Thesis (Ph. D.)--West Virginia University, 2002. / Title from document title page. Document formatted into pages; contains ix, 99 p. : ill. (some col.). Includes abstract. Includes bibliographical references.

Thesis (Ph. D.)--West Virginia University, 2008. / Title from document title page. Document formatted into pages; contains viii, 144 p. : ill. (some col.). Includes abstract. Includes bibliographical references.

Thesis (Ph. D.)--West Virginia University, 2009. / Title from document title page. Document formatted into pages; contains xvi, 162 p. : ill. (some col.). Includes abstract. Includes bibliographical references.

Thesis (M.S.)--University of California, Santa Cruz, 1992. / Typescript. Includes bibliographical references (leaves 48-51).

Thesis (Ph. D.)--University of California, Santa Cruz, 1994. / Typescript. Includes bibliographical references.

M.Sc. (Zoology) / Tilapia sparrmanii (Smith) was exposed to sub-lethal doses of chromium, manganese, zinc and iron for 96 hours at an acidic pH (5), a physiological pH (7,4) and an alkaline pH (9), as well as a prolonged exposure (2 - 4 weeks) at an uncontrolled pH. In the laboratory fish were kept in aquaria which were supplied with continuously flowing borehole water. Controlled laboratory conditions existed during experimentation. Blood and liver samples of the experimental fish were sampled after exposure. The bioconcentration and the effect of the selected metals at the mentioned conditions, were thereby determined on bloodcoagulation, total and differential leucocyte counts, and liver enzYmes to investigate the possible damage to the liver. As metals have the ability to enter and concentrate in the body, the bioconcentration of each metal was determined by atomic absorption sPectrophotometry in the blood and liver. Chromium showed an increase in concentration in both the blood and liver, with an increase in pH after short term (96h) exposure. The statistical significant increases of manganese concentration in the blood over a short term were not reflected in the liver. It may be indicative of homeostatic control. A similar phenomenon was found with .zd.nc , The concentration of zinc in the liver did not reflect the progressive decrease in the blood wi th a increase in pH. Iron revealed a statistical significant increase in bioconcentration in the liver with, an increase in pH, which is indicative of the activity of the liver. The long term exposure of fish to chromium and manganese caused a significant increase in the concentration of the metals in the blood and liver. The only significant increase in concentration after exposure to iron, occured . in the Iiver. Exposure to zinc however caused a statistical significant decrease in concentration in both the blood and liver. Differential leucocyte counts reflected lymphocytosis, eosinophilia, monocytopenia and neutropenia, after short term exposure. These conditions nearly always resulted in leucopenia. Long term exposure to manganese and zinc reflected both eosinophilia and neutropenia. Chromium reflected eosinophilia, and iron, neutropenia. The only statistically significant change in the number of leucocytes after long term exposure, was caused by zinc and resulted in leucopenia. According to the photokymographic observation of blood coagulation by the thrombelastograph, exposure to the selected heavy metals lead to a prolonged clotting time and thrombocytopenia. Long term exposure (4 weeks) to manganese caused another bleeding disease, called hemophilia. It was thus evident that the exposure to heavy metals led to clotting defects, which caused bleeding.

The regulations for water fluoridation of South African municipal waters up to the optimum fluoride (F-) concentration of 0.7 mg/L, (Government Gazette, 2001) have been legislated. Fluoridation processes need accurate analytical methodology for the determination of F- , because F- has a narrow margin of safety between beneficial and toxic levels. In this work the analytical chemistry of F- was investigated comprehensively and guidelines compiled for the accurate determination of low level F- (between 0.05 to 1 mg/L) in aqueous systems. The first part of this study focused on method validation and the evaluation of the ISE and IC methods. The analytical methodologies were applied to the analysis of natural waters such as river water (Vaal and Crocodile Rivers), dam water (Hartbeespoort Dam), and drinking water (Johannesburg municipal tap water) to evaluate the performance of the chosen methods in the analysis of real samples and to assess the effect of the sample matrix on the accuracy of F- determinations. An inter-laboratory study in collaboration with the South African Bureau of Standard (SABS) was carried out to evaluate the proficiency of South African analytical laboratories and to check the proficiency of the procedures developed in this study. In the second part of this study, the development of an IC-ICP-OES and IC-ICP-MS method was investigated for the speciation of fluoro-aluminium complexes. This work was motivated by the fact that the water fluoridation could lead to remobilisation of scale from municipal pipes. Scale may contain aluminium hydroxide or oxide precipitates that can dissolve as fluoroaluminates or hydroxofluoro aluminates. The speciation of cationic fluoro-aluminates, free Al3+, AlF2+ and, AlF2 + together with the neutral AlF3 0, was based on cation exchange Ion chromatography (IC) coupled with Inductively Coupled Plasma- Optical Emission Spectroscopy (ICP-OES) and Inductively Coupled Plasma Mass spectroscopy (ICP-MS). / Prof. P.P. Coetzee

Thesis (Ph.D. ) -- McMaster University, 1999. / Includes bibliographical references [p.47-55]. Also available via World Wide Web.

M.Sc. / The behaviour i.e. the distribution, bioavailability and toxicity of an element depends on the particular species in which it is present. That being said the prediction of the behaviour of species can therefore not be predicted by determination of the total concentration alone. Speciation analysis is thus an important process, which seeks to identify and quantify the species that occur in a sample. By identifying the species one is better equipped to predict the behaviour of the element if it were released into the ecosystem as well as if it were used in industrial processes. The speciation analysis of the dominant chromium species, Cr(III) and Cr(VI), has received much attention as these contradictory species are involved in many industrial processes such as plating and tanning for example. The species have opposing behaviour as Cr(III) is found to be a necessary micronutrient for mammals where as Cr(VI) is known to be toxic. Of the numerous methods developed for chromium speciation analysis, the on-line process of chromatographic preconcentration followed by simultaneous detection with a sensitive detector produces a synergistic effect for the successful speciation analysis of chromium. It was thus decided to study ion chromatography hyphenated with an ICP-OES as a means of studying chromium species. Anion chromatography coupled with ICP-OES was the basis for the development of the first method. Complexation of Cr(III) with EDTA to form a monovalent anion preceded its separation from Cr(VI) as the chromate anion. A carbonate-bicarbonate eluent was used to elute the species from a Dionex AG 9 guard column coupled with an AS 9 separation column. This method proved to be effective and fast, with each analysis taking less than two minutes. The second method was based on cation chromatography in the form of a Dionex CG12A guard column being coupled with an ICP-OES spectrometer as the detector. This method made use of a gradient elution program in which hexavalent chromium was eluted first with ammonium nitrate followed by trivalent chromium with nitric acid. This method was successfully applied to synthetic samples and was found to be effective.

Thesis (M. Sc.(Chemistry)) -- University of Limpopo, 2017. / Great Letaba and Mokolo Rivers are major sources of water for domestic use, agriculture and recreational activities in Limpopo Province, South Africa. These Rivers are predisposed to pollution sources from atmospheric deposition of mine dust, emissions from power stations and burning fuel, return flows from agriculture and municipal wastewater discharges and sewage effluents, which may potentially affect the quality of water and the inhabiting biota. Arsenic (As) is an element of prime concern in aquatic systems exposed to such pollution sources due to its toxicity to humans and aquatic life. The quantification and speciation of As in Mokolo and Great Letaba Rivers is important to assess the current levels and predict future trends in the quality of the two rivers. Speciation of As in water and sediments is crucial since the toxicity depends on its chemical forms. In this study, various analytical approaches were explored to precisely identify and quantify different As species in water and sediment samples collected from Great Letaba and Mokolo Rivers. Sample preparation was carried out with an intensive care to efficiently identify and quantify As species. Identification of each species in the samples was based on matching standard peaks with retention times by simple injection of standards of As species into Hamilton PRP X100 column. The chromatographic separation and determination of As3+, dimethylarsinic acid (DMA), monomethylarsonic acid (MMA) and As5+ in water and sediment samples were achieved by on-line coupling of high performance liquid chromatography (HPLC) to inductively coupled plasma-mass spectrometry (ICP-MS). A novel extraction method for As species in sediments based on 0.3 M (NH4)2HPO4 and 50 mM EDTA showed no species interconversion during extraction. Baseline separation of four As species was achieved in 12 minutes using gradient elution with 10 mM and 60 mM of NH4NO3 at pH 8.7 as mobile phases. The analytical figures of merits and validation of analytical procedures were assessed and adequate performance and percentage recoveries ranging from 81.1 – 102% for water sample and 73.0 – 92.0% for sediments were achieved. The As species concentration in water and sediment samples were found in the range 0.224 – 7.70 μg/L and 74.0 – 92.0 ng/g, respectively. The DMA was not detected in both water and sediment samples. viii The As content in sediments depends on the solid phase partitioning between inorganic As species and trace elements such as iron (Fe), manganese (Mn) and aluminium (Al). Knowledge of the extent of this partitioning is important to evaluate the distribution and pathways of As in water, aquatic organisms and possible exposure of animals and human beings. Therefore, total concentrations of As, Fe, Mn and Al in water and sediment samples were determined using ICP-MS and inductively coupled plasma–optical emission spectrometry (ICP-OES). The analytical procedures were validated using standard reference materials (SRMs) with percentage recoveries of trace elements ranging 84.0 – 95.6% for water samples and 75.0 – 120% for sediments. The As, Fe, Mn and Al concentrations obtained were further assessed for safe drinking water, irrigation water and for sediments quality about standard guidelines. Moreover, As species concentrations correlated with Fe, Mn and Al and the observed interactions depend on the adsorption capacities between As species and these trace elements. The inorganic species in water samples were also determined by employing off-line mode of solid phase extraction (SPE) procedure using multi-walled carbon nanotubes (MWCNTs) impregnated branched polyethyleneimine (BPEI) as an adsorbent material. The MWCNTs-BPEI characterised with X-ray powder diffraction (XRD), Fourier transform infrared (FTIR) spectroscopy and Thermogravimetric analysis (TGA) techniques indicated successful modification of the nanomaterial. The MWCNTs-BPEI exhibited selective retention of As5+ in the presence of As3+ in water samples with the achieved pre-concentration factor of 23.3. The retained As5+ was then eluted and detected using ICP-MS. A limit of detection (LOD) of 0.0537 μg/L and limit of quantification (LOQ) of 0.179 μg/L were achieved. The obtained percentage recovery of 81.0% validated the SPE procedure for selective retention of As5+. The As5+ concentrations determined after the SPE procedure were found in the range of 0.204 – 7.52 μg/L, which are in good agreement with As5+ results obtained using HPLC-ICP-MS.