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Generation of volatile zinc chelates from aqueous matrix
Kračmarová, Aneta ; Nováková, Eliška (advisor) ; Červený, Václav (referee)
The topic of this work was optimization of the conditions for the generation of volatile zinc chelates. The aim was to develop an alternative method for generating volatile Zn speciates to its reduction by sodium tetrahydridoborate. Detection was carried out by atomic absorption spectrometry. Optimization of the conditions of the chelation reaction itself included the selection of a suitable chelating agent and appropriate modifiers, pH adjustment, suitable reagent and carrier gas flow rates, and appropriate apparatus arrangement. The following method characteristics were obtained under optimal conditions: LOD 1.55 mg L-1 , LOQ 5.17 mg L-1 and sensitivity 0.245 s L mg-1 . The repeatability was 13,7 %. The addition of modifiers was then tested to increase the efficiency of generation of volatile zinc chelates. Potential modifiers included transition metals, organic solvents, heterocyclic organic compounds, compounds from the carbamate group and surfactants. The heterocyclic 1,10-phenanthroline and the carbamate NaPDC were included in the optimal conditions because without them it was not possible to distinguish the signal from noise. Acetonitrile proved to be the most effective modifier, increasing the efficiency to 1547 %. With the addition of acetonitrile, the LOD decreased to 0.191 mg L-1 , the...
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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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