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Investigation of Miniature Devices for Collection of Hydride Forming Elements in Atomic Spectrometry Methods
Krejčí, Pavel ; Čelechovská, Olga (referee) ; Janoš, Pavel (referee) ; Otruba, Vítězslav (referee) ; Dočekal, Bohumil (advisor)
Capability of a prototype of miniature collection device based on a strip of the molybdenum foil for collecting hydride forming elements (As, Se, Sb and Bi) was studied. The device was combined with a miniature hydrogen diffusion flame for detection by atomic absorption spectrometry. The conditions for trapping and subsequent vaporization of analytes of interest were optimized. A twin-channel hydride generation system was used for study of mutual interference effects of co-generated hydride forming elements. The influence of modification of the molybdenum surface with noble metals - Rh, Pt and Ir on trapping and vaporization processes was also studied and changes of microstructure of the foil surface after modification were investigated using scanning electron microscope equipped with energy dispersive x-ray analyzer and electron backscattered diffraction system. Complementary radiotracer and radiography experiments were performed in order to determine trapping efficiency and to assess the spatial distribution of collected analytes within the device. Practical application of the method was demonstrated on determination of antimony in water samples at trace level. Possibility of multi-element analysis was demonstrated by combining the collection device with atomization and excitation of the analyte in microwave induced plasma and with detection by atomic emission spectrometry method. The results of the experiments proved that tested miniature collection device is capable of trapping analytes that form volatile hydrides. This device can be coupled to various types of atomizers, typically used in spectrometry methods. Thus, very sensitive and specific detection of hydride forming elements can be performed.
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Study of Generation, Trapping and Atomization of Hydride Forming Elements for Atomic Spectrometry
Furdíková, Zuzana ; Sommer, Lumír (referee) ; Čelechovská, Olga (referee) ; Řehůřková, Irena (referee) ; Dočekalová, Hana (advisor)
Interference effects of co-generated hydrides of arsenic, antimony, bismuth and selenium on trapping behavior of selenium or antimony hydrides (analytes) within iridium modified, transversely heated graphite tube atomizer (THGA) was investigated. A twin-channel hydride generation system was used for independent separate generation and introduction of analyte and interferent hydrides, i.e. in simultaneous and/or sequential analyte-interferent and interferent-analyte mode of operation. Influence of the analyte and modifier mass, interferent amount, trapping temperature and composition of the gaseous phase was studied. A simple approach for elimination of mutual interference effects by modification of the gaseous phase with oxygen in substoichiometric ratio to chemically generated hydrogen is proposed and suppression of these interference effects is demonstrated. A hypothesis on mechanism of trapping and mutual interference effects is drawn.
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Thermal aging of lead-free low-temperature joints
Jansa, Vojtěch ; Šandera, Josef (referee) ; Adámek, Martin (advisor)
The aim of this masterś thesis is to investigate properties of lead-free low-temperature solders after termal aging. The theoretical part is focused on various types of lead - free solders, pastes used for the manufacture of electrical circuits by thick-film technology and methods of testing the properties of the soldered joints. The practical part deals with the design and production of test substrates for testing the solder joints formed between the SMD component and the ceramic substrate. Two solder bismuth-containing solder was selected for testing, the SAC solder was selected as the reference. After aging with temperature cycling from -30 ° C to 115 ° C, the data obtained by testing the mechanical strength of the solder joint by the shear test is evaluated.
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The influence of cast iron inoculation with bizmut containing inoculant on structure and mechanical properties
Nyékyová, Dominika ; Navrátil, František (referee) ; Roučka, Jaromír (advisor)
The diploma thesis deals with the modification and inoculation of cast iron with spheroidal graphite, the influence of the chemical composition on the shape and size of the graphite nodules and ferrite/perlite ratio in the structure. The aim of the practical part was to determine the effect of inoculant containing bismuth (SMW 605) on microstructure and mechanical properties of ferritic ductile cast iron GJS 400-15. The dissolving time of mold inoculant was further investigated. The samples were subjected to a tensile test, Charpy impact test, hardness test and graphite morphology and ferrite/perlite examination using standard ČSN EN ISO 945-1.
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Electrochemical generation of tellurium and bismuth hydrides for AAS
Resslerová, Tina ; Hraníček, Jakub (advisor) ; Šíma, Jan (referee)
Tellurium and bismuth are non-biogenous elements, which can be accumulated in human body. The aim of this work is focused on the determination of these elements by the electrochemical hydride generation with non-membrane electrolytic cell with quartz tube - atomic absorption spectrometry. The first step of the work was to optimize parameters for the continuous setup measurements and to obtain its figures of merit. After this, the arrangement with most suitable conditions for determination of these elements was converted to the flow injection setup (FIA) and all experimental parameters were again optimized and its figures of merit were obtained. The conditions of hydride generation were studied for platinum, lead and silver cathodes with hydrochloric and sulphuric acids and their sodium salts as electrolytes. The optimizations of the FIA setup were performed on platinum cathode in hydrochloric acid for bismuth and on lead cathode in sulphuric acid for tellurium. The limit of detection achieved for the generation of tellurium hydride was 1.1 ppm with a linear range up to 20 ppm; for the bismuth hydride the limit of detection was 9.5 ppm and limit of linearity 50 ppm. Keywords Bismuth, tellurium, electrochemical hydride generation, atomic absorption spectroscopy, flow injection analysis
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Modular design for in-atomizer preconcentration of hydride forming elements with AAS detection
Novák, Petr ; Kratzer, Jan (advisor) ; Korunová, Vlasta (referee)
Modular design of hydride trap-and-atomizer device for AAS is constructed and tested. Modular design enables to test different preconcentration surfaces easily. Efficient in- atomizer preconcentration allows to reach detection limits of hydride forming elements at ultratrace levels. Bismuth and arsenic were chosen as model analytes and their preconcentration efficiencies were quantified employing quartz and sapphire as preconcentration surfaces. The results reached in the modular design were compared to those found previously in the compact quartz trap-and-atomizer device. The performance of the modular design is fully comparable with that of compact trap-and-atomizer design. Modular design can thus be employed for testing of novel preconcentration surfaces.
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The influence of cast iron inoculation with bizmut containing inoculant on structure and mechanical properties
Nyékyová, Dominika ; Navrátil, František (referee) ; Roučka, Jaromír (advisor)
The diploma thesis deals with the modification and inoculation of cast iron with spheroidal graphite, the influence of the chemical composition on the shape and size of the graphite nodules and ferrite/perlite ratio in the structure. The aim of the practical part was to determine the effect of inoculant containing bismuth (SMW 605) on microstructure and mechanical properties of ferritic ductile cast iron GJS 400-15. The dissolving time of mold inoculant was further investigated. The samples were subjected to a tensile test, Charpy impact test, hardness test and graphite morphology and ferrite/perlite examination using standard ČSN EN ISO 945-1.
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