Sb(III) and Sb(V) were determined for all the above combinations. In the case of chemical generation, a surprisingly almost four times higher limit of detection of Sb(III) was found in connection with AFS detection than AAS detection. The final part was devoted to UV - photochemical vapor generation, with AAS detection for Sb(III) reaching limit of detection 4,96 ppb, for Sb(V) 8,63 ppb. Although UV - photochemical generation of volatile antimony compounds did not reach such performance parameters as chemical or electrochemical generation, it was observed that the sensitivity of antimony determination increased greatly when introducing oxygen into the apparatus. The interference study also found a significant positive effect of Fe(II) on the generation efficiency, and this modification partially persisted without further introduction of these...
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Hydride generation of bismuth for atomic absorption and fluorescence spectrometry.
Kolrosová, Marta ; Musil, Stanislav (advisor) ; Nováková, Eliška (referee)
This master's thesis deals with the optimization of conditions of chemical hydride generation (HG) of bismuth, its atomization and detection by atomic absorption spectrometry (AAS) and atomic fluorescence spectrometry (AFS). Two types of atomizers were used for atomization of volatile species, a miniature diffusion flame for AAS as well as for AFS and a flame-in-gas-shield atomizer for AFS. At first, the parameters of HG in a flow injection mode were optimized - the concentration of hydrochloric acid, the concentration of sodium borohydride and the volume of the reaction coil. Subsequently, the atomization conditions were optimized using both atomizers. The parameters optimized were hydrogen fraction, total gas flow rate and observation height. Due to the more complicated construction of the FIGS atomizer, more parameters were studied, such as the oxygen flow rate through the capillary and the flow rate of shielding argon required for shielding the free atoms. A special part of the thesis dealt with the optimization of the optical path of the atomic fluorescence spectrometer, the selection of an interference filter and the optimization of a power supply of an electrodeless discharge lamp. It was found that under optimum conditions of generation, atomization and detection excellent detection limits...
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UV-photochemical generation of cadmium volatile compounds with atomic spectrometric detection
Horová, Kateřina ; Nováková, Eliška (advisor) ; Červený, Václav (referee)
The aim of this master's thesis has been to develop and optimize the method of UV- photochemical vapor generation of cadmium volatile compounds for atomic fluorescence spectrometry. Two configurations with different materials wrapped around the low-pressure mercury vapor lamp were tested. I experimentally determined optimal conditions for both systems; the optimalized parametres included selection of photochemical reagent and its concentration, flow rate of liquids and gases, and the lenghth of the reaction coil. After finding the optimal parametres I determined the figures of merit of the method. I found from the measured data that UV-photoreactor with the quartz capillary provided lower limits of detection and thus was more suitable for generation of cadmium volatile compounds. With this arrangement and using the ferrous sulphate heptahydrate as the chemical modifier I obtained limit of detection 2,0 µg·l-1 , limit of determination 7,0 µg·l-1 , linear dynamic rate LOD-50 µg·l-1 and repeatibility 0,35 %. I also carried out the interference study in my thesis and determined the generation effeciency of cadmium volatile compounds. The interference study shows the influence of mineral acids (HCl, H2SO4, HNO3), their salts (NaNO2, NaNO3) and transition metals (Co, Ni, Cu). Based on literature review I also...
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