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Atomic fluorescence spectrometry with volatile species generation - a sensitive tool for ultra-trace elemental analysis
Štádlerová, Barbora
This thesis encompasses a development of innovative methodologies based on atomic fluorescence spectrometry, offering precise and sensitive determination of ultra-trace elements, such as bismuth, cadmium, and nickel. The common denominator of all parts of this work is the use of a research-grade non-dispersive atomic fluorescence spectrometer (AFS). First part of this work is dedicated to the development of a highly sensitive methodology for bismuth determination based on hydride generation (HG) coupled with AFS. Bismuthane was generated by the reaction with NaBH4 in HCl medium in a flow injection arrangement and directed by a stream of carrier argon and hydrogen to an atomizer. A detailed optimization of the optical path of the spectrometer (electrodeless discharge lamp, lenses and interference filter) and atomization parameters in two flame atomizers - miniature diffusion flame (MDF) and flame-in-gas-shield atomizer (FIGS) - was performed. An excellent repeatability and extremely low limits of detection were achieved, namely 1.8 ng L−1 with the MDF and 0.9 ng L−1 with the FIGS. Subsequently, a photochemical vapour generation (PVG) of bismuth was coupled to AFS, employing a flow injection arrangement of the generator, a standard mercury low-pressure UV lamp and a coiled Teflon reactor. A flow rate...
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Atomic fluorescence spectrometry with volatile species generation - a sensitive tool for ultra-trace elemental analysis
Štádlerová, Barbora ; Musil, Stanislav (advisor) ; Spěváčková, Věra (referee) ; Dočekalová, Hana (referee)
This thesis encompasses a development of innovative methodologies based on atomic fluorescence spectrometry, offering precise and sensitive determination of ultra-trace elements, such as bismuth, cadmium, and nickel. The common denominator of all parts of this work is the use of a research-grade non-dispersive atomic fluorescence spectrometer (AFS). First part of this work is dedicated to the development of a highly sensitive methodology for bismuth determination based on hydride generation (HG) coupled with AFS. Bismuthane was generated by the reaction with NaBH4 in HCl medium in a flow injection arrangement and directed by a stream of carrier argon and hydrogen to an atomizer. A detailed optimization of the optical path of the spectrometer (electrodeless discharge lamp, lenses and interference filter) and atomization parameters in two flame atomizers - miniature diffusion flame (MDF) and flame-in-gas-shield atomizer (FIGS) - was performed. An excellent repeatability and extremely low limits of detection were achieved, namely 1.8 ng L−1 with the MDF and 0.9 ng L−1 with the FIGS. Subsequently, a photochemical vapour generation (PVG) of bismuth was coupled to AFS, employing a flow injection arrangement of the generator, a standard mercury low-pressure UV lamp and a coiled Teflon reactor. A flow rate...
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