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Atomization of hydride forming elements in dielectric barrier plasma discharges
Baranová, Barbora
The aim of this diploma thesis was to optimize the atomization conditions of two hydride forming elements - bismuth and tellurium in dielectric barrier discharge (DBD) plasma atomizers using atomic absorption spectrometry (AAS) as a detector. Two types of electrode constructions of planar DBD atomizers were studied: glued and sputtered electrodes while two construction of high voltage power supply sources were investigated employing either a sinusoidal or square wave modulation of high voltage function. The effect of the gas phase dryer included in the apparatus upstream the atomizer was also investigated. A nafion membrane tube dryer was identified as the most effective one. Its efficiency was verified using optical emission spectrometry. With the nafion tube included in the apparatus, two main parameters of DBD atomizers were optimized: the voltage of the power supply source and argon flow rate, which served as a discharge gas. Using optimal conditions, analytical characteristics were determined for all atomizers used and these were subsequently compared with those achieved in an externally heated quartz (multi)atomizer (MM)QTA. In the case of bismuth, the optimal argon flow rate was determined to be 75 cm3 min-1 for all atomizers. The optimal value for the power supply source with sinusoidal...
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Atomization of hydride forming elements in dielectric barrier plasma discharges
Baranová, Barbora ; Kratzer, Jan (advisor) ; Hrdlička, Aleš (referee)
The aim of this diploma thesis was to optimize the atomization conditions of two hydride forming elements - bismuth and tellurium in dielectric barrier discharge (DBD) plasma atomizers using atomic absorption spectrometry (AAS) as a detector. Two types of electrode constructions of planar DBD atomizers were studied: glued and sputtered electrodes while two construction of high voltage power supply sources were investigated employing either a sinusoidal or square wave modulation of high voltage function. The effect of the gas phase dryer included in the apparatus upstream the atomizer was also investigated. A nafion membrane tube dryer was identified as the most effective one. Its efficiency was verified using optical emission spectrometry. With the nafion tube included in the apparatus, two main parameters of DBD atomizers were optimized: the voltage of the power supply source and argon flow rate, which served as a discharge gas. Using optimal conditions, analytical characteristics were determined for all atomizers used and these were subsequently compared with those achieved in an externally heated quartz (multi)atomizer (MM)QTA. In the case of bismuth, the optimal argon flow rate was determined to be 75 cm3 min-1 for all atomizers. The optimal value for the power supply source with sinusoidal...
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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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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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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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Miniature plasma DBD atomizer for AAS and AFS
Straka, Marek ; Kratzer, Jan (advisor) ; Hrdlička, Aleš (referee)
Five designs of dielectric barrier discharge (DBD) atomizers have been constructed and optimized employing arsane as a model analyte. The individual DBD designs differed from each other in the style of electrode attachment, electrode shape and area. An externally heated quartz tube atomizer and another DBD atomizer design that have been studied before were used as reference. All the atomizer designs studied including the reference atomizers were found compatible with detection by atomic absorption spectrometry (AAS) giving comparable sensitivity of 0.44 s ng-1 As and detection limit around 0.2 ng ml-1 As under optimum atomization conditions. However, significant differences in optimum operation conditions were found among the DBD designs in terms of the applied voltage depending strongly on the style of electrode attachment. The design with metal strip electrodes glued to a quartz body requires more than 14 kV to be operated. The design with sputtered electrodes of the same shape can reach the same sensitivity with 8.5 kV. Selected DBD designs have been proven to be compatible also with other spectrometric detectors such as atomic fluorescence spectrometry (AFS) reaching detection limit 0.05 ng ml-1 As or atomic emission spectrometry (AES) with detection limit of 30 ng ml-1 As showing the...
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Application of a dielectric barrier discharge plasma atomizer to hydride generation atomic absorption spectrometry (HG-DBD-AAS)
Albrecht, Michal ; Kratzer, Jan (advisor) ; Červený, Václav (referee)
Atomization of plumbane in a novel dielectric barrier discharge (DBD) plasma atomizer has been optimized employing detection by atomic absorption spectrometry. The performance of the DBD atomizer was subsequently compared to that of a conventional externally heated quartz tube atomizer (QTA). Lead from a standard solution was converted to plumbane by chemical reduction with sodium borohydride using an identical hydride generator for both atomizers. Argon at a flow rate of 175 cm3 min-1 was found as the best discharge gas while the DBD power supply rate was optimized to 22 W. The inner surface of the DBD atomizer was passivated by dimethyldichlorosilane (DMDCS) resulting in a twofold increase of sensitivity. Sensitivity of 0.10 s ng-1 Pb and a limit of detection of 0.82 ng cm-3 Pb were reached in the DBD atomizer with DMDCS-modified surface under the optimum atomization conditions. Better performance was achieved in a QTA atomizer, in which detection limit of 0.59 ng cm-3 Pb was reached and sensitivity was doubled (0.22 s ng-1 Pb) in comparison with DMDCS- modified DBD.
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Selenium determination by HG-AAS with preconcentration and atomization in a dielectric barrier plasma discharge
Duben, Ondřej ; Kratzer, Jan (advisor) ; Rychlovský, Petr (referee)
The aim of this thesis was to optimize atomization conditions for selenium hydride in a novel plasma atomizer based on dielectric barrier discharge (DBD) using atomic absorption spectrometry as a detector. Analytical characteristics have been subsequently determined and compared to those reached in a conventional externally heated quartz tube atomizer which was replaced by a sofisticated design of a multiatomizer (MMQTA) in this work. The limit of detection reached in DBD (0,24 ng ml−1 Se) is slightly worse to that observed in MMQTA (0,15 ng ml−1 Se). On the contrary, slightly better resistance towards interferences of Sb, Bi and As was observed in DBD atomizer in comparison with MMQTA. Possibility of selenium preconcentration in a DBD atomizer was studied reaching an overall preconcentration efficiency of 75 ± 5%. The detection limit in a preconcentration mode employing preconcentration period of 300 s has reached 0,012 ng ml−1 Se. Key words: hydride generation atomic absorption spectrometry, dielectric barrier discharge, hydride atomization, hydride trapping, selenium
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