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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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Determination of Titanium and Phosphorus by Atomic Absorption Spectrometry
Jeníková, Eva ; Hraníček, Jakub (advisor) ; Rychlovský, Petr (referee)
Předkládaná bakalářská práce se zabývá optimalizací metod stanovení titanu a fosforu technikou atomové absorpční spektrometrie s plamenovou atomizací ve složení acetylen-oxid dusný. Pro jednotlivá stanovení byly experimentálně nalezeny optimální hodnoty pro průtokovou rychlost acetylenu, koncentraci přídavku hliníku či vápníku, výšku paprsku nad hranou hořáku a jiné faktory pro zvýšení analytického signálu. Za těchto experimentálně zjištěných podmínek bylo provedeno stanovení a zjištění základní charakteristiky metod u obou prvků. Významnost stanovení těchto dvou prvků souvisí s tím, že materiály na bázi titanu a oxidu titaničitého povrchově modifikované sloučeninami fosforu jsou perspektivní pro řadu biomedicínských i průmyslových aplikací. Powered by TCPDF (www.tcpdf.org)
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Application of Atomic Absorption Spectrometry for Determination of Selected Elements from Potential Ecological Burden Area
Juránková, Lada ; Hraníček, Jakub (advisor) ; Šíma, Jan (referee)
This work is focused on the determination of selected (chemical) elements (Fe, Mn, Zn, Cr, Na, K, Mg a Ca) in a potential ecological burden area using flame atomic absorption spectrometry as a detection technique. A potential ecological burden is represented by tires which are used as a construction material or as an environment surrounding for growing decorative and consumable plants. Analytes were determined in plant origin samples. Firstly, the samples were dried in a laboratory electric dryer. The weighted amount of a dried sample (approximately 0.2 g) was digested inside a microwave decomposition device with an addition of nitric acid and hydrogen peroxide. An optimization of experimental parameters was done for each of the elements before sample measuring. A burner height was optimized and 8 mm height was chosen as a optimum for most elements. Under the optimum condition basic characteristics were measured for each element separately. These characteristics included limits of detection that were: 0.05; 0.01; 0.08; 0.21; 0.02; 0.01; 0.01; 0.01 mg L-1 for the following elements: Fe, Mn, Zn, Cr, K, Ca, Mg and Na, respectively. The limits of quantification, sensitivity and repeatability were determined for each element as well. A significant attention was paid to the content of zinc in the studied...
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Arsenic determination in beer samples and raw materials for its preparation
Švadlenová, Veronika ; Hraníček, Jakub (advisor) ; Jelínek, Ivan (referee)
This thesis describes the optimization of the method for determination of arsenic by the chemical hydride generation coupled with AAS detection in beer samples and raw materials for its preparation. The beer usually contain arsenic at ultratrace level, however, it is necessary to monitor the concentration of this element in the beer. The routinely used method for determination of arsenic is determination by electrothermal atomization. This approach is time consuming, expensive and less sensitive. It has been developer suitable determination of arsenic as a faster and less expensive method. For this method there was optimized the flow rate of argon to 75 ml·min-1, the optimum flow rate for the reagents was 4.0 ml·min-1 and for the sample 5.0 ml·min-1 . 3 % NaBH4 in 0.5 % NaOH was used as the reducing agent for the determination of arsenic, and HCl diluted 1:1 with distilled water was used to acidify the sample. With this parameter LOD was 0.32 μg·l-1 and LOQ 1.05 μg·l-1 . It has been tested the arsenic determination in samples of barley, malt and potable water as beer raw materials. It has been found that the beer matrix is unsuitable for the hydride generation technique due to a stormy reaction in the gas/liquid phase separator. The effect of pretreatment, which is likely to enhance the effect of...
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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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Mechanism of atomization of selected hydride forming elements in an externally heated quartz tube atomizer and a dielectric barrier discharge atomizer
Juhászová, Lucie ; Kratzer, Jan (advisor) ; Hrdlička, Aleš (referee)
Atomization conditions for tin hydride in the planar dielectric barrier discharge (DBD) plasma atomizer were optimized with detection by atomic absorption spectrometry (AAS). The effects of apparatus arrangement such as the shape of a waveform function of the high voltage power supply source, DBD atomizer design as well as presence of a dryer tube filled with NaOH pellets to prevent residual aerosol and moisture transport into the DBD were investigated in detail. The optimal experimental setup consisted of a square wave high voltage power supply source coupled to a DBD with vapor-deposited electrodes in the presence of NaOH dryer upstream the DBD atomizer. Argon was found as the best discharge gas under a flow rate of 120 mL min-1 while the DBD optimum high voltage supply rate was 7 kV. A sensitivity of 0.05 s ng-1 Sn and a limit of detection of 1.1 ng mL-1 Sn were reached under optimized conditions. Optimization of the whole experimental setup resulted in 7-fold improvement of sensitivity compared to the original arrangement consisting of a sinusoidal source coupled to a DBD atomizer with glued electrodes in absence of the dryer. Keywords atomic absorption spectrometry, hydride generation, hydride atomization, quart tube atomizer, dielectric barrier discharge (DBD)
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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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