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.
| Identifer | oai:union.ndltd.org:netd.ac.za/oai:union.ndltd.org:uj/uj:10538 |
| Date | 10 April 2014 |
| Creators | De Villiers, Wessel van Zyl |
| Source Sets | South African National ETD Portal |
| Detected Language | English |
| Type | Thesis |
| Rights | University of Johannesburg |
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