Bepaling van spoorelemente in uraanertse met behulp van X-straalfluoressensie-spektrometrie
- Authors: De Villiers, Wessel van Zyl
- Date: 2014-04-10
- Subjects: Uranium ores , Fluorescence spectroscopy , X-ray spectroscopy , Trace elements - Analysis
- Type: Thesis
- Identifier: uj:10538 , http://hdl.handle.net/10210/10064
- Description: M.Sc. (Chemistry) , The determination of 17 trace elements (As. Ba. Co. Cr. Cu. Mo. Nb. Ni. Pb. Rb. Sr. Th. U. V. Y. Zn and Zr) in uranium ores by X-ray fluorescence spectrometry was investigated in this study. The determination of major elements. however. was also necessary for the calculation of mass absorption coefficients. Major elements were determined on borate melts and trace elements on powder briquettes pressed at 7 t with a binder in liquid form. Initially a method was developed for the determination of the elements of interest in unmineralised rocks The rhodium tube was used for the Group 1 elements (As. Mo. Nb. Pb, Bb, Sr. Th, U. Y and Zr) and the gold tube for the Group 2 elements [Ba, Co. Cr. Cu. Ni. V and Zn). Background and peak overlap corrections were made by means of background and interference factors. Corrections for absorption of radiation by the sample were made by means of mass absorption coefficients. which were calculated from the major element composition or obtained from the relation between the inverse of the mass absorption coefficient and the intensity of the Compton scattering peak. Due to various problems. only the latter method was suitable for uranium ores. The high uranium content in uranium ores mainly affected the Group 1 elements. Because of the high intensity of various UL lines. large overlap corrections were necessary. while only a few completely interference-free background positions were available. Consequently. the Feather and Willis method was used for determining the background intensity at the peak positions as well as for mass absorption coefficients. As a result of the presence of the UL absorption edges both primarx and secondary mass absorption coefficients had to be used for matrix corrections. Furthermore. it was observed that the background intensity in the region of the uranium lines increases with increasing uranium content of the sample instead of the expected decrease due to the increasing mass absorption coefficient. This effect was greater for the LiF(11 0) crystal than for the LiF(100) and was attributed to the scattering of uranium lines in the spectrometer chamber. especially from the crystal. A method was developed to correct the measured intensities for this scattering effect. Calibration lines of the contribution from the scattering of uranium lines to the measured intensity at the different 28 positions versus the uranium peak intensity were plotted by using samples with various uranium concentrations (<2 %) and for which the mass absorption coefficients and concentrations of the various elements were known. The precision of the method was less than 2.5 % at concentrations greater than 50 ppm. With the exception of barium. detection limits varied between 1 and 5 ppm. Accurate results were obtained over large concentration ranges for various unmineralised samples and for uranium ores. The results of the analysis of a number of Karoo uranium ores are given.
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- Authors: De Villiers, Wessel van Zyl
- Date: 2014-04-10
- Subjects: Uranium ores , Fluorescence spectroscopy , X-ray spectroscopy , Trace elements - Analysis
- Type: Thesis
- Identifier: uj:10538 , http://hdl.handle.net/10210/10064
- Description: M.Sc. (Chemistry) , The determination of 17 trace elements (As. Ba. Co. Cr. Cu. Mo. Nb. Ni. Pb. Rb. Sr. Th. U. V. Y. Zn and Zr) in uranium ores by X-ray fluorescence spectrometry was investigated in this study. The determination of major elements. however. was also necessary for the calculation of mass absorption coefficients. Major elements were determined on borate melts and trace elements on powder briquettes pressed at 7 t with a binder in liquid form. Initially a method was developed for the determination of the elements of interest in unmineralised rocks The rhodium tube was used for the Group 1 elements (As. Mo. Nb. Pb, Bb, Sr. Th, U. Y and Zr) and the gold tube for the Group 2 elements [Ba, Co. Cr. Cu. Ni. V and Zn). Background and peak overlap corrections were made by means of background and interference factors. Corrections for absorption of radiation by the sample were made by means of mass absorption coefficients. which were calculated from the major element composition or obtained from the relation between the inverse of the mass absorption coefficient and the intensity of the Compton scattering peak. Due to various problems. only the latter method was suitable for uranium ores. The high uranium content in uranium ores mainly affected the Group 1 elements. Because of the high intensity of various UL lines. large overlap corrections were necessary. while only a few completely interference-free background positions were available. Consequently. the Feather and Willis method was used for determining the background intensity at the peak positions as well as for mass absorption coefficients. As a result of the presence of the UL absorption edges both primarx and secondary mass absorption coefficients had to be used for matrix corrections. Furthermore. it was observed that the background intensity in the region of the uranium lines increases with increasing uranium content of the sample instead of the expected decrease due to the increasing mass absorption coefficient. This effect was greater for the LiF(11 0) crystal than for the LiF(100) and was attributed to the scattering of uranium lines in the spectrometer chamber. especially from the crystal. A method was developed to correct the measured intensities for this scattering effect. Calibration lines of the contribution from the scattering of uranium lines to the measured intensity at the different 28 positions versus the uranium peak intensity were plotted by using samples with various uranium concentrations (<2 %) and for which the mass absorption coefficients and concentrations of the various elements were known. The precision of the method was less than 2.5 % at concentrations greater than 50 ppm. With the exception of barium. detection limits varied between 1 and 5 ppm. Accurate results were obtained over large concentration ranges for various unmineralised samples and for uranium ores. The results of the analysis of a number of Karoo uranium ores are given.
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Chemical characterisation of atmospheric aerosols in Soweto, Bethlehem and Thohoyandou using energy dispersive x-ray fluorescence spectroscopy and ion chromatography
- Authors: Lumka, Mandisile
- Date: 2012-03-05
- Subjects: Aerosols , X-ray spectroscopy , Ion exchange chromatography
- Type: Thesis
- Identifier: uj:2123 , http://hdl.handle.net/10210/4491
- Description: M.Sc. , Aerosol samples were collected at stations using simple filter unit, loaded with a 4 7 mm diameter pore size Nuclepore membrane filter. The sampling duration was 24 hours for each sample, with the total of 11 samples: seven for Thohoyandou and four for Bethlehem. The samples were analyzed with energy dispersive X-ray fluorescence spectrometry for up to 20 elements. Comparison for elemental concentrations of the data showed that the samples fall into three clusters on average (major: Ca, Cl, Si. S, Fe and AI; intermediate: K, Ti, Pb, Brand Zn; minor: Mn, Cr, As, Sr, Ni and Cu), with the samples collected from Bethlehem having high concentrations in all clusters. High concentrations in the samples collected on Bethlehem were attributed to entrainement of dust particles during the dry winter period. The results also show that the elements are associated with anthropogenic emissions. Therefore, the sampling station at Thohoyandou is considered as a background station due to the low aerosol concentration. The aerosol concentration levels at Thohoyandou can be attributed to biogenic sources because of the large presence of large forest areas in the region and in the vicinity of the sampling location. The samples collected in both regions reveal highly enriched sulphur, chlorine, zinc and lead. It is clearly proved that these elements come from local soil. Chromium and copper were both slightly enriched in Thohoyandou, but the concentration data for these two elements are not available. However it is supposed that these elements come from local soil as well. In another aerosol analysis, passive (diffusive) samplers were used to measure concentration levels for sulphur dioxide and nitrogen dioxide. The measurement campaign was carried out from Soweto in Johannesburg and Bohlokong in Bethlehem with the campaign lasting for two months during the w~nter season. A very clear result derived for sulphur dioxide was the dominating source contribution from use of coal for heating and cooking in both areas. For nitrogen dioxide, it was found that contribution from traffic in highly populated areas and from industrial activities in the neighbourhood of the two areas was the source. The role played by wood burning, is also another additional source used for domestic heating and even cooking.
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- Authors: Lumka, Mandisile
- Date: 2012-03-05
- Subjects: Aerosols , X-ray spectroscopy , Ion exchange chromatography
- Type: Thesis
- Identifier: uj:2123 , http://hdl.handle.net/10210/4491
- Description: M.Sc. , Aerosol samples were collected at stations using simple filter unit, loaded with a 4 7 mm diameter pore size Nuclepore membrane filter. The sampling duration was 24 hours for each sample, with the total of 11 samples: seven for Thohoyandou and four for Bethlehem. The samples were analyzed with energy dispersive X-ray fluorescence spectrometry for up to 20 elements. Comparison for elemental concentrations of the data showed that the samples fall into three clusters on average (major: Ca, Cl, Si. S, Fe and AI; intermediate: K, Ti, Pb, Brand Zn; minor: Mn, Cr, As, Sr, Ni and Cu), with the samples collected from Bethlehem having high concentrations in all clusters. High concentrations in the samples collected on Bethlehem were attributed to entrainement of dust particles during the dry winter period. The results also show that the elements are associated with anthropogenic emissions. Therefore, the sampling station at Thohoyandou is considered as a background station due to the low aerosol concentration. The aerosol concentration levels at Thohoyandou can be attributed to biogenic sources because of the large presence of large forest areas in the region and in the vicinity of the sampling location. The samples collected in both regions reveal highly enriched sulphur, chlorine, zinc and lead. It is clearly proved that these elements come from local soil. Chromium and copper were both slightly enriched in Thohoyandou, but the concentration data for these two elements are not available. However it is supposed that these elements come from local soil as well. In another aerosol analysis, passive (diffusive) samplers were used to measure concentration levels for sulphur dioxide and nitrogen dioxide. The measurement campaign was carried out from Soweto in Johannesburg and Bohlokong in Bethlehem with the campaign lasting for two months during the w~nter season. A very clear result derived for sulphur dioxide was the dominating source contribution from use of coal for heating and cooking in both areas. For nitrogen dioxide, it was found that contribution from traffic in highly populated areas and from industrial activities in the neighbourhood of the two areas was the source. The role played by wood burning, is also another additional source used for domestic heating and even cooking.
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Minimising uncertainty in measurement and improving limit of detection in gold bearing materials from concentrations predicted by linear regression in atomic absorption spectrometry
- Authors: Fraser, Allan William
- Date: 2015-11-09
- Subjects: Gold - Assaying , Gold - Analysis , X-ray spectroscopy
- Type: Thesis
- Identifier: uj:14527 , http://hdl.handle.net/10210/15057
- Description: M.Sc. (Geology) , Refer to full text for abstract
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- Authors: Fraser, Allan William
- Date: 2015-11-09
- Subjects: Gold - Assaying , Gold - Analysis , X-ray spectroscopy
- Type: Thesis
- Identifier: uj:14527 , http://hdl.handle.net/10210/15057
- Description: M.Sc. (Geology) , Refer to full text for abstract
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