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Příspěvky ke generování těkavých sloučenin arsenu, stříbra a zlata pomocí reakce s tetrahydroboratem pro atomovou absorpční spektrometrii / Contributions to Volatile Compound Generation of Arsenic, Silver and Gold by Tetrahydroborate Reaction for Atomic Absorption SpectrometryMusil, Stanislav January 2011 (has links)
(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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UV-fotochemické generování těkavých sloučenin selenu pro potřeby ultrastopové analýzy metodou AAS / UV-photochemical generation of volatile selenium compounds for ultratrace analysis by AASRybínová, Marcela January 2016 (has links)
This thesis deals with the study of UV-photochemical generation of volatile compounds (UV-PVG) in connection with atomic absorption spectrometry (AAS). Selenium (Se(IV)) was selected as a model analyte and many experiments were carried out to expand the current sum of knowledge of the topic. The study was commenced by assembling the UV-PVG apparatus in the continuous flow mode. The detection method used was AAS with externally heated quartz furnace atomizer. The focus of the first step of the study was on the construction of the volatile compounds generator (UV-photoreactor) with emphasis on the material used; tubes made of teflon or quartz of different diameters were tested. The construction of the apparatus was followed by optimization of the reaction conditions (the type and concentration of the photochemical agent and other agents, which increase the analytical signal; the carrier gas and the auxiliary hydrogen gas flow rate; the sample flow rate). Eventually, the analytical figures of merit of the selenium determination using the proposed method were found. The results showed that teflon reaction tubes are a good competitor to those made of quartz. The accuracy of the method has been successfully verified by analysis of certified reference material and its applicability has been further tested...
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