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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.

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Made available in DSpace on 2014-10-09T12:52:19Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:00:31Z (GMT). No. of bitstreams: 0 / Os pára-raios radioativos foram fabricados no Brasil até 1989, quando a Comissão Nacional de Energia Nuclear (CNEN) suspendeu a concessão de uso de material radioativo nesses artefatos. Desde então, o pára-raios radioativo tem sido substituído por outro, do tipo Franklin, e recolhido como rejeito radioativo. Entretanto, apenas 23 % do total fabricado no país foram entregues à CNEN. Esta situação é preocupante, pois a chance, desses artefatos serem descartados como resíduo comum e chegarem a lixões, é grande, uma vez que, segundo dados do Instituto Brasileiro de Geografia e Estatística (IBGE), em 2000, 63,6 % dos municípios brasileiros dispunham o resíduo nesses locais. Além disso, o amerício, o radionuclídeo mais empregado, é classificado como sendo um elemento de alta toxicidade, quando ingerido ou inalado. No presente trabalho, foram realizados experimentos de migração de Am-241 em lisímetros, com o objetivo de se avaliar o risco de contaminação provocada por pára-raios radioativos descartados como resíduo comum. Fontes radioativas removidas de pára-raios foram inseridas em lisímetros preenchidos com resíduo orgânico, coletado no restaurante do Instituto de Pesquisas Energéticas e Nucleares, IPEN-CNEN/SP, e chorume gerado foi periodicamente analisado para determinar suas características como pH, potencial redox, teor de sólidos e a concentração do material radioativo. O crescimento microbiano também foi avaliado, pelo método de contagem direta do número de unidades formadoras de colônia. A estimativa de risco foi baseada no cálculo de dose para membros do público, sendo a ingestão de água a via mais provável de exposição. O valor obtido foi cerca de 1000 vezes inferior ao limite de dose anual estabelecido, pela Comissão Internacional de Proteção Radiológica (ICRP), demonstrando que o risco de contaminação provocado pelo descarte de pára-raios em lixões é baixo. / Tese (Doutoramento) / IPEN/T / Instituto de Pesquisas Energeticas e Nucleares - IPEN/CNEN-SP

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