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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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The Speciation Analysis of the Toxicological Important Forms of the Arsenic in Urban Particulate Matter Samples with the Detection QF-AAS
Jelínek, Petr ; Rychlovský, Petr (advisor) ; Červený, Václav (referee)
The topic of this diploma thesis was the speciation analysis of the toxicological important forms of the arsenic in urban particulate matter samples. The detection technique used in this work was atomic absorption spectrometry with quartz atomizer. Acetic acid, ammonium acetate, hydroxylamine, potassium hydroxide and sodium carbonate are recommended leaching agents for extraction of metals from urban particulate matter samples. Results of the presenting work are following: Acidic extraction reagents can be not recommended for the speciation analysis of the arsenic, because these reagents lower sensitivity of the determination of As3+ and As5+ too and destroy the quartz atomizer. Alkaline extraction reagents don't lower sensitivity of the determination of As3+ and these reagents don't destroy the atomizer, but lower sensitivity of the determination of As5+ was obtained. Recommended reagents aren't useful for extraction of the metals from urban particulate matter samples for the speciation analysis.
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Speciation analysis of chromium in particulate matter of urban dust
Rybínová, Marcela ; Hraníček, Jakub (referee) ; Rychlovský, Petr (advisor)
Anion-exchange chromatography with inductively coupled plasma - atomic emission spectrometry (ICP-AES) has been used for the speciation of chromium (Cr). Chromium speciation has attracted attention because of the different toxicity, Cr(III) is relatively non-toxic and Cr(VI) has been classified as a human carcinogen. The aim of the present study was to develop simple method for the speciation analysis of Cr (Cr(III) and Cr(VI)) in particulate matter of urban dust. A combination of 2% KOH + 3% Na2CO3 has been chosen as the optimal reagent for the extraction of chromium from particular matter. It was found that there was no conversion of Cr(VI) into Cr(III). The effect of separation parameters such as acidity of mobile phase was also studied. The detection limit for Cr(VI) was about 12 ng.ml-1 . Results for the determination of Cr(VI) were confirmed by the analysis of standard reference material (BCR CRM 545, Cr(VI) in welding dust loaded on a filter) with good agreement between certified (40,16 ± 0,60 μg.g-1 ) and found (37,83 ± 1,14 μg.g-1 ) values.
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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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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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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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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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