Made available in DSpace on 2014-10-09T12:38:08Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:04:39Z (GMT). No. of bitstreams: 1 05649.pdf: 6795207 bytes, checksum: c03839663e599700ba2154bbedff9b1c (MD5) / Dissertacao (Mestrado) / IPEN/D / Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP

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Made available in DSpace on 2014-10-09T12:48:36Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T13:57:51Z (GMT). No. of bitstreams: 1 09249.pdf: 8213081 bytes, checksum: e62b849d5f56043393427a2373a3d1d5 (MD5) / Tese (Doutoramento) / IPEN/T / Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP

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Submitted by Claudinei Pracidelli (cpracide@ipen.br) on 2016-04-08T12:24:41Z No. of bitstreams: 0 / Made available in DSpace on 2016-04-08T12:24:41Z (GMT). No. of bitstreams: 0 / Dissertação (Mestrado em Tecnologia Nuclear) / IPEN/D / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

Submitted by Claudinei Pracidelli (cpracide@ipen.br) on 2016-04-08T12:24:41Z No. of bitstreams: 0 / Made available in DSpace on 2016-04-08T12:24:41Z (GMT). No. of bitstreams: 0 / Os radionuclídeos naturais das séries radioativas do 238U, 235U e 232Th são frequentemente utilizados como traçadores em estudos ambientais para a compreensão da dinâmica que ocorre no ambiente marinho e terrestre, como por exemplo, em pesquisas de processos oceânicos e gerenciamento da região costeira. No ambiente marinho, estes radionuclídeos podem ser empregados para estimar fluxos biogeoquímicos de partículas e de nutrientes que ocorrem tanto na coluna dágua, quanto nos sedimentos. Várias pesquisas aplicam a distribuição e o respectivo desequilíbrio dos radionuclídeos naturais no meio ambiente, inclusive em modelos geocronológicos para se obter informações históricas em testemunhos sedimentares. Nesse estudo, realizou-se a caracterização radioquímica das distribuições de 226Ra, 228Ra e 210Pb de uma coluna sedimentar denominada 1B (248 cm de comprimento), coletada na Baía do Almirantado, Antártica. A metodologia utilizada incluiu a lixiviação ácida de amostras de sedimentos, seguida de separação radioquímica sequencial de 226Ra e de 228Ra pela co-precipitação com Ba(Ra)SO4 e de 210Pb pela co-precipitação com PbCrO4. Todas as medidas foram realizadas pela contagem alfa e beta total dos precipitados obtidos, em um detector proporcional de fluxo gasoso de baixa radiação de fundo. As concentrações de atividade de 226Ra e 210Pb foram empregadas para se estimar a atividade de 210Pbnão-suportado presentes no perfil sedimentar 1B. Considerando-se as concentrações de atividade de 210Pbnão-suportado obtidas e a aplicação do modelo CIC(Constant Initial Concentration), foi possível determinar a taxa de sedimentação de 0,59±0,05 cm/ ano. / Dissertação (Mestrado em Tecnologia Nuclear) / IPEN/D / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

Methods for the determination of the actinide elements in water, biological, soil and sediment samples have been developed using on-line solid phase extraction and high performance liquid chromatography (HPLC) coupled with inductively coupled plasma mass spectrometry (ICP-MS). Initial applications utilised a commercially available resin, namely TRU-Spec resin, for efficient removal of the matrix prior to elution of uranium and thorium analytes. Comparative analyses of reference materials and natural water samples from Plymouth and Dartmoor demonstrated significant improvement in precision and speed of analysis by using TRU-Spec coupled to ICP-MS compared with alpha spectrometry. Further applications of the TRU-Spec resin for the determination of the transuranic actinide elements neptunium, plutonium and americium, resulted in the successful determination of 239Pu and 237Np in biological reference materials. Detection limits were 700, 850, and 600 attograms (ag) for 237Np, 233Pu, and 241Am, respectively, for a 0.5 ml sample injection, and better than 200 ag/g with 50 ml pre-concentration when sector field (SF) ICP-MS was used. A method for the selective sequential elution of uranium and plutonium was also developed to facilitate the determination of 239Pu without interference due to the 238U1H+ polyatomic ion, caused by high concentrations of 238U in sediment samples. Investigations were performed into the use of a polymeric substrate, which was dynamically coated with chelating dyes such as xylenol orange and 4-(2-pyridylazo) resorcinol, and a silica substrate coated with permanently bonded iminodiacetic acid. The latter was used for the successful determination of uranium and thorium in certified reference material waters. However, the column was found to have a high affinity for iron, making it unsuitable for the determination of the actinides in soil and sediment samples. Subsequently, a polystyrene substrate which was dynamically coated with dipicolinic acid was used for HPLC coupled with SF-ICP-MS. Using this column it was possible to separate the various actinides from each other and from the matrix. In particular, it was possible to separate plutonium and uranium to facilitate interference-free determination of the former. The column also exhibited some selectivity for different oxidation states of Np, Pu and U. Two oxidation states each for plutonium and neptunium were found, tentatively identified as Np(V) and Pu(III) eluting at the solvent front, and Np(IV) and Pu(IV) eluting much later. Detection limits were 12, 8, and 4 fg for 237Np, 239Pu, and 241Am, respectively, for a 0.5 ml injection, and the system was successfully used for the determination of 239Pu in water, biological and soil reference materials.