Les fluorures fondus sont utilisés dans les Réacteurs à Sels Fondus tels que le réacteur non modéré, à neutrons rapides, MSFR où le sel fondu LiF-ThF4 joue le rôle du combustible et du liquide caloporteur. La formation des produits de fissions (PF) tels que les lanthanides, au cours du fonctionnement de ce réacteur, peut modifier les propriétés physicochimiques du bain fondu. Il est ainsi important de caractériser le bain fondu de point de vue structural et dynamique afin de remonter à ses propriétés. En raison des problèmes de radioactivité liés au thorium, et des conditions requises liées aux méthodes spectroscopiques utilisées, le système étudié dans ce manuscrit est le LiF-ZrF4-LaF3 (le zirconium et le lanthane étant des PF potentiels). L'approche développée dans cette thèse combine des mesures par spectroscopies RMN et EXAFS à 850 °C avec des simulations de dynamique moléculaire. Dans le bain fondu, nous avons montré la coexistence de complexes à base de zirconium et de lanthane de différentes coordinences, dont les proportions et les interactions dépendent de la composition. En fonction de la teneur en ZrF4, les espèces [ZrF7]3- majoritaires évoluent peu mais se connectent davantage via des fluors pontants. L’ajout de LaF3 au mélange stabilise la coordinence 7 autour du zirconium et tend à enrichir l’environnement du lanthane en fluors. Un ordre à moyenne portée s’établit entre les différents complexes à base de zirconium et de lanthane par l’intermédiaire des fluors pontants. La dynamique des espèces est ralentie en fonction de l’ajout de ZrF4 et LaF3. Nous avons noté un effet important sur la structure et la dynamique des espèces à partir de 10% mol. LaF3 ajouté au mélange. Les données obtenues par cette approche originale de la chimie du bain fondu dans le RSF en présence des PF, sont fondamentales pour améliorer la séparation de ces derniers et optimiser le procédé. / Molten fluorides are used in Molten Salt Reactors MSR such as the non moderated fast reactor MSFR, where the molten salt LiF-ThF4 is the fuel and the coolant. The formation of fission products (FP) such as lanthanides, during the reactor operation, possibly modifies the physicochemical properties of the melt. It is therefore important to characterize the melt from the structural and the dynamics point of view in order to determine its properties. Because of problems related to the radioactivity of thorium, as well as requirements related to spectroscopic methods, the system studied in this thesis is the LiF-ZrF4-LaF3 (zirconium and lanthanum are possible FP). The approach followed in this thesis combines measurements by NMR spectroscopy and EXAFS at 850 °C with molecular dynamics simulations. In the molten salt, we have shown the existence of zirconium and lanthanum complexes with different coordination numbers, whose proportions depend on the composition. Depending on the content of ZrF4, [ZrF7]3- species are dominant but change slightly and are further connected between each other’s via bridging fluorine. The addition of LaF3 to the mixture stabilizes the 7 coordination number around the zirconium and tends to enrich the environment of lanthanum with fluorides. A medium-range order is established between the various complexes containing zirconium and lanthanum due to bridging fluorine. Species dynamics is slower when the amount of either ZrF4 or LaF3 is higher. We noted a significant effect on the structure and dynamics of species starting 10 mol%. LaF3 added to the medium. The data obtained by this novel approach concerning the chemistry of the molten salt in MSR containing FP, are fundamental to improve the separation of these products and optimize the process.

CoordenaÃÃo de AperfeiÃoamento de Pessoal de NÃvel Superior / Eugenia uniflora L. à um fruto tropical muito apreciado pelo seu sabor e aroma exÃticos. A pitangueira pertence à famÃlia das mirtÃceas, sendo facilmente cultivada em regiÃes de clima tropical e subtropical. O fruto apresenta coloraÃÃo que varia do laranja ao roxo, devido à presenÃa de pigmentos como carotenÃides e antocianinas. A pitanga possui um alto potencial econÃmico, no entanto, à muito vulnerÃvel à depreciaÃÃo quando madura, tornando-se necessÃrio a formulaÃÃo de produtos, visando um melhor aproveitamento tecnolÃgico. Dessa forma, este trabalho teve como objetivo avaliar as caracterÃsticas quÃmicas, fÃsico-quÃmicas, compostos bioativos e atividade antioxidante das polpas de pitanga de coloraÃÃes vermelha e roxa, desenvolver diferentes bebidas (refresco, nÃctar e suco tropical adoÃado) com polpa de pitanga roxa e avaliar suas caracterÃsticas microbiolÃgicas, sensoriais, quÃmicas e fÃsico-quÃmicas, bem como sua atividade antioxidante e principais compostos bioativos. As polpas de pitanga vermelha e roxa apresentaram caracterÃsticas quÃmicas e fÃsico-quÃmicas diferentes para todos os parÃmetros avaliados, exceto para a coordenada a*. A polpa roxa apresentou os maiores teores de compostos bioativos, exceto para a determinaÃÃo de carotenÃides totais, onde nÃo foi constatada diferenÃa significativa entre as polpas. Foram formuladas bebidas com teor de sÃlidos solÃveis fixados em 11ÂBrix e teor de polpa de 15% (refresco), 25% (nÃctar) e 35% (suco tropical adoÃado). O refresco, o nÃctar e o suco tropical apresentaram diferentes concentraÃÃes de vitamina C, carotenÃides totais, antocianinas totais, polifenÃis extraÃveis totais e atividade antioxidante total, sendo estes valores maiores na bebida com maior concentraÃÃo de polpa (suco tropical adoÃado). O nÃctar e o suco tropical apresentaram valores de acidez e aÃÃcares totais dentro dos limites fixados pela legislaÃÃo brasileira. As bebidas apresentaram condiÃÃes higiÃnico-sanitÃrias satisfatÃria. A avaliaÃÃo sensorial revelou que o refresco, o nÃctar e o suco tropical adoÃado apresentaram escores mÃdios entre a faixa de aceitaÃÃo e indiferenÃa para os testes de aceitaÃÃo e intenÃÃo de compra, com maiores notas para o nÃctar e o refresco. As maiores mÃdias atribuÃdas Ãs bebidas foram para os atributos cor e aparÃncia. A intenÃÃo de compra das bebidas parece ter sido influenciada pelos atributos sabor e doÃura. / Eugenia uniflora L. is a tropical fruit appreciated for its exotic flavor. Belonging to Myrtaceae family. It is cultivated easily in regions of tropical and subtropical climates. The fruits have colour ranges from orange to purple, due to the presence of pigments such as carotenoids and anthocyanins. The Surinam cherry has a high economic potential, but ripe fruits are vulnerable to depreciation, thus, it is necessary to formulate products with cherry pulp to stimulate a better use of technological fruit. Thus, the purpose of this study was evaluate the chemical and physicochemical characteristics in the pulps of red and purple colour and its antioxidant activity and content of bioactive compounds, develop different beverages (refreshment, nectar and tropical juice) with purple pulp, evaluate the microbiology, sensory, chemical and physicochemical characteristics, and its antioxidant activity and content of bioactive compounds. The pulps showed chemical and physicochemical characteristics different, excepting colour parametric a*. The purple pulp shower higher values of bioactive compounds, save the evaluation of carotenoids, that showed difference no significant. Was developing beverages with 11ÂBrix and 15% of pulp (refreshment), 25% de pulp (nectar) and 35% de pulp (tropical juice). The refreshment, nectar and tropical juice showed different values of vitamin C, carotenoids, anthocyanins, polyphenols and antioxidant activity, with higter values for the beverage with higter content of pulp (tropical juice). The tropical juice and nectar had values of acidity and total sugars within the limits established by Brazilian legislation. The fruit beverages showed hygienic and sanitary conditions. The sensory evaluation revealed that the refreshment, nectar and tropical juice had mean scores between the range of acceptance and indifference to the acceptance tests and purchase intent. The sensory parameters colour and appearances given the higher means. The attribute flavor and sweetness influenced the purchase intent.

O objetivo deste trabalho foi identificar, por meio de análise polínica de amostras de mel e cargas de pólen, a fonte dos recursos alimentares utilizados por cinco espécies de meliponíneos, numa área rural do município de Piracicaba, Estado de São Paulo, bem como acompanhar o desenvolvimento anual das colônias, além de determinar as características físico-químicas e microbiológicas de 31 amostras de mel produzido no local. Para tanto foram realizadas as análises de açúcares, umidade, HMF, proteínas, cinzas, pH, acidez, índice de formol, condutividade elétrica, cor, atividade diastásica, atividade de água e pesquisa de coliformes totais, fecais, fungos e leveduras. Os resultados demonstram que as espécies Tetragonisca angustula, Scaptotrigona bipunctata, Nanotrigona testaceicornis, Tetragona clavipes, com exceção de F. varia, são generalistas quanto ao uso dos recursos florais, e que o desenvolvimento de suas colônias é influenciado pelos fatores climáticos, necessitando de alimentação complementar em períodos de queda da temperatura, chuvas ou estigens intensas. Com relação às características físico-químicas do mel, pode-se verificar que a legislação atual, referente ao mel de Apis mellifera não é adequada para todos os caracteres analisados, reforçando a necessidade do desenvolvimento de um padrão próprio para os méis de meliponíneos, incluindo critérios microbiológicos, uma vez que 64,52% do total das amostras de mel analisadas apresentaram contagem superior a 100 UFC.g-1 para fungos e leveduras, além de 2 amostras de T. angustula positivas para coliformes totais. / This research deals with the pollinic analyses of honey samples and pollen loads in order to identify the source of food resources used by five species of meliponine bees, in Piracicaba, State of São Paulo, Brazil. One also evaluated the annual development of the colonies and the determination of the physicochemical and microbiological characteristics of 31 honey samples. The following parameters were evaluated: sugars, moisture content, HMF, protein, ashes, pH, acidity, formol index, electrical conductivity, color, diastase activity, water activity and the presence of fecal coliforms, fungi and yeast. The results have indicated that excepting for Friseomelita varia, the species Tetragonisca angustula, Scaptotrigona bipunctata, Nanotrigona testaceicornis and Tetragona clavipes are generalist regarding the use of floral resources. Also the development of their colonies is influenced by climatic factors, once they need complementary food during rainfall, low temperatures and long drought periods. As to the physicochemical characteristics of honey samples, one observes that the Brazilian standard rules for Apis mellifera honey are not suitable for all the analyzed parameters, thus indicating the necessity of a standard rule for the meliponine honeys including microbiological criteria once 64.52% of the analyzed honey samples presented values higher than 100 CFU.g-1 for fungi and yeast and 2 positive samples of T.angustula for total number of coliforms.

FundaÃÃo Cearense de Apoio ao Desenvolvimento Cientifico e TecnolÃgico / O presente trabalho teve como objetivo avaliar os parÃmetros fÃsico-quÃmicos e quÃmicos e a atividade da polifenoloxidase (PPO) e peroxidase (POD) nas etapas de processamento e durante a vida de prateleira do suco tropical de manga nÃo adoÃado envasado pelo processo hot fill. Foram retiradas amostras apÃs as etapas de despolpa, homogeneizaÃÃo e pasteurizaÃÃo e do produto logo apÃs o processamento e aos 55, 110 e 165 dias de armazenamento (28ÂC Â 2ÂC). A acidez total titulÃvel, pH, sÃlidos solÃveis totais (ÂBrix), aÃÃcares redutores e totais, Ãcido ascÃrbico, carotenÃides, antocianinas e cor (L*, a* e b*) foram analisados. Os resultados apresentaram que o pH, a acidez total titulÃvel, o conteÃdo de aÃÃcar total e carotenÃides nÃo apresentaram significÃncia estatÃstica ao nÃvel de 5% durante o perÃodo de armazenagem. Foi observada uma maior atividade da PPO durante as etapas de processamento estudadas bem como na vida de prateleira do produto, de um modo geral mantendo-se oscilante. A POD apresentou atividade crescente nas etapas de processamento e em seguida mantendo-se constante durante o armazenamento. Conclui-se que os parÃmetros fÃsico-quÃmicos e quÃmicos para esse produto encontram-se dentro dos limites estabelecidos pela LegislaÃÃo Brasileira e o tratamento tÃrmico nÃo se apresentou eficiente para a inativaÃÃo dessas enzimas, devido possivelmente a presenÃa de isoformas com diferentes graus de termoestabilidade e/ou renaturaÃÃo de isotipos. / O presente trabalho teve como objetivo avaliar os parÃmetros fÃsico-quÃmicos e quÃmicos e a atividade da polifenoloxidase (PPO) e peroxidase (POD) nas etapas de processamento e durante a vida de prateleira do suco tropical de manga nÃo adoÃado envasado pelo processo hot fill. Foram retiradas amostras apÃs as etapas de despolpa, homogeneizaÃÃo e pasteurizaÃÃo e do produto logo apÃs o processamento e aos 55, 110 e 165 dias de armazenamento (28ÂC Â 2ÂC). A acidez total titulÃvel, pH, sÃlidos solÃveis totais (ÂBrix), aÃÃcares redutores e totais, Ãcido ascÃrbico, carotenÃides, antocianinas e cor (L*, a* e b*) foram analisados. Os resultados apresentaram que o pH, a acidez total titulÃvel, o conteÃdo de aÃÃcar total e carotenÃides nÃo apresentaram significÃncia estatÃstica ao nÃvel de 5% durante o perÃodo de armazenagem. Foi observada uma maior atividade da PPO durante as etapas de processamento estudadas bem como na vida de prateleira do produto, de um modo geral mantendo-se oscilante. A POD apresentou atividade crescente nas etapas de processamento e em seguida mantendo-se constante durante o armazenamento. Conclui-se que os parÃmetros fÃsico-quÃmicos e quÃmicos para esse produto encontram-se dentro dos limites estabelecidos pela LegislaÃÃo Brasileira e o tratamento tÃrmico nÃo se apresentou eficiente para a inativaÃÃo dessas enzimas, devido possivelmente a presenÃa de isoformas com diferentes graus de termoestabilidade e/ou renaturaÃÃo de isotipos. / The present work aimed to evaluate the physicochemical and chemical parameters and polyphenoloxidase (PPO) and peroxidase (POD) activity on the processing stages and shelf life of the tropical non sweetened mango juice preserved by hot fill method. The samples were removed afterwards the pulp discharged, homogenation, pasteurization and the product in the end of the processing and after 55, 110 and 165 days of storage (28ÂC Â 2ÂC). Total titratable acidity, pH, total soluble solids (ÂBrix), reducing and total sugar, ascorbic acid, carotenoids, anthocyanins and colour (L*, a* e b*) were analysed. The results showed that pH, total titratable acidity, total sugar content and carotenoids not have a statistical significance at a level of 5% along the storage time. It was observed a higher PPO activity during the studied processing stages and in the shelf life of the product, keeping oscillating in a general manner. The POD showed an increasing activity during the processing stages and keeping stable along the storage. In conclusion the physicochemical and chemical parameters for this product were within the limits established by the Brazilian legislation and the thermal treatment was not efficient to inactivate these enzymes probably due to the possible presence of isoforms with different thermo stability grades and/or isotypes renaturation. / The present work aimed to evaluate the physicochemical and chemical parameters and polyphenoloxidase (PPO) and peroxidase (POD) activity on the processing stages and shelf life of the tropical non sweetened mango juice preserved by hot fill method. The samples were removed afterwards the pulp discharged, homogenation, pasteurization and the product in the end of the processing and after 55, 110 and 165 days of storage (28ÂC Â 2ÂC). Total titratable acidity, pH, total soluble solids (ÂBrix), reducing and total sugar, ascorbic acid, carotenoids, anthocyanins and colour (L*, a* e b*) were analysed. The results showed that pH, total titratable acidity, total sugar content and carotenoids not have a statistical significance at a level of 5% along the storage time. It was observed a higher PPO activity during the studied processing stages and in the shelf life of the product, keeping oscillating in a general manner. The POD showed an increasing activity during the processing stages and keeping stable along the storage. In conclusion the physicochemical and chemical parameters for this product were within the limits established by the Brazilian legislation and the thermal treatment was not efficient to inactivate these enzymes probably due to the possible presence of isoforms with different thermo stability grades and/or isotypes renaturation.

FundaÃÃo Cearense de Apoio ao Desenvolvimento Cientifico e TecnolÃgico / O presente trabalho teve como objetivo avaliar os parÃmetros fÃsico-quÃmicos e quÃmicos e a atividade da polifenoloxidase (PPO) e peroxidase (POD) nas etapas de processamento e durante a vida de prateleira do suco tropical de manga nÃo adoÃado envasado pelo processo hot fill. Foram retiradas amostras apÃs as etapas de despolpa, homogeneizaÃÃo e pasteurizaÃÃo e do produto logo apÃs o processamento e aos 55, 110 e 165 dias de armazenamento (28ÂC Â 2ÂC). A acidez total titulÃvel, pH, sÃlidos solÃveis totais (ÂBrix), aÃÃcares redutores e totais, Ãcido ascÃrbico, carotenÃides, antocianinas e cor (L*, a* e b*) foram analisados. Os resultados apresentaram que o pH, a acidez total titulÃvel, o conteÃdo de aÃÃcar total e carotenÃides nÃo apresentaram significÃncia estatÃstica ao nÃvel de 5% durante o perÃodo de armazenagem. Foi observada uma maior atividade da PPO durante as etapas de processamento estudadas bem como na vida de prateleira do produto, de um modo geral mantendo-se oscilante. A POD apresentou atividade crescente nas etapas de processamento e em seguida mantendo-se constante durante o armazenamento. Conclui-se que os parÃmetros fÃsico-quÃmicos e quÃmicos para esse produto encontram-se dentro dos limites estabelecidos pela LegislaÃÃo Brasileira e o tratamento tÃrmico nÃo se apresentou eficiente para a inativaÃÃo dessas enzimas, devido possivelmente a presenÃa de isoformas com diferentes graus de termoestabilidade e/ou renaturaÃÃo de isotipos. / The present work aimed to evaluate the physicochemical and chemical parameters and polyphenoloxidase (PPO) and peroxidase (POD) activity on the processing stages and shelf life of the tropical non sweetened mango juice preserved by hot fill method. The samples were removed afterwards the pulp discharged, homogenation, pasteurization and the product in the end of the processing and after 55, 110 and 165 days of storage (28ÂC Â 2ÂC). Total titratable acidity, pH, total soluble solids (ÂBrix), reducing and total sugar, ascorbic acid, carotenoids, anthocyanins and colour (L*, a* e b*) were analysed. The results showed that pH, total titratable acidity, total sugar content and carotenoids not have a statistical significance at a level of 5% along the storage time. It was observed a higher PPO activity during the studied processing stages and in the shelf life of the product, keeping oscillating in a general manner. The POD showed an increasing activity during the processing stages and keeping stable along the storage. In conclusion the physicochemical and chemical parameters for this product were within the limits established by the Brazilian legislation and the thermal treatment was not efficient to inactivate these enzymes probably due to the possible presence of isoforms with different thermo stability grades and/or isotypes renaturation.

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No. of bitstreams: 2 Dissertação - Jennifer Vieira Pinto - 2016.pdf: 3207260 bytes, checksum: 75e3617cc1ca4e537ea4eb6d34fb3ef8 (MD5) license_rdf: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5) Previous issue date: 2016-08-25 / Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPES / We aimed to characterize the physical, chemical, technological, nutritional and functional properties of beans from different color groups in order to feed the Embrapa Rice and Beans database, contributing with useful information to the scientific community and food industries. Carioca (Pérola - "PER" and BRS Estilo - "ETL"), black (BRS Esteio - "EST" and IPR Uirapuru - "IPR") and special beans (BRS Agreste - "AGR" and BRS Pitanga - "PIT") were grown in June (winter / 2014) in Santo Antônio de Goiás -GO, and analyzed for: the 100-seed weight, size, sphericity, color, moisture, water activity and density. Flours were analyzed for: granulometry, color, water absorption and solubility index, oil retention capacity, foam properties, emulsifiers, stabilizers, paste properties, kaempferol content, proximal composition, minerals, amino acid profile, protein in vitro digestibility and anti-nutritional factors. Black grains were lighter, and carioca, heavier. Grains of "PER" presented greater length and "AGR", greater sphericity; "ETL" tended to lighter grains; "PIT", "IPR" and "EST", darker. Flours of "EST" and "IPR" had greater uniformity; "ETL", "PER" and "AGR" presented lighter and more yellow flours; the "IPR" flour showed higher values of water absorption; "EST", higher values of oil absorption; the "PIT", better solubility; AGR, higher foaming (pH 2.5); the "IPR", the higher maximum viscosity. Grains of "PIT" presented higher concentration of kaempferol; "PIT" and "PER", higher protein levels; "EST" had more lipids; and "AGR", more carbohydrates. All flours had high mineral contents. Black beans showed higher levels of essential and non-essential amino acids, followed by special and carioca beans; "EST" had the lowest Essential Amino Acid Score (EAS) (1.20), and "ETL", highest EAS (1.40); "EST", lower protein digestibility; carioca and special beans, higher levels of phytic acid; "PIT" showed higher molar ratio (phytate: iron) and "AGR", higher molar ratio (phytate: zinc); "PER", lower tannin contents; "IPR", lower levels of trypsin inhibitors and "PIT", greater inhibition of α-amylase. The specialty beans presented excellent physical, chemical, technological, nutritional and functional characteristics, and can be used as ingredients of new products by the food industry. / Objetivou-se caracterizar propriedades físicas, químicas, tecnológicas, nutricionais e funcionais de feijões de diferentes grupos de cor, a fim de alimentar o banco de dados da Embrapa Arroz e Feijão, contribuindo com informações úteis à comunidade científica e indústrias de alimentos. Feijões carioca (Pérola – “PER” e BRS Estilo – “ETL”), preto (BRS Esteio – “EST” e IPR Uirapuru – “IPR”) e especial (BRS Agreste – “AGR” e BRS Pitanga – “PIT”) foram cultivados em Junho (inverno/2014), em Santo Antônio de Goiás-GO, e analisados quanto à/ao: peso de 100 grãos, tamanho, esfericidade, cor, umidade, aw e densidade. Farinhas foram analisadas quanto à/ao: granulometria, cor, índice de absorção e solubilidade em água, capacidade de retenção de óleo, propriedades espumantes, emulsificantes, estabilizantes, propriedades de pasta, teor de kaempferol, composição centesimal, minerais, perfil de aminoácidos, digestibilidade proteica in vitro, e fatores antinutricionais. Grãos pretos apresentaram-se mais leves, e carioca, mais pesados. Grãos de “PER” apresentaram maior comprimento e da cultivar “AGR”, maior esfericidade; ”ETL” tendeu a grãos mais claros; ”PIT”, “IPR” e “EST”, mais escuros. Farinhas de “EST” e “IPR” tiveram maior uniformidade; “ETL”, “PER” e “AGR” apresentaram farinhas mais claras e amareladas; farinha do “IPR” apresentou maiores valores de absorção de água; “EST”, maiores valores de absorção de óleo; a da “PIT”, melhor solubilidade; a da “AGR”, maior formação de espuma (pH 2,5); a do “IPR”, maior viscosidade máxima. Grãos da “PIT” apresentaram maior concentração de kaempferol; “PIT” e “PER”, maiores teores protéicos; “EST”, mais lipídeos; e “AGR”, mais carboidratos. Todas as farinhas tiveram altos teores de minerais. Feijões pretos apresentaram maiores teores de aminoácidos essenciais e não essenciais, seguidos dos feijões especiais e carioca; “EST” teve o menor Escore de Aminoácidos Essenciais (EAE) (1,20), e “ETL”, maior EAE (1,40); “EST”, menor digestibilidade proteica; feijões carioca e especiais, maiores teores de ácido fítico; “PIT” apresentou maior razão molar (fitato:ferro) e “AGR”, maior razão molar (fitato:zinco); “PER”, menores teores de taninos; “IPR”, menores teores de inibidores de tripsina e “PIT”, maior inibição de α-amilase. Os feijões especiais apresentaram ótimas características físicas, químicas, tecnológicas, nutricionais e funcionais, podendo ser utilizados como matéria prima na elaboração de novos produtos pela indústria alimentícia.

Le classement de la famille des dibutylétains par l’Union Européenne comme reprotoxique et mutagène conduit les fabricants d’élastomères silicones à développer des solutions de remplacement de ces composés, largement employés comme catalyseur de réticulation. L’augmentation grandissante de la consommation de ce type d’élastomères amène à s’interroger sur leurs impacts dans les filières de traitement des déchets et sur l’influence du changement de catalyseur sur leur comportement environnemental. Ce domaine de recherche, très peu exploré, demande la mise en place d’une méthodologie spécifique, alliant des expériences de dégradations physico-chimiques et biologiques. Deux types d’élastomères simplifiés, réticulés par trois catalyseurs de polycondensation (un dibutylétain servant de référence et deux nouveaux) sont ciblés comme objet d’étude. Le premier axe, consacré à la matrice silicone, a permis de mettre en évidence une dégradation se déroulant en deux étapes successives, comme lors de la fin de vie de silicones fluides du type PolyDiMéthylSiloxane (PDMS). La première repose sur une hydrolyse chimique des chaînes siloxanes, formant majoritairement des oligosiloxanols (et principalement le monomère diméthylsilanediol) et des méthylsiloxanes cycliques (comme l’octaméthylcyclotétrasiloxane D4). La seconde est une biodégradation des sous-produits d’hydrolyse, aussi bien en aérobiose qu’en anaérobiose. Le second axe, consacré aux catalyseurs de polycondensation, prouve que ces composés prennent une place importante dans les mécanismes de dégradation. Ils impactent principalement les vitesses d’hydrolyse mais peuvent aussi influencer la nature des siloxanes relargués. De plus, ils ont des comportements totalement différents face à la dégradation biologique : ainsi, les catalyseurs organométalliques testés sont assimilables par les micro-organismes comme source primaire de carbone, alors que le catalyseur organique (un dérivé de guanidine) perturbe les métabolismes. Les composés biodégradables, même très peu mobiles en phase aqueuse, sont biodisponibles dans les élastomères et ont un impact sur la diversité des communautés bactériennes. Un champignon du genre Fusarium est d’ailleurs identifié comme capable de métaboliser une des nouvelles molécules développées. Le remplacement des dibutylétains permet de diminuer indiscutablement la toxicité des catalyseurs utilisés dans les élastomères silicones. La méthodologie mise en œuvre apporte de nombreuses informations quant aux impacts environnementaux et pourrait être transposée sans difficulté à l’étude d’autres matériaux. / Dibutyltin compounds are widely used as crosslinking catalysts in silicone elastomer industry. The classification of dibutyltins by the European Union as mutagenic and reprotoxic molecules lead manufacturers of silicone materials to develop alternatives. The increase of silicone elastomers demand requires to study their impacts during waste treatment and to assess the influence of the catalyst change on their environmental behavior. This unexplored area of research requires the establishment of a specific methodology, combining physico-chemical and biological degradation experiments. Two types of simplified elastomers are targeted in this study. They are crosslinked with three polycondensation catalysts: a dibutyltin derivative using as a reference and two new molecules. The first part, devoted to the silicone matrix, demonstrates a two stages degradation pathway in the environment. Silicone elastomers end-of-life is very similar to some silicone fluids, also known as PolyDiMethylSiloxanes (PDMS). The first stage is a chemical hydrolysis of siloxane chains, giving oligosiloxanols (mainly the monomer dimethylsilanediol) and cyclic methylsiloxanes (e.g. octamethylcyclotetrasiloxane D4). The second one is a biodegradation of hydrolysis by-products, in aerobic and anaerobic conditions. The second part, devoted to the polycondensation catalysts, demonstrates that these compounds play an important role in the degradation mechanisms. They mainly impact hydrolysis rates but also affect the nature of released products. In addition, they have a very distinct biological behavior: organometallic catalysts tested are assimilated as a single carbon source by microorganisms, while the organic catalyst (a derivative of guanidine) disrupts bacteria metabolism. Even if they have a limited mobility in the aqueous phase, biodegradable catalysts trapped in the silicone matrix are bioavailable and have an impact on bacterial communities. Moreover, a Fusarium fungus capable of metabolizing one of the new molecules developed is identified. The replacement of dibutyltin compounds undoubtedly reduces the toxicity of catalysts used to synthesized silicone elastomers. The methodology developed provides a lot of information about the environmental impacts of silicone elastomers and could be easily transposed to the study of other materials.

Ce travail porte sur la caractérisation physico-chimique de l'huile de Jatropha Curcas et sa capacité à remplacer l'huile minérale dans les transformateurs de puissance. Ce produit présente plusieurs avantages sur les autres huiles végétales comme l'huile de palme ou l'huile de colza, qui recommandent sa production et son utilisation. En effet, la plante de Jatropha Curcas peut être cultivée sur des sols pauvres à faibles précipitations, évitant ainsi d'utiliser des sols plus fertiles pour sa culture permettant ainsi aux petits exploitants de réserver leurs terres aux cultures de base. Cette plante peut pousser facilement dans des zones où les niveaux de précipitations annuelles sont nettement inférieures à celles requises par d'autres espèces telles que le colza, le tournesol, le soja, le maïs, le palmier à huile et d'autres. Elle peut être cultivée sur tous les types de sol en Indonésie, même sur des terres arides, dans de nombreuses régions de l'Indonésie orientale, inexploitées en raison des difficultés à planter d'autres cultures. En outre, l'huile de Jatropha Curcas est un produit non alimentaire. En faisant subir à l’huile de Jatropha Curcas brute une estérification à base alcaline avec de l'hydroxyde de potassium (KOH), on obtient de l’huile de méthylester de Jatropha Curcas (JMEO) dont la viscosité et l’acidité sont acceptables pour les équipements à haute tension en particulier pour les transformateurs de puissance. Les propriétés physico-chimiques et électriques de JMEO ont été mesurées ainsi que celles de l'huile minérale (MO) pour la comparaison. Pour les propriétés physico-chimiques, il s’agit de la densité relative, la teneur en eau, la viscosité, l'acidité, l'indice d'iode, la corrosivité, le point d'éclair, le point d'écoulement, la couleur, l'examen visuel, et la teneur en ester méthylique. Quant aux propriétés électriques, elles concernent la rigidité diélectrique sous différentes formes de tension (alternative, continu et choc de foudre), les phénomènes de pré-claquage et de claquage sous choc de foudre, les décharges glissantes sur les surfaces de carton comprimé, immergé dans JMEO et MO. Les résultats obtenus montrent que les tensions de claquage moyennes en continu et en choc de foudre des huiles JMEO et MO sont très proches ; la tension de claquage moyenne de JMEO est même plus élevée que celle de l'huile minérale (de type naphténique). La mesure des tensions de claquage des mélanges d'huiles «80% JMEO + 20% MO» et «50% JMEO et 50% MO» montrent que la tension de claquage du mélange «80% JMEO + 20% MO» est toujours supérieure à celle de l'huile minérale sous tensions alternative et continue. Cela indique que le mélange d'huile minérale et de JMEO avec un rapport de 20:80 ne dégrade pas ses performances. Le mélange d'huiles peut se produire lors du remplacement de l'huile minérale par JMEO dans les transformateurs installés et en exploitation. L'analyse des caractéristiques des streamers (la forme, le temps d'arrêt, le courant associé et la charge électrique) se développant dans les huiles JMEO et MO sous tension impulsionnelle de foudre, montre une grande similitude. Aussi, la longueur finale (Lf) et la densité des branches des décharges surfaciques se propageant sur le carton comprimé immergé dans l'huile de Jatropha Curcas de méthylester (JMEO) et de l'huile minérale (MO), sous tensions de choc de foudre positif et négatif (1,2/50 μs), pour deux configurations d'électrodes divergentes (électrode pointe haute tension perpendiculaire et tangente au carton, respectivement), sont fortement influencées par l'épaisseur du carton comprimé. Pour une épaisseur donnée, Lf augmente avec la tension et décroît lorsque l'épaisseur augmente. Lf est plus long lorsque la pointe est positive que lorsque la pointe est négative. Pour une tension et une épaisseur du carton comprimé donnée, les valeurs de Lf dans l’huile minérale et l’huile JMEO sont très proches. [...] / This work is aimed at the investigation of the physicochemical characterization of Jatropha Curcas seeds oil and its capacity to be an alternative option to replace mineral oil in power transformers. This product presents several advantages that recommend both its production and usage over those of other vegetable oils as crude palm oil and rapeseeds oil. Indeed, it may be grown on marginal or degraded soils avoiding thus the need to utilize those more fertile soils currently being used by smallholders to grow their staple crops; and it will readily grow in areas where annual rainfall levels are significantly lower than those required by other species such as palm oil, rape-seeds oil, sunflower oil, soybeans oil, corn oil and others. For instance, these plants can grow on all soil types in Indonesia, even on barren soil. The barren soil types can be found in many parts of eastern Indonesia that remain untapped because of the difficulty planted with other crops. Moreover, jatropha curcas oil is nonfood crops. Jatropha Curcas oil was processed by alkali base catalyzed esterification process using potassium hydroxide (KOH) to produce Jatropha Curcas methyl ester oil (JMEO) has a viscosity and a acidity that are acceptable for high voltage equipment especially in power transformer. The physicochemical and electrical properties of JMEO were measured as well as those of mineral oil (MO) for comparison. The physicochemical properties cover relative density, water content, viscosity, acidity, iodine number, corrosivity, flash point, pour point, color, visual examination, and methyl ester content. Meanwhile the electrical properties cover dielectric strength under AC, DC and lightning impulse voltages, pre-breakdown / streamers under lightning impulse voltage, creeping discharge over pressboard immersed in JMEO and MO. The obtained results show that the average DC and lightning impulse breakdown voltages of JMEO and MO are too close, even the average AC breakdown voltage of JMEO are higher than that of mineral oil (napthenic type). The measurement of breakdown voltages of two oil mixtures namely “80% JMEO + 20% MO” and “50% JMEO and 50% MO” shows that the breakdown voltage of the first mixture (i.e., “80%JMEO+20%MO”) is always higher than that of mineral oil under both AC and DC voltages. This indicates that mixing 20:80 mineral oil to JMEO ratio does not degrade its performance. The mixing of oils can occur when replacing mineral oil by JMEO in installed transformers. The analysis of the streamers characteristics (namely; shape, stopping length, associated current and electrical charge) developing in JMEO and MO under lightning impulse voltages, shows that these are too close (similar). It is also shown that the stopping (final) length Lf and the density of branches of creeping discharges propagating over pressboard immersed in Jatropha Curcas methyl ester oil (JMEO) and mineral oil (MO), under positive and negative lightning impulse voltages (1.2/50 μs), using two divergent electrode configurations (electrode point perpendicular and tangential to pressboard), are significantly influenced by the thickness of pressboard. For a given thickness, Lf increases with the voltage and decreases when the thickness increases. Lf is longer when the point is positive than with a negative point. For a given voltage and thickness of pressboard, the values of Lf in mineral oil and JMEO are very close. It appears from this work that JMEO could constitute a potential substitute for mineral oil for electrical insulation and especially in high voltage power transformers.

The concern about food safety, animal welfare, and environmental impacts caused by intensive production systems has led to an increasing interest in foods derived from a sustainable production system. In this context, organic milk production in Brazil has grown considerably in recent years, but little is known about the quality of the food produced in the country. In order to evaluate the quality of organic milk, the hygienic quality, chemical composition, and safety concerning pesticide residues was assessed. Five brands of certified organic pasteurized milk and five brands of conventional pasteurized milk commercialized in three Brazilian states were collected between May 2011 and March 2012, every two months, totaling 29 samples of organic milk (OM) and 27 conventional milk (CM). The collection of raw milk samples was made every two months, from July 2011 to May 2012 in 20 organic farms and 20 conventional farms in western Santa Catarina, totaling 120 OM and 115CM samples. In pasteurized milk, physicochemical analyzes were performed and the fatty acid profile was determined. In raw milk, chemical composition analyzes, somatic cell count (SCC), and total bacterial count (TBC) were carried out. Both types of milk were subjected to the determination of pesticides and veterinary drugs. When the results of raw milk production in the two systems were compared, no difference for the mean value of fat, protein and total solids, or SCC was found. Organic milk showed better quality in relation to microbial contamination and higher content of lactose. For pasteurized milk with the exception of non fat solids, all average values of physical and chemical parameters of milk met the limits of the Brazilian legislation. The fatty acid profile was affected by geographical origin, and to a lesser extent, the effect of season, probably due to differences on the feeding regime. The milk obtained in Rio Grande do Sul and São Paulo were characterized by having higher values of health-promoting fatty acids, including conjugated linoleic acid (CLA). However, the milk collected in the Federal District was characterized by higher concentrations of saturated fatty acids (SFA). The results for raw and pasteurized milk indicate that the organic management alone had no effect on milk quality regarding chemical composition, which are determined by several factors that are independent of the production system. No veterinary drugs was found in any of the samples analyzed. However, for contamination with pesticides no difference was observed when considering the number of contaminated samples in either production system. Results indicate the need to monitor milk for the presence of pesticides in order to improve food safety, especially for organic milk, which should be free of such contaminants. / A preocupação com segurança alimentar, bem-estar animal e impactos no meio ambiente causados pelos sistemas intensivos de produção, tem levado a um maior interesse por alimentos que sejam oriundos de um sistema de produção sustentável. Neste contexto, a produção de leite orgânico no Brasil cresceu consideravelmente nos últimos anos, porém pouco se sabe sobre a qualidade deste alimento produzido no país. Para avaliar a qualidade do leite orgânico foram realizadas análises que contemplaram aspectos da qualidade higiênica, composição química e a segurança quanto à presença de resíduos químicos. Cinco marcas de leite orgânico pasteurizado certificado e cinco de leite pasteurizado convencional comercializados em três Estados brasileiros foram coletadas entre maio de 2011 e março de 2012, com intervalo de dois meses, totalizando 29 amostras de leite orgânico (LO) e 27 de leite convencional (LC). As coletas de leite cru foram feitas de julho de 2011 a maio de 2012, também bimestrais, em 20 propriedades orgânicas e 20 propriedades convencionais na região Oeste de Santa Catarina, totalizando 120 amostras de LO e 115 de LC. No leite pasteurizado foram realizadas análises físico-químicas e o perfil de ácidos graxos. No leite cru foram realizadas as análises de composição química, contagem de células somáticas (CCS) e contagem bacteriana total (CBT). Ambos os tipos de leite foram submetidos à determinação de agrotóxicos e medicamentos veterinários. Comparando-se os resultados do leite cru, entre os dois sistemas de produção, não foi encontrado diferença para o valor médio de gordura, proteína e sólidos totais, assim como para CCS. O leite orgânico apresentou melhor qualidade em relação a contaminação microbiana e teor superior de lactose. Para o leite pasteurizado com exceção do extrato seco desengordurado (ESD), todos os valores médios dos parâmetros físicos e químicos atenderam aos limites da legislação brasileira. O perfil de ácidos graxos sofreu efeito da origem geográfica, e em menor escala o efeito da sazonalidade, provavelmente por diferenças no regime alimentar. Os leites obtidos no Rio Grande do Sul e em São Paulo se caracterizaram por possuir valores superiores de ácidos graxos promotores da saúde, entre eles o ácido linoléico conjugado (CLA), enquanto os leites coletados no Distrito Federal se caracterizaram por concentrações superiores de ácidos graxos saturados. Os resultados para o leite cru e pasteurizado indicam que o manejo orgânico por si só, não influenciou na qualidade do leite quanto aos aspectos de composição química, que são determinados por vários fatores que independem do sistema de produção. Não foram encontrados medicamentos veterinários em nenhuma das amostras analisadas. Quanto à contaminação por agrotóxicos não houve diferença quando considerado o número de amostras contaminadas em ambos os sistemas de produção. Os resultados indicam a necessidade de monitorar o leite quanto a presença de agrotóxicos a fim de melhorar a segurança alimentar, principalmente para leite orgânico, que deve estar livre desse tipo de contaminantes.

L’odontologie conservatrice a connu une véritable révolution avec l’avènement de la dentisterie adhésive et le développement des résines composites associé au collage aux tissus dentaires. L’apparition il y a 20 ans des résines composites fluides a élargi encore les possibilités thérapeutiques des praticiens. La mise sur le marché d’un grand nombre de résines composites qui diffèrent par leur nature matricielle et par le type, la taille et la proportion des charges incorporées associée au manque d’informations des fabricants sur les compositions exactes de leurs produits empêchent les praticiens de réellement connaitre les caractéristiques des matériaux qu’ils utilisent. L’hyper-caractérisation in vitro desdits matériaux est une voie importante pour avancer dans la compréhension de leur comportement. Afin de juger de l’impact de la variation du taux de charges dans le comportement mécanique et physico-chimique des résines composites fluides, nous avons étudié deux groupes de matériaux : un premier groupe constitué de résines composites fluides expérimentales à matrice commune et à taux de charges variable et un deuxième groupe composé de résines composites fluides disponibles dans le commerce. Pour chacun de ces matériaux après la détermination du taux de charges par la méthode de la calcination, l’évaluation des caractéristiques rhéologiques (viscosité complexe et module de conservation), la mesure de la micro-dureté (micro-dureté Vickers), la contraction volumétrique de prise selon la méthode de la déflexion d’une lame de verre, l’analyse thermo-mécanique dynamique en flexion (module de conservation, module de perte, facteur d’amortissement) ainsi que les capacités d’absorption d’eau et de solubilisation (détermination par différentiel de gravimétrie après immersion dans différents milieux) sont autant de facteurs potentiellement influencés par ledit taux de charges qui ont été étudiés. Si le taux de charges devrait clairement faire partie des critères de choix du praticien tant il apparait influant sur les plans mécaniques et physico-chimiques, il apparait qu’un taux de charges élevé ne représente pas une garantie suffisante pour répondre de façon optimale au cahier des charges du matériau d’obturation idéal. L’emploi de résines composites fluides déformulées à taux de charges variable permet d’évaluer le rôle de la phase dispersée, pour autant, l’étude en parallèle de matériaux commerciaux met en lumière l’influence de la nature matricielle et des différentes entités monomériques entrant dans la structure polymère. / Conservative dentistry has undergone a genuine revolution, with the advent of adhesive dentistry and the development of resin composites combined with dental bonding. The emergence of flowable resin composites 20 years ago further expanded the treatment options open to dental practitioners. The appearance on the market of a large number of resin composites that differ in terms of their matrix type, along with the size and the proportion of the fillers incorporated, combined with a lack of information from manufacturers concerning the exact compositions of their products, means that practitioners do not really know all the characteristics of the materials they are using. In vitro hypercharacterization of these materials is an important approach to help us gain a better understanding of their properties. In order to assess the impact of variation of filler contents on the mechanical and physicochemical properties of flowable resin composites, we studied two groups of materials: a first group, composed of experimental flowable resin composites with the same matrix and a variable filler content, and a second group, composed of commercially available flowable resin composites. For each of these materials, after determination of the filler content using the calcination method, assessment of their rheological properties (complex viscosity and storage modulus), measurement of microhardness (Vickers microhardness), volumetric setting shrinkage using the glass slide deflection technique, dynamic thermo-mechanical analysis in flexure (storage modulus, loss modulus, damping factor), along with the water absorption and dissolution capacities (determination by thermal gravimetry differential following immersion in different media) are all factors potentially influenced by the said filler contents studied. While the filler content should clearly be one of the decision-making criteria used by practitioners given the influence it seems to have on both mechanical and physicochemical properties, it nonetheless appears that a high filler content is not, in itself, a sufficient guarantee that the material meets the optimum specifications for an ideal filling material. The use of deformulated flowable composite resins with a variable filler content makes it possible to assess the role of the dispersed phase. However, a parallel study of commercially available materials highlights the influence of the matrix type and the various monomeric entities included in the polymer structure.