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UV-photochemical generation of volatile selenium compounds for ultratrace analysis by AAS
Rybínová, Marcela
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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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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Electrochemical generation of tellurium volatile compounds with atomic absorption spectrometry
Labancová, Katarína ; Hraníček, Jakub (advisor) ; Jelínek, Ivan (referee)
EN The present diploma thesis deals with the electrochemical generation of volatile tellurium compounds in connection with atomic absorption spectrometry with the main goal to increase the response of the tellurium signals and thus expand the existing knowledge about this element. Tellurium is one of the heavier elements that forms less stable volatile compounds. The reason for choosing these elements was the fact that its concentration increases mainly in landfills where it is released into the environment, which can have an ecological impact and an impact on human health. In the first step, two types of electrochemical cells were constructed - a thin-film flow electrochemical cell with and without an ion exchange membrane and an apparatus with a flow injection arrangement. The choice of cell types, cathode and anode material and apparatus design was chosen based on a literature research. Attention was paid to the optimization of reaction conditions for electrochemical generation of volatile tellurium compounds, which significantly affect the efficiency of generation using a heated quartz tube atomizer. The optimized parameters were electrolyte concentration, carrier gas volume flow rate, electrolyte volume flow rate and generation current. In the second step, the effect of the temperature of the...
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Chemical vapor generation of cadmium for analytical atomic spectrometry
Sagapova, Linda ; Kodríková, Barbora ; Svoboda, Milan ; Musil, Stanislav ; Kratzer, Jan
Chemical vapor generation of cadmium volatile compounds was optimized, several reaction modifiers based on inorganic salts and complexes of CrIII+, CoII+, TiIII+, TiIV+ were tested. Their use resulted in 4-5 times enhancement in sensitivity, reflected also in corresponding increase of generation efficiency and better repeatability. Generation efficiency was determined from a comparison between sensitivities obtained with chemical vapor generation and conventional solution nebulization, both simultaneously coupled with inductively coupled plasma mass spectrometry. The identity of the generated cadmium compounds was identified.
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Determination of lead and cadmium in fruits and vegetables extracts by atomic absorption spectrometry
Záškodová, Terezie ; Hraníček, Jakub (advisor) ; Červený, Václav (referee)
The content of this thesis was to analyse fruit and vegetable extracts. In the samples, the concentration of lead and cadmium was determine by atomic absorption spectrometry. First, it was necessary to conduct an optimalization study to find the optimal conditions of the method and select the appropriate method of atomization of the sample. It was chosen between flame and electrothermal atomization. For optimization, the following parameters were studied for atomization in flame: beam height above the burner, fuel flow rate, horizontal burner position, spectral interval width and lamp supply current. An optimization study for electrothermal atomization included the effect of atomization a pyrolysis temperature on signal size. Standard lead and cadmium solutions were used to determine the detection limits of the instruments used. The limit of detection in flame atomization was for lead respectively cadmium 0,002 mg/l, resp. 0,003 mg/l. In electrothermal atomization the detection limit was for lead, resp. cadmium 0,026 μg/l, resp. 0,029 μg/l. The experimentally determined values were statistically processed and the lead and cadmium contents were compared with the lead and cadmium limit values that may be contained in a sample of fruit and vegetables according to Commission Regulation (EC) No...
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Determination of Te(IV) by photochemical generation of volatile compounds with atomic spectrometric detection
Ruxová, Helena ; Hraníček, Jakub (advisor) ; Šíma, Jan (referee)
This thesis deals with the development of a method suitable for determination Te(IV) by UV-photochemical generation of volatile compounds (UV-PVG) in liquid samples. Atomic absorption spectrometry (AAS) and atomic fluorescent spectrometry (AFS) were used as detection methods. The basis of the apparatus for UV-PVG was a mercury lamp wrapped by PTFE capillary. Firstly, the experimental parameters were optimized for both methods. The optimized parameters were the type, concentration, pH and flow rate of the reaction medium, the length of the PTFE reaction coil, carrier gas flow rate (argon), supportive gas flow rate (hydrogen) and atomization temperature. The figures of merit with both detection methods were determined and compared after the method was optimized. Detection limits achieved for these two detection methods were 6,0 µg dm-3 for AFS and 1,50 µg dm-3 for AAS. Performed interference study confirmed a significant effect of many cations of transition metals and hydride forming elements on tellurium determination. The influence of nitric acid in the sample was studied separately. The suitability of the method for tellurium determination was confirmed by using a spiked certified reference material.
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Chemical generation of volatile mercury species for speciation analysis - method optimization and analytical applications
Migašová, Michaela ; Petry-Podgórska, Inga (advisor) ; Spěváčková, Věra (referee)
Experimental conditions have been optimized for volatile species generation (VSG) of four mercury species and their subsequent atomization with detection by atomic absorption spectrometry (AAS). The species investigated were mercury (+II), methylmercury (+I), ethylmercury (+I) and phenylmercury (+I). Flow injection construction of volatile species generator and externally heated quartz tube atomizer were employed. The optimized parameters were the concentration of hydrochloric acid and sodium borohydride, the length of the reaction coil, carrier gas flow rate, atomization temperature and the amount of oxygen present in the atomizer. Furthermore, the effect of the drying tube on the signal of Hg species as well as the applicability of tin chloride as an alternative reductant instead of sodium borohydride were studied. Calibration curves were measured and the basic analytical figures of merit were determined, under optimum experimental conditions, for all four mercury species investigated. Limits of detection for Hg species ranged from 0.12 to 0.25 ng cm-3 , while sensitivity reached ca 0.10 s ng-1 at atomization temperature of 500 řC. Experiments focused on atomization temperature optimization have revealed that volatile compounds generated from organic Hg species decompose significantly. Speciation...
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Determination of manganese in food supplements by atomic absorption spectrometry
Melicharová, Zuzana ; Hraníček, Jakub (advisor) ; Šíma, Jan (referee)
EN The main content of this thesis was the determination of manganese in the form of manganese ions in food supplements by the atomic absorption spectrometry. It was necessary to find the optimum conditions for this method, to conduct interference studies, to find a suitable way of transferring samples into solution and to determin manganese to achieve this goal. Following parameters were examined in optimalization study: beam height above burner edge, burner horizontal position, acetylene flow rate, torch angle, and spectral interval width. Copper, iron, sodium and calcium ions were investigated as interferents as they were present at the highest concentration in selected food supplements. The conversion of solid samples into solution was carried out in water and nitric acid at a room temperature as well as elevated temperature. These food supplements were selected for analysis: Calibrum 50 Plus, Caltrate Plus, Center A to Iron, DAS Gesunde Plus A-Z Multispectrum, GS Extra Strong Multivitamin, Spectrum 50+ and Supradyn Energy Complex. The manganese assay was performed on a GBC 933 AA spectrophotometer. Standard solutions were measured to determine the detection limit and the limit of determination of the instrument. The detection limit was 0.001 mg/l and the limit of determination was 0.004 mg/l...
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Determination of rubidium in selected plant extracts by atomic absorption spectrometry
Šatrová, Lucie ; Hraníček, Jakub (advisor) ; Jelínek, Ivan (referee)
In this diploma thesis, rubidium in plant material samples was determined by atomic absoption spectrometry. Determination of plant material rubidium was performed on two different atomic absorption spectrometers (GBC 933 AA and ContrAA 700) for comparison. The selection of a proper method of atomization was essential, therefore optimizations for the flame atomizer and electrothermal atomizer were performed. On the GBC 933 AA, flame atomization was tested. The flow rate of the acetylene-air, vertical and horizontal flame profile, spectral interval width was optimized for the instrument. On the ContrAA 700, the conditions for flame atomization were optimized as well as for electrothermal atomization. The optimized parameters included the acetylene-air flow rate and the vertical flame profile again. For the electrothermal atomization, the temperature dependence of pyrolysis and the temperature dependence of atomization were optimized. Under experimentally determined optimal conditions, the determination of rubidium in fruit and vegetable juice samples was performed by the method of calibration curve. Rubidium usually accompanies toher alkali metals. In the absence of essential biogenic elements iportant for plant growth, rubidium is able to help out and take on the role of potassium.
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