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Comparison of selenium extraction efficiency from food supplements
Molnárová, Lucia ; Hraníček, Jakub (advisor) ; Červený, Václav (referee)
The aim of this bachelor thesis was comparison of selenium extraction efficiency from food supplements which contain various declared forms of selenium. The method of atomic absorption spectrometry with flame atomization was used to determine the efficiency of the extraction. The first step for the determination of selenium in four real samples was the experimental finding of optimal conditions for selenium determination by flame AAS technique. Optimized parameters included the flame composition, the fuel flow rate, the angle of burner rotation, the horizontal burner position and the spectral range. During the testing the flame composition, higher responses were measured by using air as an oxidant, and therefore acetylene-air flame was used to other optimize and measure real samples. After optimization of the conditions, the calibration dependence was determined and the basic characteristics of the measurements were calculated. The detection limit and determination repeatability, sensitivity and operating range were determined for selenium determination. The detection limit was 0.12 mg dm-3 . The real samples of the food supplement tablets were mechanically homogenized and transferred to aqueous solutions, which were subsequently analyzed by the optimal conditions. The highest extraction efficiency...
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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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Electrochemical generation of tellurium hydride for AAS
Resslerová, Tina ; Hraníček, Jakub (advisor) ; Červený, Václav (referee)
Tellurium is non-biological element which is not common in the earth. It can be accumulated in a body and cause many health problems. In this work, tellurium is determined by the electrochemical hydride generation technique coupled with atomic absorption spectrometry with quartz tube atomizer. In the first part of this work, various relevant parameters of tellurium hydride generation were optimized to achieve high sensitivity. Under the optimal working parameters, calibration dependences and other basic characteristics were measured. Finally, the influence of oxygen added on the different places of set up was carried out. Optimized parameters were flow rate of the carrier gas, generation current, flow rate and concentration of electrolytes. Optimizations were measured for two different catholytes: hydrochloric and sulfuric acid, with similar results. In addition the calibration was measured with orthophosporic acid. Further experiments with oxygen were performed for sulfuric acid as the catholyte. Influence of oxygen on the baseline and the process of determination were performed, for both continuous and limited time addition.
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Mercury Speciation in a Historical Medical Preparation
Landl, Richard ; Červený, Václav (advisor) ; Nesměrák, Karel (referee)
In this final work, extraction methods for the determination of the total mercury concentration and its speciation analysis in a sample of historical medicinal product are evaluated. The first half of the experimental part is devoted to the determination of total mercury concentration in a sample of the historical medicinal product Naso Merfen unguentum using different evaluation methods with different standards used. Extraction with a mixture of hydrochloric acid and nitric acid was used for this determination. In this sample mercury is in the form of sparingly soluble phenylmercuric borate. The concentration (5.4 ± 2.0) · 10−2 % phenylmercuric borate was determined by evaluating the individual procedures. The next step was the speciation analysis of the historical drug sample and other samples that were used as reference materials. Extractions with tetramethyl ammonium hydroxide were used for specific analysis. From the determination of the mercury concentration in the reference materials, the extraction yields for both extraction methods was evaluated. For the standards of mercuric sulphide and phenylmercuric borate, both methods of extraction and determination were unsuitable due to their very low solubility. For mercuric sulfide, the yield of extraction with tetramethyl ammonium hydroxide was...
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Determination of sodium and potassium in honey samples by atomic absorption spectrometry
Venclová, Veronika ; Hraníček, Jakub (advisor) ; Šíma, Jan (referee)
This bachelor thesis was focused on the determination of sodium and potassium in honey samples by atomic absorption spectrometry with a flame atomization technique. An acetylene-air flame was used. Prior to the analysis of the honey samples, the optimal working parameters of the used method were found. The optimized parameters were: the height of the beam above the burner, the flow rate of acetylene, and the burner's horizontal position. Under the optimal conditions, the basic characteristics of the determination of sodium and potassium were studied. Sodium and potassium concentrations in the honey samples were determined under optimal conditions. A total number of 27 honey samples were analyzed. The sodium content ranged from 0.880 to 25.3 mg/kg. The potassium content was in the range of 223 - 2750 mg/kg. In the end, the measured concentrations of honey samples originating from the Czech Republic were compared with the foreign studies. Keywords Potassium, sodium, honey, atomic absorption spectrometry, flame spectrometry
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Monitoring of mercury and methylmercury content in fish meat and evaluation of risks associated with the consumption of this meat
Křížová, Lucie ; Pořízka, Jaromír (referee) ; Diviš, Pavel (advisor)
Mercury and its compounds are one of the most toxic global pollutants in the environment. It occurs in all segments of the environment, and it attains the food chain ang human body by people consuming fish. The theoretical part of this thesis examines the characteristics of mercury, its occurrence, the roots of its pollution, and the toxicity of various forms of mercury. Consequently, the thesis delineates analytical methodologies applied to determine the overall level of mercury and chemical forms of mercury. The practical part focuses on monitoring the level of mercury and methylmercury in 12 extracts of fish meat. The analyzer AMA 254 has been used to determine the level of mercury and methylmercury in these extracts. Based on the level that resulted from the measurements, the thesis concludes a risk that correlates with consuming this type of meat.
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Determination of lead in lung and brain samples of experimental mice after the inhalation of nanoparticles
Demydenko, Yana ; Zlámalová Gargošová, Helena (referee) ; Vašinová Galiová, Michaela (advisor)
Lead is a heavy toxic metal whose nanoparticles are present in the air due to combustion processes. Data on the safe concentration of lead nanoparticles for human health have not been sufficiently investigated. Previous studies in experimental mice have shown that inhalation of lead nanoparticles first damages lungs and kidneys, then liver, spleen and brain. With prolonged exposure, lead accumulates in the teeth and bones. This bachelor thesis is focused on monitoring of the lead content in lung and brain samples of experimental mice after different periods of nanoparticle inhalation. The aim of this bachelor thesis was to develop an analytical method for the determination of lead in biological samples using atomic absorption spectrometry with electrothermal atomization (ET-AAS). In this work, a decomposition method for mineralization of the biological matrix in a microwave mineralizer was proposed, and a procedure for the determination of lead using ET-AAS was further developed. The determination of lead at 217 nm using the NH4H2PO4/Mg(NO3)2 matrix modifier was verified by analysis of certified reference materials. Analysis of organ samples from experimental mice confirmed the detoxification mechanism in exposed individuals with a dependence on the time since the end of inhalation of lead nanoparticles.
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Next generation of hydride atomizers based on dielectric barrier plasma discharge
Kráľová, Zuzana ; Kratzer, Jan (advisor) ; Hrdlička, Aleš (referee)
Atomization conditions for selenium and lead hydrides in a dielectric barrier discharge (DBD) plasma atomizer with detection by atomic absorption spectrometry (AAS) were investigated in this work. Two designs of DBD atomizers were studied, the first one with glued electrodes and the second one with sputtered electrodes. The main experimental parameters were optimized, including supplied power and discharge gas (argon) flow rate. Additionally, the effect of several dryers was studied. Analytical figures of merit were determined for both plasma atomizers under the optimized conditions and compared to multiatomizer (MMQTA) as the most common hydride atomizer. The optimum flow rate for selenium determination was 75 cm3 min-1 Ar for both DBD atomizer designs as well as for MMQTA. In case of lead hydride atomization, ideal flow rate of argon was 175 cm3 min-1 for DBD atomizer with glued electrodes and 150 cm3 min-1 with DBD atomizer with sputtered electrodes, while MMQTA required only 100 cm3 min-1 Ar. The optimal power supply for DBD with sputtered electrodes was found significantly lower at 7.3 W for selenium and 13.3 W for lead. A dryer based on nafion membrane was found as the most effective for both analytes studied. Its efficacy was verified by optical emission spectrometry. As for analytical...
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