M.Sc. / The understanding of the classification and origin of geological systems is facilitated by the acquisition of accurate and precise analytical data. New instrumentation is rapidly developed for the preparation and quantitative analysis of geological materials using smaller amounts of sample, with lower limits of detection and faster analysis times. The development of new methodologies is crucial for the effective utilisation of new instrumentation. This study was conceptualised because of the relationship between the Department of Geology and the Central Analytical Facility of the Faculty of Science, University of Johannesburg. There is a high demand for accurate and precise chemical data for various lithologies and the availability of high-end analytical equipment, but little practical expertise to utilise this equipment to its full potential. The study is centred round the analysis of four common sedimentary lithological groups that are routinely studied by the Department of Geology namely carbonate rocks, shales, iron ore and manganese ore. A large literature base exists for the decomposition and analysis of geological materials. The bulk of this literature is centred round more established and conventional methods of sample preparation and analysis. The use of microwave digestion instrumentation and methodologies in recent times has revolutionised sample decomposition with shorter decomposition times, smaller sample masses required for decomposition, lower loss of analytes to volatilisation and creating a safer laboratory environment for analysts to work in. Inductively coupled plasma optical emission spectroscopy (ICP-OES) is a more mature method of sample analysis, being commercialised in the mid 1970’s, while inductively coupled plasma mass spectroscopy (ICP-MS) is a newer technique, v being commercialised as of the mid 1980’s. These two techniques are multi-element techniques, with low limits of detection and fast analysis times for a plethora of analytes, over seventy elements for ICP-OES and over eighty elements for ICP-MS. Samples from all four lithological groups were successfully digested in a microwave digestion unit with varying combinations of nitric acid (HNO3), hydrochloric acid (HCl), perchloric acid (HClO4) and hydrofluoric acid (HF) and various digestion programs. Accurate and repeatable methods of analysis were developed for iron, manganese, calcium and potassium for all four lithologies with ICP-OES; aluminium was successfully determined for shale, iron and manganese ore with ICP-OES. Titanium, sodium, arsenic, barium, bismuth, chromium, copper, molybdenum, scandium, strontium and vanadium were determined for all four lithotypes with acceptable accuracy and repeatability using ICP-MS.

Thesis (Ph. D.)--University of Texas at Austin, 2001. / Vita. Includes bibliographical references. Available also in a digital version from Dissertation Abstracts.

abstract / Chemistry / Doctoral / Doctor of Philosophy

Not available / text

The objective of this study was to fully characterise drift phenomena in inductively coupled plasma atomic emission spectroscopy (ICP-AES) in order to develop novel correction procedures to aid routine analysis. Long-term drift of the analytical signal continues to be a potential disadvantage when using ICP-AES and often necessitates regular recalibration. The long-term stability of three commercially available Instruments was studied using In each case a range of analyte and intrinsic plasma emission lines. Long-term fluctuations were observed which generated drift bias of up to 20% on the initial values. The drift pafterns were characterised and found to be qualitatively reproducible. In most cases, similar long-term fluctuations were observed independent of the analyte or nature of the emission line. In addition, high inter-element correlation was observed on the long-term fluctuations even when sequential acquisition was employed. In order to study the fundamental causes of drift, the effect of two key instrumental parameters, i.e. the RF power and the nebutiser gas flow rate were studied with respect to the stability of the signal. Different drift patterns were found depending on the working conditions. Classical statistical methods and a multi-way approach. PARAFAC. were then employed to describe the system. The use of intemal standards to correct for drift has also been investigated, but found to be of benefit only under certain defined conditions (i.e. robust conditions, high RF power and low nebuliserflow rate). At soft conditions, low RF power and medium to high nebuliser flow rate, the system Is very unstable and intemal standardisation is not fully effective as a correction method. For such conditions, a novel correction procedure has been developed, which employs the drift pattem of one intrinsic plasma line (i.e. an argon line) and a correction factor which is specific for each emission line. The drift values were reduced from around 20% before correction to better than ±2% following the described protocol. Finally, the effects of chemical matrices on the long-term stability of the emission signals have been evaluated. Three synthetic matrices were prepared simulating nitric, soil and water matrices. The stability of the instrument when working wrth these matrices at both robust and soft conditions was found to be poor, especially when the solution was matched with the soil matrix. The use of more robust conditions did not improve the long-temi stability of the emission signals. The outcome of this study proved to be a better understanding of drift phenomena and a novel method for drift correction.

Thesis (Ph. D.)--University of Texas at Austin, 2005. / Vita. Includes bibliographical references.

published_or_final_version / abstract / Chemistry / Master / Master of Philosophy

published_or_final_version / Statistics and Actuarial Science / Master / Master of Philosophy

No description available.

The introduction of deep reactive ion etching (DRIE) technology has greatly expanded the accessible design space for microscopic systems. Structures that are hundreds of micrometers tall with aspect ratios of 40:1, heretofore impossible, can now be achieved. However, this technology is primarily a forming technology, sculpting structures from a substrate. This work seeks to complement deep reactive ion etching by developing an electrical isolation technology to enable electro-mechanical function in these new deep reactive ion etched structures. The objective of the research is twofold. The first is to develop and characterize an electrical isolation technology for DRIE, single crystal silicon (SCS) micro-electro-mechanical systems (MEMS) using temperature gradient zone melting (TGZM) of aluminum junctions for diodic isolation. The second is to demonstrate the utility of this electrical isolation technology in the design, simulation, fabrication, and testing of a MEMS device, i.e. a micro-gyroscope, in such a way that the benefits from junction isolated, deep reactive ion etched, single crystal silicon devices are preserved.