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Made available in DSpace on 2014-10-09T12:53:19Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T13:58:38Z (GMT). No. of bitstreams: 0 / O trabalho desenvolvido teve com objetivos demonstrar se houve alteração no crescimento de UFC em placa e na viabilidade (método DF-BE) de leveduras e bactérias totais quando o fermento biológico seco foi tratado por diferentes doses de radiação gama e armazenado sob diferentes tempos de estocagem, determinar a dose D10 para bactérias Totais e Leveduras neste produto e analisar se o processamento deste produto promoveu algum beneficio sem causar inviabilidade do mesmo. As diferentes amostras de fermento biológico foram irradiadas com doses de 0 (controle); 0,5; 1; 2 e 3kGy no Centro de Tecnologia das Radiações do (IPEN/CNEN – SP) em fonte de 60Co (Gammacell-220), com taxa de dose de 3,51kGy/h. Após este procedimento amostras referentes a cada dose de radiação foram destinadas à análise microbiológica e ao teste de viabilidade enquanto as demais amostras foram armazenadas a temperatura ambiente (23ºC). O aumento da dose de radiação provocou uma diminuição na contagem de UFC de leveduras, UFC de bactérias totais e também na freqüência de células viáveis de leveduras, evidenciadas pelo método fluorescente DF-BE. Além da radiação o tempo de armazenamento também influenciou na redução da contagem de bactérias totais e na diminuição da freqüência de células viáveis. De acordo com a análise de regressão linear simples, a dose de radiação necessária para eliminar 90% da população leveduriforme ficou entre 1,10 e 2,23kGy e para a população bacteriana variou entre 2,31 e 2,95kGy. Nos resultados são demonstrados claramente os pontos negativos da aplicação de radiação ionizante em fermento biológico seco, pois o intervalo de D10 encontrado para bactérias totais é superior ao encontrado para leveduras. Sendo assim, torna-se inviável a utilização deste recurso para a melhora da qualidade do produto, visto que para reduzirmos consideravelmente a população bacteriana necessariamente temos que diminuir a população leveduriforme. Com a redução das leveduras iremos alterar significativamente a qualidade e a viabilidade do produto. / Dissertação (Mestrado) / IPEN/D / Instituto de Pesquisas Energéticas e Nucleares - IPEN-CNEN/SP

Made available in DSpace on 2014-10-09T12:35:08Z (GMT). No. of bitstreams: 0 / Made available in DSpace on 2014-10-09T14:00:33Z (GMT). No. of bitstreams: 0 / O processo de conformação por prensagem uniaxial é um dos mais utilizados na indústria cerâmica devido ao seu baixo custo e alta produtividade. O entendimento e controle dos diversos fatores que interferem neste processo são cruciais, pois grande parte dos defeitos encontrados na peça final é originada nesta etapa. Este trabalho trata da avaliação da compactação de pós a base de alumina processados em spray-dryer, com diferentes composições e contendo distintos aditivos orgânicos, sendo caracterizados em relação a fluidez, densidade solta e batida, determinação da distribuição do tamanho de grânulos e morfologia. Parâmetros como umidade (10, 64 e 85%) e temperatura (5, 25 e 45°C) foram variados. O comportamento do pó foi analisado nas diferentes etapas de compactação, as quais envolvem a deformação plástica e quebra dos grânulos e também redução da porosidade intergranular e intragranular. Posteriormente foram estudadas a influência da temperatura e da umidade relativa do ar durante a compactação, sendo o efeito dos mesmos avaliados por meios de curvas de compactação. A resistência mecânica das peças também foi avaliada por meio do módulo de Weibull. Através da análise da microestrutura (MEV e porosimetria) e de curvas de compactação constatou-se que os parâmetros citados acima interferem nas características dos compactados, particularmente na resistência mecânica dos grânulos em relação à deformação e fratura. Os resultados mais importantes são que quanto maior a temperatura e umidade ocorre a redução da Tg dos ligantes, diminuindo a resistência ao esmagamento dos mesmo e que através do módulo de Weibull é possível determinar qual a melhor condição para realizar a prensagem que no caso deste estudo foi a condição intermediária. / Dissertação (Mestrado) / IPEN/D / Instituto de Pesquisas Energeticas e Nucleares - IPEN-CNEN/SP

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Despite the significant progress in medicine, infectious diseases are life-threatening thanks to an increasing number of multiresistant strains of microorganisms and late detection of pathological agents. An opportunistic fungus Aspergillus fumigatus cause respiratory system diseases called aspergillosis. The invasive pulmonary aspergillosis affects immunocompromised patients after inhalation of ubiquitous conidia of A. fumigatus and results in 450,000 deaths per year. The biofilm formation in the infected tissue protects A. fumigatus against antimicrobial drugs. Late therapy may not be effective. Infection of immunocompromised patients and biofilm formation is characteristic also for gram negative bacteria Pseudomonas aeruginosa, which is due to the production of many factors of virulence and multiresistance a dreaded opportunistic pathogen. Scanning electron microscopy (SEM) provides detail information about morphology of microorganisms with the resolution in range of tens of nanometers that allows to observe microorganisms in the infected tissue and its pathological changes. Mass spectrometry allows to detect infection and its course based on identification of characteristic microbial molecules. The aim of this study was to optimize sample preparation of tissues infected with A. fumigatus or P....

<p> A textural and mineralogical study of the magnetite, hemoilmenite and minor sulfide phases of the Whitestone anorthosite, Dunchurch, Ontario, was carried out. The composition of magnetite and hemo-ilmenite was determined by chemical analysis, X-ray diffraction and electron probe microanalysis. A modification of the solvus shape in the hematite-ilmenite system consistent with the composition of hemo-ilmenite lamellae, as well as a mechanism for formation of metamorphic magnetite porphyroblasts from ferrianilmenite is proposed. Buddington and Lindsley's experimental data cannot be used directly to obtain f02 and T of formation of the anorthosite because compositions fall in the highly oxidizing and as yet undetermined portion of their diagram. </p> / Thesis / Master of Science (MSc)

Platinum-based catalysts for hydrogen fuel-cell applications have progressed greatly with the addition of a second element in either a mixed-alloy or core-shell structure. Not only do they contain a reduced amount of the more expensive platinum metal but they have been shown to demonstrate a significant improvement in catalytic activity. Further improvement of these systems can only be made by careful investigation of such catalyst panoparticles on an atomic scale. These nanoparticles provide a significant characterisation challenge due to their minute size and beam sensitivity. A new method of quantifying the annular dark-field (ADF) scanning transmission electron microscope (STEM) signal on an absolute scale has been developed to address this problem. Experimental images are scaled to a fraction of the incident beam intensity from a detector map. The integrated intensity of each individual atomic column is multiplied by the pixel area to yield a more robust imaging parameter: a scattering cross section, &sigma;. Using this cross section approach and simulated reference data, I show it is possible to count the number of atoms in individual columns. With some prior knowledge of the sample, this makes it possible to reconstruct the 3-dimensional structures of pure platinum nanoparticles. Such an approach has subsequently been extended to bimetallic particles here the elements are close in atomic number, using the platinum-iridium system as an example. In the same way that the cross section can be calculated from ADF image intensity, it is possible to calculate an energy dispersive x-ray (EDX) partial scattering cross section, beneficial especially because of the simplicity of its implementation. In sufficiently thin samples such that the number of x-ray counts is linearly proportional to sample thickness, we can determine element-specific atom counts. Finally, it is possible to combine EDX and ADF cross sections to provide us with quantitative structural and compositional information.

Solid state chemical storage of hydrogen in metals offers promising advantages over compressed hydrogen gas and condensed liquid hydrogen, especially for mobile applications with respect to safety and energy efficiency. However, no single metal hydride simultaneously satisfies the essential performance criteria for onboard hydrogen storage namely, high gravimetric and/or volumetric energy density, fast kinetics and favorable thermodynamics. Recently, a breakthrough achievement was made by the development of reactive hydride composites in which two metal hydride systems (e.g. NaBH₄ and MgH₂) are mixed together resulting in better sorption properties than the individual pure systems. In this approach, the formation of MgB₂ by exothermic reaction destabilizes the composite and consequently reduces the overall enthalpy and sorption temperature of the endothermic desorption reaction. In this work the thermodynamic and kinetic properties of reactions in 2NaH + MgB₂ + 4H₂ &harr; 2NaBH₄ + MgH₂ and 3NaH + MgB₂ + 4H₂ &harr; 2NaBH₄ + NaMgH₃ were established using multiple experimental techniques like volumetric measurements, ex-situ and in-situ X-ray diffraction, calorimetry, and especially electron microscopy. Under the applied experimental conditions of 50 bar hydrogen and 400 &deg;C during the hydrogenation of 2NaH + MgB2 and 0.1 bar hydrogen and 450 &deg;C during the dehydrogenation of 2NaBH₄ + MgH₂, both reactions were kinetically limited and proceeded in multisteps. The absorption reaction was partial, being restricted by the unexpected formation of NaMgH₃ which limits the formation of NaBH₄ while the desorption reaction was complete and limited by the growth of MgB₂ through some intermediate complexes at the Mg/NaBH₄ interface where the intermediate phase forms a barrier to diffusion. Conversely, in the 3NaH + MgB₂ system, absorption in 100 bar hydrogen and 300 &deg;C was complete but slow, while in the 2NaBH₄ + NaMgH₃ system, complete desorption was achieved in multisteps under 0.1 bar hydrogen and 450 &deg;C. The formation of intermediate and stable complexes during these reactions poses a significant restraint to hydrogen sorption reactions. However, lower onset sorption temperatures have been established in these systems than in the pure compounds due to their simultaneous destabilization in the composite state. This study have demonstrated the complexity of desorption and absorption mechanisms in these composite systems and the difficulty of obtaining such reactions at low temperatures required for mobile applications. This understanding of the rate limiting reaction steps in reactive hydride composites provides the basis for further optimization of these materials for efficient hydrogen storage applications.

L'analyse par microsonde électronique (EPMA) permet de quantifier, avec une grande précision, les concentrations élémentaires d'échantillons de compositions inconnues. Elle permet, par exemple, de quantifier les actinides présents dans les combustibles nucléaires neufs ou irradiés, d'aider à la gestion des déchets nucléaires ou encore de dater certaines roches. Malheureusement, ces analyses quantitatives ne sont pas toujours réalisables dû à l'indisponibilité des étalons de référence pour certains actinides. Afin de pallier cette difficulté, une méthode d'analyse dite « sans standard » peut-être employée au moyen d'étalons virtuels. Ces derniers sont obtenus à partir de formules empiriques ou à partir de calculs basés sur des modèles théoriques. Toutefois, ces calculs requièrent la connaissance de paramètres physiques généralement mal connus, comme c'est le cas pour les sections efficaces de production de rayons X. La connaissance précise de ces sections efficaces est requise dans de nombreuses applications telles que dans les codes de transport de particules et dans les simulations Monte-Carlo. Ces codes de calculs sont très utilisés en médecine et particulièrement en imagerie médicale et dans les traitements par faisceau d'électrons. Dans le domaine de l'astronomie, ces données sont utilisées pour effectuer des simulations servant à prédire les compositions des étoiles et des nuages galactiques ainsi que la formation des systèmes planétaires.Au cours de ce travail, les sections efficaces de production des raies L et M du plomb, du thorium et de l'uranium ont été mesurées par impact d'électrons sur des cibles minces autosupportées d'épaisseur variant de 0,2 à 8 nm. Les résultats expérimentaux ont été comparés avec les prédictions théoriques de sections efficaces d'ionisation calculées grâce à l'approximation de Born en ondes distordues (DWBA) et avec les prédictions de formules analytiques utilisées dans les applications pratiques. Les sections efficaces d'ionisation ont été converties en sections efficaces de productions de rayons X grâce aux paramètres de relaxation atomique extraits de la littérature. Les résultats théoriques du modèle DWBA sont en excellents accords avec les résultats expérimentaux. Ceci permet de confirmer les prédictions de ce modèle et de valider son utilisation pour le calcul de standards virtuels.Les prédictions de ce modèle ont été intégrées dans le code Monte-Carlo PENELOPE afin de calculer l'intensité de rayons X produite par des standards pur d'actinides. Les calculs ont été réalisés pour les éléments dont le numéro atomique est 89 ≤ Z ≤ 99 et pour des tensions d'accélération variant du seuil d'ionisation jusque 40 kV, par pas de 0,5 kV. Pour une utilisation pratique, les intensités calculées pour les raies L et M les plus intenses ont été regroupées dans une base de données.Les prédictions des standards virtuels ainsi obtenus ont été comparées avec des mesures effectuées sur des échantillons de composition connue (U, UO2, ThO2, ThF4, PuO2…) et avec les données acquises lors de précédentes campagnes de mesures. Le dosage des actinides à l'aide de ces standards virtuels a montré un bon accord avec les résultats attendus. Ceci confirme la fiabilité des standards virtuels développés et démontre que la quantification des actinides par microsonde électronique est réalisable sans standards d'actinides et avec un bon niveau de confiance. / Electron probe microanalysis (EPMA) is used to quantify with a high accuracy the amount of different elements present on a sample of unknown composition. EPMA is largely used to quantify the amount of actinides present in fresh and irradiated fuels, to manage waste disposal and to date rocks. However, quantitative EPMA is not always possible to achieve for these materials due to the lack of suitable reference standards for the radionuclides. To overcome this difficulty, standardless methods of analysis are employed with mean of virtual calculated standards. These calculated standards are generally obtained from empirical formulae based on experimental extrapolations or from theoretical calculations that require physical parameters which are poorly known as it is the case for the X-ray production cross section.The accurate knowledge of these cross sections is required in many applications such as in particle transport code and in Monte Carlo simulations. The computer simulations are widely used in the medical field and particularly in medical imaging and in electron beam therapy. In the field of astronomy, these data are used to perform simulations that predict the compositions of stars and galactic clouds, and the formation of planetary systems.In the present work, L- and M-shell absolute x-ray production cross sections were determined experimentally for elements lead, thorium and uranium by electron impact using ultrathin self-supporting targets with thickness varying from 0.2 to 8 nm. The measured cross sections have been compared, with the distorted-wave Born approximation (DWBA) calculated by Bote et al. and with the predictions of analytical formulae widely used in practical applications. For the conversion of inner-shell ionization cross sections into x-ray production cross sections, atomic relaxation parameters were extracted from the literature. The predictions of the DWBA calculations are in excellent agreement with our measured x-ray production cross sections. This confirms the predictive results of this model and its usefulness for the calculation of virtual standards.The DWBA calculations were used into the Monte Carlo simulation code PENELOPE to calculate the X-ray intensity produced by pure actinide standards. The X-ray intensities were calculated for elements with atomic number 89 ≤ Z ≤ 99 and for accelerating voltage ranging from the ionization threshold up to 40 kV with a step of 0.5 kV. For a practical use, the calculated intensities for the most intense L and M lines were stored in a database.The predictions of our calculated standards have been compared with the x-ray intensity of known composition actinide samples (such as U, UO2, ThO2, ThF4, PuO2…) and with the data acquired during previous measurement projects. Actinide quantifications performed by virtual standards were found to be in fair agreement with the expected results. This confirms the reliability of the developed virtual standards and demonstrates that actinide quantification by EPMA can now be possible to perform without material actinide standards and with a good level of accuracy.

<p>Cystic fibrosis (CF) is the most common lethal genetic disease in the white population. It is due to mutations in the gene coding for the cystic fibrosis transmembrane conductance regulator (CFTR), a protein that functions mainly as a cAMP-activated chloride channel. The disease impairs ion and water transport in epithelia-lined organs such as airways, digestive tract, reproductive epithelium and sweat glands. At present the only therapy is symptomatic and development of curative treatment depends on uncovering the links between the defective CFTR and the disease, as well as on improving end-point measurements. </p><p>A method has been established for studying ion transport in an easily accessible cell type (nasal epithelial cells) from normal and cystic fibrosis patients by X-ray microanalysis. This method represents a rather simple and direct way of measuring simultaneously several chemical elements of biological interest.</p><p>Studies of chloride transport by means of a fluorescent indicator (MQAE) in nasal epithelial cells from CF patients showed that the phenotype cannot exclusively be explained by the CFTR activity in patients with severe genotype. </p><p>A common Portuguese CFTR mutation (A561E) causes protein mislocalization in the endoplasmic reticulum similar to the most common CF mutation (ΔF508) and thus it should be possible to treat it with the same pharmacological strategies.</p><p>Chronic treatment of CF airway epithelial cells with nanomolar concentrations of colchicine increased the chloride efflux via chloride channels other than CFTR, strengthening the notion that colchicine could be beneficial to CF patients.</p><p>Successful <i>in vitro </i>transfection of CF airway epithelial cells with cationic vectors was possible with short incubation times. Heparin added at the end of the transfection incubation time could help to maintain the viability of the cells, without interfering with the transfection efficiency. It seems possible that heparin could be an adjuvant for non-viral mediated gene therapy.</p>