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Electrochemical generation of tellurium and bismuth hydrides for AAS
Resslerová, Tina ; Hraníček, Jakub (advisor) ; Šíma, Jan (referee)
Tellurium and bismuth are non-biogenous elements, which can be accumulated in human body. The aim of this work is focused on the determination of these elements by the electrochemical hydride generation with non-membrane electrolytic cell with quartz tube - atomic absorption spectrometry. The first step of the work was to optimize parameters for the continuous setup measurements and to obtain its figures of merit. After this, the arrangement with most suitable conditions for determination of these elements was converted to the flow injection setup (FIA) and all experimental parameters were again optimized and its figures of merit were obtained. The conditions of hydride generation were studied for platinum, lead and silver cathodes with hydrochloric and sulphuric acids and their sodium salts as electrolytes. The optimizations of the FIA setup were performed on platinum cathode in hydrochloric acid for bismuth and on lead cathode in sulphuric acid for tellurium. The limit of detection achieved for the generation of tellurium hydride was 1.1 ppm with a linear range up to 20 ppm; for the bismuth hydride the limit of detection was 9.5 ppm and limit of linearity 50 ppm. Keywords Bismuth, tellurium, electrochemical hydride generation, atomic absorption spectroscopy, flow injection analysis
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Electrochemical generation of tellurium hydride for AAS
Resslerová, Tina ; Hraníček, Jakub (advisor) ; Červený, Václav (referee)
Tellurium is non-biological element which is not common in the earth. It can be accumulated in a body and cause many health problems. In this work, tellurium is determined by the electrochemical hydride generation technique coupled with atomic absorption spectrometry with quartz tube atomizer. In the first part of this work, various relevant parameters of tellurium hydride generation were optimized to achieve high sensitivity. Under the optimal working parameters, calibration dependences and other basic characteristics were measured. Finally, the influence of oxygen added on the different places of set up was carried out. Optimized parameters were flow rate of the carrier gas, generation current, flow rate and concentration of electrolytes. Optimizations were measured for two different catholytes: hydrochloric and sulfuric acid, with similar results. In addition the calibration was measured with orthophosporic acid. Further experiments with oxygen were performed for sulfuric acid as the catholyte. Influence of oxygen on the baseline and the process of determination were performed, for both continuous and limited time addition.
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Electrochemical generation of tellurium and bismuth hydrides for AAS
Resslerová, Tina ; Hraníček, Jakub (advisor) ; Šíma, Jan (referee)
Tellurium and bismuth are non-biogenous elements, which can be accumulated in human body. The aim of this work is focused on the determination of these elements by the electrochemical hydride generation with non-membrane electrolytic cell with quartz tube - atomic absorption spectrometry. The first step of the work was to optimize parameters for the continuous setup measurements and to obtain its figures of merit. After this, the arrangement with most suitable conditions for determination of these elements was converted to the flow injection setup (FIA) and all experimental parameters were again optimized and its figures of merit were obtained. The conditions of hydride generation were studied for platinum, lead and silver cathodes with hydrochloric and sulphuric acids and their sodium salts as electrolytes. The optimizations of the FIA setup were performed on platinum cathode in hydrochloric acid for bismuth and on lead cathode in sulphuric acid for tellurium. The limit of detection achieved for the generation of tellurium hydride was 1.1 ppm with a linear range up to 20 ppm; for the bismuth hydride the limit of detection was 9.5 ppm and limit of linearity 50 ppm. Keywords Bismuth, tellurium, electrochemical hydride generation, atomic absorption spectroscopy, flow injection analysis
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Electrochemical generation of tellurium hydride for AAS
Resslerová, Tina ; Hraníček, Jakub (advisor) ; Červený, Václav (referee)
Tellurium is non-biological element which is not common in the earth. It can be accumulated in a body and cause many health problems. In this work, tellurium is determined by the electrochemical hydride generation technique coupled with atomic absorption spectrometry with quartz tube atomizer. In the first part of this work, various relevant parameters of tellurium hydride generation were optimized to achieve high sensitivity. Under the optimal working parameters, calibration dependences and other basic characteristics were measured. Finally, the influence of oxygen added on the different places of set up was carried out. Optimized parameters were flow rate of the carrier gas, generation current, flow rate and concentration of electrolytes. Optimizations were measured for two different catholytes: hydrochloric and sulfuric acid, with similar results. In addition the calibration was measured with orthophosporic acid. Further experiments with oxygen were performed for sulfuric acid as the catholyte. Influence of oxygen on the baseline and the process of determination were performed, for both continuous and limited time addition.
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