|
|
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...
|
|
| |
|
| |
|
|
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.
|
|
| |
|
|
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...
|
|
|
Determination of zinc, cadmium and nickel in leaves by inductively coupled plasma-mass spectrometry
Plodík, Michal ; Hraníček, Jakub (advisor) ; Červený, Václav (referee)
Práce je zaměřena na stanovení těžkých kovů (zinku, kadmia a niklu) v listech různých druhů stromů. Vzorky byly odebrány z různých lokalit na území České republiky. Pro analýzu byla použita hmotnostní spektrometrie s indukčně vázaným plazmatem, která je dostatečně citlivá pro předpokládané nízké koncentrace vybraných kovů. Pro stanovení koncentrace byla klíčová příprava vzorků pro mikrovlnný rozklad v koncentrované kyselině dusičné. Naměřené koncentrace sledovaných kovů se lišily nejen mezi lokalitami a jednotlivými rostlinnými druhy, ale také v rámci jedné lokality. Použitá metoda ICP-MS prokázala dostatečnou citlivost i u prvků s přirozeně nízkou koncentrací v životním prostředí, což bylo v této práci kadmium.
|
|
|
Interferences in determination of antimony by electrochemical generation of volatile compounds and atomic fluorescence spectrometry
Kostúrová, Dominika ; Červený, Václav (advisor) ; Nováková, Eliška (referee)
Antimony is a highly toxic element that enters the environment through natural processes and human activities as well. It is necessary to determine its ultra-trace amounts in various materials such as water, soil and biological samples. Due to the heterogeneity of sample matrices, the determination of antimony is problematic because of frequent interactions. The aim of this work was to investigate the effects of various interferents on the determination of antimony by electrochemical generation of volatile compounds and atomic fluorescence spectrometry. In total, 18 interference dependencies were measured in the determination of Sb(III) and Sb(V). The following ions were selected for the interference study: SO4 2- , Cl- , NO3 - , NO2 - , Fe3+ , Fe2+ , As3+ , Se4+ and Bi3+ . The As3+ ion had the most interesting course of all the interferents and could be used as a suitable additive to increase the sensitivity of antimony determination.
|
|
|
Spectrophotometric determination of stability constants of cyclodextrin derivatives by phenolphthalein method
Haiklová, Simona ; Dian, Juraj (advisor) ; Červený, Václav (referee)
This bachelor thesis deals with the determination of stability constants of cyclodextrins and their derivatives in the formation of supramolecular complexes with phenolphthalein. Cyclodextrins - macrocyclic oligosaccharides - are characterized by the shape of a truncated cone, whose internal hydrophobic cavity can form, with suitable substances, host-guest inclusion complexes. The formation of these inclusion complexes is accompanied by a change of a number of physicochemical parameters of the included compounds. In this bachelor thesis, the change of optical absorption of phenolphthalein, which has characteristic violet color in the alkaline area, was studied during its interaction with selected CD macrocycles. The formation of a supramolecular complex resulted in a decrease in optical absorption, which was quantified and used to determine stability constant. In the bachelor thesis, the supramolecular interaction of phenolphthalein with six derivatives of cyclodextrins were studied - basic cyclodextrins β-CD a γ-CD and their two derivatives. In the selected derivatives of these CDs the -OH groups in positions 2, 3, and 6 were replaced either by hydroxypropyl groups (hydroxypropyl-β-CD and hydroxypropyl-γ- CD) or (randomly) by methyl groups (RaMe-β-CD and RaMe-γ-CD). For these CD derivatives, the...
|
|
|
Interferences in determination of antimony by UV-photochemical generation of volatile compounds and atomic fluorescence spectrometry
Kračmarová, Aneta ; Červený, Václav (advisor) ; Hraníček, Jakub (referee)
This work is focused on the study of interferents of selected elements during UV-photochemical generation of volatile antimony compounds. The interferents included transition metals, halides, hydride-forming elements and salts of mineral acids. Detection was performed by atomic fluorescence spectrometry. Some of the tested added substances proved to be potential reaction modifiers; in their presence, an increase in responses was observed. The best results were obtained using Fe3+ for the determination of Sb3+ and SO4 2- had the best results for the determination of Sb5+ . The largest interferent, i.e. the substance causing the most significant decrease in signal, was for both antimony ions Se4+ .
|
guest ::
RSS feed.