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Analysis of selected elements in dendrological sample of spruce trunk
Pastrňáková, Aneta ; Hraníček, Jakub (advisor) ; Šíma, Jan (referee)
The aim of this bachelor thesis was to determine selected elements, specifically iron, manganese, sodium, potassium, calcium, magnesium, barium, copper, zinc, strontium and aluminium in the sample of a spruce wood, taken from a dry tree from an area of South Bohemia. As a suitable and sufficiently sensitive method an atomic absorption spectrometry with flame atomization was used in this bachelor thesis. Before the analysis optimal conditions for the determination of these elements were experimentally found. The beam height above the burner edge and the acetylene flow rate were optimized depending on the type of oxidant used. Under the optimal conditions, the basic characteristics of the determination of individual elements were determined. These characteristics include mainly the limit of detection and quantification, sensitivity and repeatability. Optimized methods for determination of the selected elements were further applied for the analysis of real spruce wood samples. These samples were prepared by decomposition of the wood in a microwave device in the presence of nitric acid. In order to suppress interference, the suitable reagents were added to the analyzed samples to determine the selected elements (sodium, potassium, magnesium, calcium, barium). In total, 22 samples of wood of different...
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Determination of selenium and manganese in cerebrospinal fluid by atomic absorption spectrometry
Jiráková, Lucie ; Kotaška, Karel (advisor) ; Klapková, Eva (referee)
The aim of this study was to confirm the use of electrothermal atomic absorption spectrometry for the determination of selenium and manganese in the cerebrospinal fluid and to investigate concentrations of selenium and manganese in selected group of patients. For selenium was determined the detection limit 2,9 μg/l, for manganese 0,26 μg/l. 73 patients were examined (31 women, 42 men) whose average age was 14,1 years. The patients were divided into two groups according to age (56 children, 17 adults) and into two subgroups according to diagnoses (oncological, neurological). The control group consists of 18 subjects (5 women, 13 men, average age 21,7 years) with non-oncological and non-neurological diagnoses. We found significantly increased selenium concentrations in cerebrospinal fluid in the control group, compared with the group with neurological diagnoses (median = 14,4 μg/l vs. 12,4 μg/l, p < 0.05). Elevated levels of manganese in cerebrospinal fluid was observed in a group of children with oncological diseases compared with control group (1,2 μg/l vs. 0,5 μg/l, p < 0.05). Determination of selenium and manganese in the cerebrospinal fluid may have diagnostic importance in selected groups of patients. Powered by TCPDF (www.tcpdf.org)
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Contribution to optimization of parameters of speciation analysis of As based on selective hydride generation in direct transfer mode and detection by atomic absorption spectrometry
Vyvadilová, Tereza ; Dědina, Jiří (advisor) ; Korunová, Vlasta (referee)
The presented thesis deals with optimization of parameters speciation analysis based on a selective hydride generation in a direct transfer mode of hydrides and on-line atomization in an atomic absorption spectrometer. In the first part of the thesis processes during generation were investigated. Important indicator of a reactions taking place in a generator is volume of hydrogen (created by decomposition of NaBH4) which is subsequently introduced to the atomizer. In this part of the thesis a new approach to determine a flow rate of hydrogen delivered to the atomizator was developed. An influence of relevant paremeters of the atomizers and atomic absorption spectrometers on basic analytical characteristics of arsenic determination based on hydride generation was performed in the second part. Three atomic absorption spectrometers were used and three sources of radiation were compared. The most important analytic characteristic was the limit of detection which is influenced by standard deviation of measurement values of blank samples and by sensitivity. The best values of the limit of detection were achieved with electrodeless discharge lamps. Key words: hydride generation, arsenic, speciation analysis, atomic absorption spectrometry
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Speciation Analysis of Selected Mercury Compounds Using HPLC, UV-Photochemical Cold Mercury Vapor Generation and its AAS Detection
Linhart, Ondřej ; Červený, Václav (advisor) ; Spěváčková, Věra (referee)
The mercury occurs in the environment in a variety of forms. Mercury compounds can be found in the soil, atmosphere, water and living organisms. Although some of the mercury substances are very toxic, they are often used in various sectors of industry, agriculture and medicine. Mercury compounds differ in their toxicity, so it is necessary to do speciation analysis. The aim of this diploma thesis was to develop and validate a new analytical method for the determination of mercury compounds in different samples. This method involves the combination of high performance liquid chromatography, UV-photochemical cold vapor mercury generation and atomic absorption spectrometry. Effective separation of mercury(II), methylmercury(I), ethylmercury(I) and phenylmercury(I) ions and subsequent comparable efficient of mercury cold vapor generation from all of forms was achieved using these techniques. The reached detection limits were 8 µg l-1 , 31 µg l-1 , 16 µg l-1 and 38 µg l-1 . At the end of experimental work, the proposed method of RP-HPLC-UV-CVG- QTAAS was used for the determination of mercury compounds in real samples (fish tissue and water samples: Labe, Vltava and tap water) and in certified reference materials (DORM-3 and DOLT-4). Several methods for extraction of mercury species from solid samples...
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Hydride generation of tellurium for atomic absorption spectrometry
Bufková, Kateřina ; Musil, Stanislav (advisor) ; Matoušek, Tomáš (referee)
This master's thesis deals with optimization of conditions of chemical hydride generation of tellurium and conditions of its atomization, specifically in three types of atomizers - in a diffusion flame (DF), in a heated multiple microflame quartz tube atomizer (MMQTA) and in a dielectric barrier discharge (DBD) atomizer. Tellurium hydride was generated in a flow injection arrangement and a high-resolution continuum source atomic absorption spectrometer was used for detection. As hydride generation can be only done from tetravalent species of tellurium, at first a simple procedure of pre-reduction of hexavalent species of tellurium by heating a standard in hydrochloric acid at 6 mol dm-3 was verified. Further, conditions of chemical generation were optimized with a goal to achieve as high generation efficiency as possible, namely, concentration of hydrochloric acid and sodium tetrahydroborate, volume of the reaction coil and a flow rate of carrier gas. Subsequently, conditions of atomization of tellurium hydride were examined with chosen optimal generation conditions. In the case of DF, it was an amount of hydrogen in the flame, a total flow rate of gases and observation height. In the case of MMQTA, temperature of the atomizer, a flow rate of carrier gas and a flow rate of air or oxygen needed for...
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Application of non-membrane electrolytic cell for electrochemical volatile species generation of transition metals
Kobrlová, Andrea ; Hraníček, Jakub (advisor) ; Šíma, Jan (referee)
This diploma thesis is focused on the study of electrochemical generation volatile species of gold and silver. Two non-membrane electrolytic cells were constructed for electrochemical generation volatile species. These cells differ in the volume of electrode chamber. An atomic absorption spectrometry with quartz tube atomizer was used in most experiments. The equipment was performed in flow continuous mode. Experiments confirmed, that it is possible to use an atomic absorption spectrometry with quartz tube atomizer for generate volatile species of gold and silver by using two non-membrane electrolytic cells. The main part of this thesis was to find optimal conditions for the electrochemical generation of volatile species of gold and silver. These optimized parameters were: the cathode material, the type of electrolyte, the flow rate of the carrier gas, the generation current and the electrolyte flow rate. The calibration curves for both analytes were measured for both non-membrane electrolytic cells and the basic characteristics of the measurement were observed. Detection limit for electrochemical generation of gold was 1,61mg dm 3 and repeatability 3,93 %, detection limit for electrochemical generation of silver was 0,20 mg dm 3 and repeatability 7,33 %. Thanks to the experiments with a...
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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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Optimization of chemical generation and subsequent atomization of volatile cadmium species for atomic absorption spectrometry
Sagapova, Linda ; Kratzer, Jan (advisor) ; Marschner, Karel (referee)
Generation and atomization of cadmium volatile compounds was optimized in this work in order to determine trace Cd concentration levels by volatile compound generation (VCG) with subsequent detection by atomic absorption spectrometry (AAS). Three designs of volatile compound generators have been tested including a conventional hydride generator in flow injection analysis (FIA) mode, a batch generator as well as a generator of volatile compounds of transition metals. The generation efficiency of Cd species was quantified as low as 4 % in the conventional hydride generator. Providing that dissolved oxygen was removed from the reaction solutions, the generation efficiency of Cd increased to 12 % in the same experimental arrangement. The highest Cd generation efficiency of 54 % was reached in the generator of volatile compounds of transition metals. In this set up a detection limit of 0.07 ng ml-1 Cd and a sensitivity of 3.2 s ng-1 Cd, respectively, were reached. Moreover, the structure of the volatile Cd species generated was identified as free atoms in all experimental arrangements of the generators investigated. Keywords atomic absorption spectrometry, cadmium, generation of volatile compounds, atomization of volatile compounds
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