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Trace metal and speciation analysis using ion-exchange and energy dispersive X-ray fluorescence spectrometryMenendez-Alonso, Elena January 2000 (has links)
Studies have been carried out on specific ion-exchange (Dowex 50W-X8 and Dowex 1-X8) and chelation (Chelex-100) resins, in order to determine their physical and chemical characteristics, to understand and explain their limits of function and to optimise their use as substrates in trace metal and speciation measurement by EDXRF. Structural information was obtained by scanning electron microscopy and x-ray microanalysis showing a homogeneous distribution of functional groups and retained ions on both sectioned and whole resins. Particle size experiments performed on Dowex 50W-X8 (38 - 840 µm) showed that this parameter has no effect on the relationship between intensity of fluorescence and concentration or mass of resin. Inter-element effects were not observed in the analysis of multielemental specimens prepared on ion-exchange / chelation media by EDXRF. This indicates that the proposed method has a significant advantage when compared with other methodologies. A theoretical ‘model’, based on the formation of thin films on the surface of the resin beads, has been proposed in order to link and explain the effects observed in these experiments. The use of a batch retention system has shown distinct advantages over using columns in terms of linearity, accuracy, precision, rapidity and simplicity. Parameters such as pH and ionic strength of the solution, concentration of competing ions and volume of the sample have been proven to be critical. The maximum retention capacity has been determined as 3.2, 1.1 and 0.67 mEq/g for Dowex 50W-X8, Dowex 1-X8 and Chelex-100 respectively. The optimum mass of resin for XRF analysis was found to be 0.5 g, for all resins tested. The linear range covered 4 to 5 orders of magnitude. These findings show the potential of the investigated media to overcome instrumental and sample limitations. Based on the physico-chemical information found, methodologies for three different applications of the resins to EDXRF determinations have been developed and their analytical possibilities explored. The multi-elemental determination of metals in sewage sludge digests was achieved by retaining the metals on Dowex 50W-X8 at pH 2 and Chelex-100 at pH 4. Chelex-100 allows quantitative recoveries for Cu and Zn. A wider range of elements was determined on Dowex 50W-X8, although with poorer recoveries (60 - 90%). The limits of detection were 10 - 21 µg when Dowex 50W-X8 was used and 8 - 49 µg for Chelex-100. The method was validated by the analysis of a certified material. The determination of Kβ/Kα intensity ratios for Cr and Mn species and its potential as a tool for direct elemental speciation has also been studied. A difference in Kβ/Kα between the oxidation states of the analytes was only observed during the analysis of solutions of the metal species by EDXRF at the 98% level of confidence. Finally, the speciation and preconcentration of Cr(III) and Cr(VI) in waters has been performed by retention on Dowex 50W-X8 and Dowex 1-X8 followed by EDXRF determination. Efficient recoveries and preconcentration factors of up to 500 were achieved, leading to limits of detection of 30 µg/L for Cr(VI) and 40 µg/L for Cr(III). This method is simple, fast and inexpensive, allowing quantitative recoveries in the speciation of chromium in waste waters.
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Serrapilheira aplicada como biomonitor na avaliação do bosque urbano do Instituto de Pesquisas Energéticas e Nucleares, São Paulo, SP / Litterfall as biomonitors applied the evaluation of urban forest of the Nuclear and Energy Research Institute, São Paulo, SPCOELHO, JOAQUIM M.S. 09 October 2014 (has links)
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Investigação do processo de obtenção de aluminatos de bário e cálcio para construção e caracterização de catodos termiônicos impregnados para a aplicação em dispositivos de microondas de potênciaHIGASHI, CRISTIANE 09 October 2014 (has links)
Made available in DSpace on 2014-10-09T12:52:11Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T13:57:49Z (GMT). No. of bitstreams: 0 / Dissertacao (Mestrado) / IPEN/D / Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP
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Estudo da formação de fases secundárias no compósito LSM/YSZRODRIGUES, RANIERI A. 09 October 2014 (has links)
Made available in DSpace on 2014-10-09T12:53:18Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T13:59:02Z (GMT). No. of bitstreams: 0 / Dissertação (Mestrado) / IPEN/D / Instituto de Pesquisas Energéticas e Nucleares - IPEN-CNEN/SP
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Caracterização de silicatos e carbonatos de cálcio aplicados à dosimetria de doses altas / Characterization of silicates and calcium carbonates applied to high-dose dosimetryVILA, GUSTAVO B. 09 October 2014 (has links)
Made available in DSpace on 2014-10-09T12:35:56Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T13:59:32Z (GMT). No. of bitstreams: 0 / Tese (Doutoramento) / IPEN/T / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP
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Utilização da escória de alumínio na fabricação de argila expandidaTAKAHASHI, ELISA A.N. 09 October 2014 (has links)
Made available in DSpace on 2014-10-09T12:52:10Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:01:02Z (GMT). No. of bitstreams: 0 / Dissertacao (Mestrado) / IPEN/D / Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP
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Obtenção de fritas vitroceramicas a partir de resíduos sólidos industriaisFERREIRA, MATHEUS C. 09 October 2014 (has links)
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Emprego da fluorescencia de raios X por dispersao de energia no estudo da dinamica da vinhaca no soloSIMABUCO, SILVANA M. 09 October 2014 (has links)
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Caracterizacao qualitativa e quantitativa de elementos pela tecnica de fluorescencia de raios X em suplementos minerais para animaisZUCCHI, ORGHEDA L.A.D. 09 October 2014 (has links)
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Separação de efeitos de sobreposição de espectros obtidos por WDXRF usando o método de RietveldSALVADOR, VERA L.R. 09 October 2014 (has links)
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