Graduate Theses & Dissertations

Characterization of Synthetic and Natural Se8 and Related SenSm Compounds by Gas Chromatography-Mass Spectrometry
Elemental selenium has been extensively quantitatively measured in sediments; however, its physical composition is largely unknown, despite it being the dominant selenium species in some reducing environments. Here, for the first time, it is shown that small, cyclic selenium compounds can account for a quantitatively-relevant fraction of the total elemental selenium present. A new method was developed to analyze for cyclooctaselenium (Se8) in both synthetic samples and selenium-impacted sediments. Despite some analytical limitations, this gas chromatography-mass spectrometry (GC-MS) method is the first GC-MS method developed to identify and quantify Se8 in sediments. Once this method was established, it was then applied to more complex systems: first, the identification of compounds in mixed selenium-sulfur melt solutions, and then the determination of SenSm in selenium-impacted sediments. Despite complications arising from pronounced fragmentation in the ion source, assignment of definitive molecular formulae to chromatographically-resolved peaks was possible for five compounds. Developing a fully quantitative method to obtain elemental ratio information can aid in the assignment of molecular formulae to chromatographically-resolved SeS-containing chromatographic peaks. Coupling the existing gas chromatography method to an inductively coupled plasma-mass spectrometer (ICP-MS) system should accomplish this. However, due to a number of complications, this was not completed successfully during the duration of this thesis project. High detection limits for sulfur, retention time discrepancies, and inconsistent injection results between the GC-MS and GC-ICP-MS system led to difficulties in comparing results between both analytical methods. Despite these limitations, GC-ICP-MS remains the most promising method for the identification and quantification of SenSm compounds in synthetic melt mixtures and selenium impacted sediments. Author Keywords: gas chromatography-mass spectrometry, sediments, selenium
An Evaluation of Wastewater Treatment by Ozonation for Reductions in Micropollutant Toxicity to Fish
Micropollutants are discharged into the aquatic environment with industrial and domestic wastewater and these compounds may cause toxic effects in aquatic organisms. In this study, the toxic effects to fish of micropollutants extracted from ozonated and nonozonated municipal wastewater effluent (MWWE) were measured in order to assess the effectiveness of ozonation in reducing toxicity. Juvenile rainbow trout (Oncorhynchus mykiss) injected with extracts prepared from ozonated MWWE had significantly reduced induction of plasma vitellogenin (VTG), significantly reduced hepatic total glutathione (tGSH) levels and an elevated oxidized-to-total glutathione (GSSG-to-tGSH) ratio. Exposure of Japanese medaka (Oryzias latipes) embryos to extracts prepared from both ozonated and non-ozonated MWWE resulted in elevated developmental toxicity in both treatment groups. These results indicate that wastewater treatment by ozonation reduces the estrogenicity of wastewater, but treatment may induce oxidative stress and embryonic developmental toxicity due to the production of toxic by-products. Author Keywords: Estrogenicity, Micropollutants, Oxidative stress, Ozonation, Toxic by-products, Wastewater

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