Thesis (Ph. D.)--University of Washington, 2001. / Vita. Includes bibliographical references (leaves 152-156).

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Graduation date: 1995

M. Tech. (Department of Chemistry, Faculty of Applied and Computer Sciences), Vaal University of Technology / Water soluble metal sulfide nanoparticles were successfully synthesized using an aqueous, simple and environmentally friendly synthetic method in the presence of ʟ-alanine, ʟ-aspartic acid and lactose, acting as both stabilizers and crystal growth modifiers. The structural and optical properties of the synthesized metal sulfide nanoparticles were characterized by X-ray diffraction (XRD), transmission electron microscopy (TEM), Fourier transform infrared (FTIR), Ultraviolet-visible (UV-Vis) and photoluminescence spectroscopy. Colloidal method was employed in the synthesis of CuS, ZnS and FeS nanoparticles from metal chlorides as precursors and thioacetamide (TAA) as a sulphur source. The effect of temperature on the growth and solubility of nanoparticles was investigated. The absorption spectra of all samples prepared were blue shifted as compared to their bulk materials indicating small particles size. The morphologies and sizes of the nanoparticles were influenced by the variation of temperature and capping agent. TEM images revealed interesting changes in the morphology of CuS nanoparticles formed from various capping agents. By varying the temperature, ʟ-aspartic acid-capped CuS nanoparticles changed from rod-shaped particles to particles dominated with hexagonal shape. However, the morphologies of both ZnS and FeS nanoparticles were close to spherical shape and were unaffected by either change of temperature or capping agent. Water-solubility of bio-functionalized CuS, ZnS and FeS nanoparticles was investigated. Amongst the three capping agents used, ʟ-alanine (Ala) was found to be the most effective capping agent to render solubility of the nanoparticles. As the temperature was increased, the solubility of the particles also increased. Cytotoxicity and antimicrobial activity of ʟ-alanine-capped CuS and ZnS nanoparticles were investigated. The particles were less toxic at low to moderate concentrations and only induced toxicity at higher concentrations. Particles synthesized at 95 °C were less toxic compared to other nanoparticles (35 and 65 °C) for both two set of experiments, as informed by the CC50 values. Antimicrobial properties were tested using different strains of both positive and negative bacteria and fungi. It was found that Ala-capped CuS nanoparticles were more effective against the bacteria than Ala-capped ZnS nanoparticles.

Alkali metal chloride melts are used to refine refractory metals and as a heat carrier for promising nuclear reactors. The oxygen content is a critical parameter for such systems. It determines technological process and the quality of obtained products. The work is devoted to the development of methods for the determination of oxygen in chloride melts. HORIBA EMGA-620W/C gas analyzer was used. The paper presents information on the choice of methods for determining oxygen in various oxygen-containing compounds of tungsten and molybdenum. An inert chamber has been developed and combined with a gas analyzer. This allowed to determine low oxygen contents in volatile matrices with high affinity for oxygen. / Системы хлоридных расплавов щелочных металлов применяются для рафинирования ряда тугоплавких металлов и в качестве теплоносителя в перспективных реакторах нового типа. Содержание кислорода в таких системах является критическим параметром, обуславливающим правильный ход технологического процесса и качество получаемой продукции. Работа посвящена разработки методики определения кислорода в хлоридных расплавах. Для измерений использовали газоанализатор HORIBA EMGA-620W/C. В работе представлены сведения о выборе способов определения кислорода в различных кислородсодержащих соединениях вольфрама и молибдена. Разработана и совмещена с газоанализатором инертная камера, позволяющая проводить определения низких содержаний кислорода в относительно летучих матрицах, в том числе с макрокомпонентами, имеющими высокое сродство к кислороду. Выбраны оптимальные условия проведения измерений.