Este estudo procurou avaliar as mudanças físicas e/ou químicas que ocorrem na hidroxiapatita (HAP) sintética e na presente no esmalte dental sob ação de aquecimento térmico em forno ou irradiação com o laser de Er,Cr:YSGG (2,79 m). Busca-se obter variações em sua estrutura a fim de torná-los mais resistentes à desmineralização, visando e prevenir a formação da cárie dental. A HAP sintética foi produzida pela reação das soluções de Ca(NO3) e (NH4)2HPO4 com controle de temperatura e pH. O esmalte foi coletado do dentes bovinos e triturados. As amostras em pó de HAP sintética e esmalte foram submetidas a aquecimento térmico em forno nas temperaturas de 200 °C, 400 °C, 600 °C, 800 °C e 1000 °C. Foram feitas irradiações laser com 5,79 J/cm2, 7,65 J/cm2, 10,55 e 13,84 J/cm2 para a HAP sintética e de 7,53 J/cm2, 10,95 J/cm2 e 13,74 J/cm2 para o esmalte. As amostras foram avaliadas por difração de raios-X(DRX) para análise das fases cristalográficas presentes e análise pelo método de Rietveld para comprovação destas fases cristalográficas e determinação de respectivas proporções no material. Foram obtidos também as variações de parâmetros de rede da cela unitária (eixo-a, eixo-c e volume), tamanho dos cristalitos e taxas de ocupações dos sítios dos átomos de Ca e P de ambos os materiais. As amostras foram ainda analisadas por espectroscopia de absorção no infravermelho por transformada de Fourier (FTIR), que mostrou as variações composicionais ocasionadas pelos tratamentos calculando-se as áreas das bandas referentes aos radicais carbonato, fosfato, água adsorvida e hidroxila. A termografia no infravermelho foi usada para medir a temperatura superficial gerada pelo feixe do laser nas amostras sólidas de esmalte. Com relação às fases cristalográficas presentes só foram encontradas além da fase majoritária de hidroxiapatita, as fases de fosfato de octacálcio (OCP) nas amostra de HAP sintética e tricálcio 9 fosfato da fase b (b -TCP) no esmalte aquecido a 800 °C. Apresentaram-se mudanças nos parâmetros de rede da cela unitária da HAP sintética e do esmalte, com diminuição do eixo-a, volume e tamanho dos cristalitos até as temperaturas entre 400 °C e 600 °C e também nas amostras irradiadas a laser. Acima da temperatura de 600 °C há o aumento destes parâmetros de rede. A relação Ca/P em todas as amostras sofreram diminuições, sendo que na amostra de esmalte irradiada a 7,53 J/cm2 apresentou Ca/P igual a 1,6817 e a irradiada a 13,74 J/cm2 apresentou Ca/P igual a 1,6831. A espectroscopia mostrou que os efeitos tanto do aquecimento como da irradiação laser podem ser observados principalmente nas bandas de carbonato, água adsorvida e hidroxila e que as mudanças da rede cristalográfica podem ser correlacionadas com substituições de carbonato em sítios de hidroxilas e fosfatos. Ambos os tratamentos causam também diminuição da concentração de carbonatos, sendo que este efeito ocorreu com maior intensidade nas irradiações a laser e houve ainda diminuição na quantidades de água adsorvida e hidroxilas. Todas estas alterações modificam as propriedades do material, como sua solubilidade e consequentemente influenciam na resistência à desmineralização de interesse para processos como prevenção da cárie dental e erosão dental. / The study evaluate the physical changes and/or chemical that occurs in synthetic hydroxyapatite (HAP) and in enamel under action of thermal heating in oven or laser irradiation of Er,Cr:YSGG that may cause changes in its structure to make them more resistant to demineralization aiming the formation of dental caries. The synthetic HAP was produced by reaction of solutions of Ca(NO3) and (NH4)2HPO4 with controlled temperature and pH. The enamel powder was collected from the bovine teeth. Samples of powder enamel and synthetic HAP were subjected to thermal heating in oven at temperatures of 200 °C, 400 °C, 600 °C, 800 °C and 1000 °C. For the laser irradiation of materials, were made with 5,79 J/cm2 of irradiation, 7,65 J/cm2, 10,55 J/cm2 and 13,84 J/cm2 for synthetic HAP and 7,53 J/cm2, 10,95 J/cm2, and 13,74 J/cm2 for the enamel. The samples were evaluated by X-ray diffraction (XRD) for analysis of crystallographic phases and analysis by the Rietveld method, to determine their respective proportions in the material, as well as results of changes of the lattice unit cell parameters (axisa, axis-c and volume), crystallites sizes and the occupation rate of sites of Ca and P atoms. The samples were analyzed by Fourier transform infrared spectroscopy (FTIR), which should compositional changes due to treatment related to carbonate, phosphate, adsorbed water and hydroxyl radicals content. The infrared was used to measure the surface temperature generated by the laser beam in the solid samples of enamel. Besides the major hydroxyapatite crystallographic phases, there was formations of octacalcium phosphate (OCP) and phase of tricalcium phosphate (-TCP ) in enamel heated at 800 °C. There was reduction of the axis-a, volume and size of crystallites to the temperatures between 400 °C and 600 °C and also on laser irradiated samples. Above the temperature of 600 °C it is observed the effect in the lattice parameters. The Ca/P relation in all the samples decreased. The enamel samples irradiated by 7,53 J/cm2 showed Ca/P equal to 1,6817 and by 13,74 J/cm2 Ca/P was 1,6831. Spectroscopy results showed that both the heating and laser irradiation cause changes primarily in the bands of carbonate, water adsorbed and hydroxyl and the crystallographic changes of the lattice may be correlated with changes in carbonate in the sites of hydroxyl and phosphates. The effects of heating in oven and laser irradiation causes reduction of carbonate content, and this effect was more evident in laser irradiated samples, there was also decreases in water and adsorbed hydroxyl contents. All these changes alter the properties of the material, as its solubility and therefore affect the demineralization process and can be useful for caries prevention as well as dental erosion prevention.

O uso do óxido de nióbio como promotor e como suporte tem sido investigado em numerosas aplicações catalíticas, tais como, na oxidação seletiva, conversão de hidrocarbonetos, polimerização, eliminação de poluentes (NOx), desidrogenação, etc. Sabe-se que a adição de nióbio na γ-Al2O3 melhora a acidez, a seletividade e a estabilidade térmica e, conseqüentemente, a atividade catalítica desses materiais. A atividade catalítica dos sistemas contendo nióbia suportada é decorrente das diferentes espécies redox do óxido de nióbio presentes nas superfícies do sólido. O presente trabalho tem como objetivo avaliar a influência do teor de nióbio e vanádio no sistema catalítico V2O5/Nb2O5-Al2O3 na reação de desidrogenação oxidativa do propano. A fim de alcançar o objetivo deste trabalho, as seguintes técnicas de caracterização foram utilizadas: volumetria de N2 (área específica e volume de poros), redução a temperatura programada, difratometria de raios X (DRX) e espectroscopia Raman. As propriedades ácidas e/ou básicas dos suportes e catalisadores foram avaliadas através da reação de decomposição do isopropanol. / The use of niobium oxide as a promoter and as a support has been investigated in various catalyst applications, such as selective oxidation, hydrocarbonate conversion, polymerization, elimination of (NOx) pollutants, dehydrogenation, etc. It is known that adding niobium to γ-Al2O3 improves acidity, selectivity and thermal stability and consequently the catalyst activity of these materials. The catalyst activity of systems containing supported niobium is due to the different redox species of niobium oxide present on the solid surface. This study aims to evaluate the influence of the niobium and vanadium content in the V2O5/Nb2O5-Al2O3 catalyst system in the propane oxidative dehydrogenation reaction. Aiming the target of this study, the following characterization techniques were used: N2 volumetry (specific area and pore volume), temperature-programmed reduction, X-ray diffractometry (DRX), and Raman spectroscopy. The acid-base properties of the supports and catalysts were studied through isopropanol decomposition reaction.

O comportamento térmico, a obtenção e caracterização de formas cristalinas do anti-histamínico loratadina foram investigado. A escolha do anti-histamínico loratadina como objeto de estudo resulta do seu interesse farmacológico. A loratadina é a Denominação Comum Internacional (DCI) dada ao etil 4-(8-cloro-5,6-dihidro-11H-benzo[5,6]cicloheptano[1,2-b]piridino-11-ilideno)-1-piperidinocarboxilato, que é um potente antialérgico e anti-histamínicos tricíclico, não-sedativo de ação prolongada. Formas cristalinas foram preparadas e estudadas com vista à identificação de formas polimórficas. Os solventes utilizados na preparação das soluções foram: álcool etílico, acetonitrila, álcool isopropílico, acetona, álcool metílico, éter isopropílico, éter metil terc-butílico, tolueno, clorofórmio. A cristalização foi realizada por evaporação do solvente em diferentes temperaturas. A calorimetria exploratória diferencial (DSC), termogravimetria e termogravimetria derivada (TG/DTG), análise térmica diferencial (DTA), difração de raios X (DRX) e a ressonância magnética nuclear (RMN) foram às técnicas utilizadas na caracterização das formas polimórficas. A maioria das amostras obtidas pelas técnicas de cristalização consistiam de misturas de formas cristalinas, contendo, por vezes, formas metaestáveis e formas amorfas. Identificaram-se duas formas cristalinas como polimorfos da loratadina, cujas curvas DSC mostrou interconversão entre ambas. / The preparation, characterization and thermal behavior of the crystalline forms of the antihistamine loratadine has been developed. The selection of loratadine as an object of study results from its pharmacological interest. Loratadine is the International Common Denomination (ICD) given to ethyl 4-(8-chloro-5,6-dihydro-11H-benzo [5,6] cyclohepta[1,2-b]pyridin-11-ylidene)-1-piperidinecarboxylate, a potent anti-allergic and anti-histamincs, tricyclic, non-sedating long acting. Crystalline forms were prepared and studied for the identification of polymorphic forms. The solvents used in preparing the solutions were: ethanol, acetonitrile, isopropyl alcohol, acetone, methyl alcohol, isopropyl ether, methyl tert-butyl ether, toluene, chloroform. The crystallization was performed by evaporating the solvent at different temperatures. The differential scanning calorimetry (DSC), thermogravimetry and derivative thermogravimetry (TG/DTG), differential thermal analysis (DTA), X-ray diffraction (XRD) and nuclear magnetic resonance (NMR) techniques were used to characterize the polymorphic forms. Most of the samples obtained by the crystallization were mixtures of crystalline forms, containing sometimes forms metastable and amorphous forms. It was identified as two crystalline polymorphic forms of loratadine, whose DSC curves demonstrated that they are interconvertable.

Made available in DSpace on 2014-12-17T15:41:40Z (GMT). No. of bitstreams: 1 AnaCPC.pdf: 1447913 bytes, checksum: 8f65c2f6df911f6db297163eb551fb69 (MD5) Previous issue date: 2008-02-29 / Conselho Nacional de Desenvolvimento Cient?fico e Tecnol?gico / The metalic oxides have been studies due to differents applications as materials semiconductor in solar cells, catalysts, full cells and, resistors. Titanium dioxide (TiO2) has a high electric conductivity due to oxygen vacancies. The Ce(SO4)2.2H2O doped samples TiO2 and TiO2 pure was obtained sol-gel process, and characterized by X-ray diffractometry,thermal analysis, and impedance spectroscopy. The X-ray diffraction patterns for TiO2 pure samples shows at 700?C anatase phase is absent, and only the diffraction peaks of rutile phase are observed. However, the cerium doped samples only at 900?C rutile in the phase present with peaks of cerium dioxide (CeO2). The thermal analysis of the TiO2 pure and small concentration cerium doped samples show two steps weight loss corresponding to water of hydration and chemisorbed. To larger concentration cerium doped samples were observed two steps weight loss in the transformation of the doped cerium possible intermediate species and SO3. Finally, two steps weight loss the end products CeO2 and SO3 are formed. Analyse electric properties at different temperatures and concentration cerium doped samples have been investigated by impedance spectroscopy. It was observed that titanium, can be substituted by cerium, changing its electric properties, and increased thermal stability of TiO2 anatase structure / Os ?xidos met?licos t?m sido muito estudados devido suas diversas aplica??es como materiais semicondutores em c?lulas solares, catalisadores, c?lulas combust?veis e resistores. O Di?xido de Tit?nio possui uma alta condutividade el?trica devido ?s suas vac?ncias de oxig?nio. Amostras de TiO2 puro, obtidas pelo m?todo sol-gel e dopadas com solu??es de Ce(SO4)2.2H2O, foram analisadas atrav?s de difratometria de raios-X, an?lise t?rmica e espectroscopia de imped?ncia. Atrav?s dos difratogramas de raios-X observou-se a transi??o completa das fases anat?sio-rutilo, para a amostra do TiO2 puro a partir de 700?C. Entretanto, para as amostras dopadas, essa transi??o s? ? completa a partir de 900?C, aparecendo picos correspondentes ao ?xido de c?rio. Atrav?s da an?lise t?rmica se observou uma perda de massa, para o TiO2 puro e dopado com a menor concentra??o de c?rio, correspondente ? desidrata??o e a ?gua quimissorvida. Para as amostras dopadas em uma maior concentra??o, foram observados dois est?gios de perda de massa, devido a decomposi??o do dopante em intermedi?rios e SO3. Essas amostras apresentaram mais duas perdas de massa devido a forma??o do CeO2 e SO3. A partir da espectroscopia de imped?ncia analisou-se as propriedades el?tricas das amostras em fun??o da temperatura de calcina??o e em fun??o da concentra??o do dopante. Tamb?m foi observado que o c?rio, por ter a capacidade de substituir o tit?nio na sua estrutura cristalina, modifica suas propriedades el?tricas e tem o poder de estabiliz?-lo termicamente em certas temperaturas

O uso do óxido de nióbio como promotor e como suporte tem sido investigado em numerosas aplicações catalíticas, tais como, na oxidação seletiva, conversão de hidrocarbonetos, polimerização, eliminação de poluentes (NOx), desidrogenação, etc. Sabe-se que a adição de nióbio na γ-Al2O3 melhora a acidez, a seletividade e a estabilidade térmica e, conseqüentemente, a atividade catalítica desses materiais. A atividade catalítica dos sistemas contendo nióbia suportada é decorrente das diferentes espécies redox do óxido de nióbio presentes nas superfícies do sólido. O presente trabalho tem como objetivo avaliar a influência do teor de nióbio e vanádio no sistema catalítico V2O5/Nb2O5-Al2O3 na reação de desidrogenação oxidativa do propano. A fim de alcançar o objetivo deste trabalho, as seguintes técnicas de caracterização foram utilizadas: volumetria de N2 (área específica e volume de poros), redução a temperatura programada, difratometria de raios X (DRX) e espectroscopia Raman. As propriedades ácidas e/ou básicas dos suportes e catalisadores foram avaliadas através da reação de decomposição do isopropanol. / The use of niobium oxide as a promoter and as a support has been investigated in various catalyst applications, such as selective oxidation, hydrocarbonate conversion, polymerization, elimination of (NOx) pollutants, dehydrogenation, etc. It is known that adding niobium to γ-Al2O3 improves acidity, selectivity and thermal stability and consequently the catalyst activity of these materials. The catalyst activity of systems containing supported niobium is due to the different redox species of niobium oxide present on the solid surface. This study aims to evaluate the influence of the niobium and vanadium content in the V2O5/Nb2O5-Al2O3 catalyst system in the propane oxidative dehydrogenation reaction. Aiming the target of this study, the following characterization techniques were used: N2 volumetry (specific area and pore volume), temperature-programmed reduction, X-ray diffractometry (DRX), and Raman spectroscopy. The acid-base properties of the supports and catalysts were studied through isopropanol decomposition reaction.

Ce travail porte sur l’étude des phénomènes induits par implantation d’hydrogène et/ou d’hélium dans le silicium monocristallin. Le cloquage et l’exfoliation dus à la coimplantation d’hélium et d’hydrogène ont été étudiés en fonction des paramètres d’implantation (énergie, fluence, courant, rapport H/He) et des conditions de recuit. Un comportement de type fenêtre à été observé dont le maximum de surface exfoliée dépend uniquement de la fluence. Deux mécanismes d’exfoliation liés aux régimes de fluence ont été identifiés et discutés. D’autre part, la microstructure des échantillons a été étudié par MET, et les déformations ont été mesurées par diffraction des Rayons X. Un modèle décrivant la distribution des contraintes dans le substrat implanté a été proposé. Le phénomène de delamination des substrats qui apparaît pour des conditions particulières d’implantation a également été étudié, comparé aux phénomènes de cloquage et exfoliation, et expliqué en utilisant des concepts de la mécanique de la fracture. Enfin, l’interaction élastique entre précipités d’He et d’H a été étudiée pour des profils d’implantation superposés et décalés. Dans ce dernier cas, nous avons montré que le champ de contraintes générées par les plaquettes d’hélium en surpression pouvait être utilisé comme source locale de contraintes pour contrôler la formation et la croissance de plaquettes d’hydrogène. Afin d’interpréter nos résultats expérimentaux, nous avons développé un modèle basé sur l’interaction élastique pour la nucléation des précipités dans un solide semi-infini. / The present work relates an investigation of H2 + and He+ coimplanted (001)-Si substrates. The phenomena of blistering and exfoliation were studied by SEM as a function of the implantation parameters (energy, fluence, current and H/He ration) and annealing protocol. A window behavior as function of the implanted fluence was observed and two distinct fluence dependents mechanisms of exfoliation were indentified and discussed. The microstructure of the implanted samples was studied using TEM and related to ballistic effects and stress-strain dependent interactions. The strain was measured using DRX and a model to describe the stress-strain distribution into the implanted layer is developed. A new phenomenon of delamination of thin layer from implanted Si substrates was observed to emerge from particular implantation conditions. The behavior was studied and explained using fracture mechanics concepts and contrasted to blistering/exfoliation processes. Finally, the elastic interaction between He and H plate-like precipitates giving rise to arranged nanostructure was demonstrated and studied using TEM. An elasticity based model was developed to understand the behavior. The result set the basis for further developments of nanostructures within a crystalline matrix by manipulating preferential orientations of precipitates in nanometric scale.

Ce travail porte sur l’étude des phénomènes induits par implantation d’hydrogène et/ou d’hélium dans le silicium monocristallin. Le cloquage et l’exfoliation dus à la coimplantation d’hélium et d’hydrogène ont été étudiés en fonction des paramètres d’implantation (énergie, fluence, courant, rapport H/He) et des conditions de recuit. Un comportement de type fenêtre à été observé dont le maximum de surface exfoliée dépend uniquement de la fluence. Deux mécanismes d’exfoliation liés aux régimes de fluence ont été identifiés et discutés. D’autre part, la microstructure des échantillons a été étudié par MET, et les déformations ont été mesurées par diffraction des Rayons X. Un modèle décrivant la distribution des contraintes dans le substrat implanté a été proposé. Le phénomène de delamination des substrats qui apparaît pour des conditions particulières d’implantation a également été étudié, comparé aux phénomènes de cloquage et exfoliation, et expliqué en utilisant des concepts de la mécanique de la fracture. Enfin, l’interaction élastique entre précipités d’He et d’H a été étudiée pour des profils d’implantation superposés et décalés. Dans ce dernier cas, nous avons montré que le champ de contraintes générées par les plaquettes d’hélium en surpression pouvait être utilisé comme source locale de contraintes pour contrôler la formation et la croissance de plaquettes d’hydrogène. Afin d’interpréter nos résultats expérimentaux, nous avons développé un modèle basé sur l’interaction élastique pour la nucléation des précipités dans un solide semi-infini. / The present work relates an investigation of H2 + and He+ coimplanted (001)-Si substrates. The phenomena of blistering and exfoliation were studied by SEM as a function of the implantation parameters (energy, fluence, current and H/He ration) and annealing protocol. A window behavior as function of the implanted fluence was observed and two distinct fluence dependents mechanisms of exfoliation were indentified and discussed. The microstructure of the implanted samples was studied using TEM and related to ballistic effects and stress-strain dependent interactions. The strain was measured using DRX and a model to describe the stress-strain distribution into the implanted layer is developed. A new phenomenon of delamination of thin layer from implanted Si substrates was observed to emerge from particular implantation conditions. The behavior was studied and explained using fracture mechanics concepts and contrasted to blistering/exfoliation processes. Finally, the elastic interaction between He and H plate-like precipitates giving rise to arranged nanostructure was demonstrated and studied using TEM. An elasticity based model was developed to understand the behavior. The result set the basis for further developments of nanostructures within a crystalline matrix by manipulating preferential orientations of precipitates in nanometric scale.

Ce travail porte sur l’étude des phénomènes induits par implantation d’hydrogène et/ou d’hélium dans le silicium monocristallin. Le cloquage et l’exfoliation dus à la coimplantation d’hélium et d’hydrogène ont été étudiés en fonction des paramètres d’implantation (énergie, fluence, courant, rapport H/He) et des conditions de recuit. Un comportement de type fenêtre à été observé dont le maximum de surface exfoliée dépend uniquement de la fluence. Deux mécanismes d’exfoliation liés aux régimes de fluence ont été identifiés et discutés. D’autre part, la microstructure des échantillons a été étudié par MET, et les déformations ont été mesurées par diffraction des Rayons X. Un modèle décrivant la distribution des contraintes dans le substrat implanté a été proposé. Le phénomène de delamination des substrats qui apparaît pour des conditions particulières d’implantation a également été étudié, comparé aux phénomènes de cloquage et exfoliation, et expliqué en utilisant des concepts de la mécanique de la fracture. Enfin, l’interaction élastique entre précipités d’He et d’H a été étudiée pour des profils d’implantation superposés et décalés. Dans ce dernier cas, nous avons montré que le champ de contraintes générées par les plaquettes d’hélium en surpression pouvait être utilisé comme source locale de contraintes pour contrôler la formation et la croissance de plaquettes d’hydrogène. Afin d’interpréter nos résultats expérimentaux, nous avons développé un modèle basé sur l’interaction élastique pour la nucléation des précipités dans un solide semi-infini. / The present work relates an investigation of H2 + and He+ coimplanted (001)-Si substrates. The phenomena of blistering and exfoliation were studied by SEM as a function of the implantation parameters (energy, fluence, current and H/He ration) and annealing protocol. A window behavior as function of the implanted fluence was observed and two distinct fluence dependents mechanisms of exfoliation were indentified and discussed. The microstructure of the implanted samples was studied using TEM and related to ballistic effects and stress-strain dependent interactions. The strain was measured using DRX and a model to describe the stress-strain distribution into the implanted layer is developed. A new phenomenon of delamination of thin layer from implanted Si substrates was observed to emerge from particular implantation conditions. The behavior was studied and explained using fracture mechanics concepts and contrasted to blistering/exfoliation processes. Finally, the elastic interaction between He and H plate-like precipitates giving rise to arranged nanostructure was demonstrated and studied using TEM. An elasticity based model was developed to understand the behavior. The result set the basis for further developments of nanostructures within a crystalline matrix by manipulating preferential orientations of precipitates in nanometric scale.

O comportamento térmico, a obtenção e caracterização de formas cristalinas do anti-histamínico loratadina foram investigado. A escolha do anti-histamínico loratadina como objeto de estudo resulta do seu interesse farmacológico. A loratadina é a Denominação Comum Internacional (DCI) dada ao etil 4-(8-cloro-5,6-dihidro-11H-benzo[5,6]cicloheptano[1,2-b]piridino-11-ilideno)-1-piperidinocarboxilato, que é um potente antialérgico e anti-histamínicos tricíclico, não-sedativo de ação prolongada. Formas cristalinas foram preparadas e estudadas com vista à identificação de formas polimórficas. Os solventes utilizados na preparação das soluções foram: álcool etílico, acetonitrila, álcool isopropílico, acetona, álcool metílico, éter isopropílico, éter metil terc-butílico, tolueno, clorofórmio. A cristalização foi realizada por evaporação do solvente em diferentes temperaturas. A calorimetria exploratória diferencial (DSC), termogravimetria e termogravimetria derivada (TG/DTG), análise térmica diferencial (DTA), difração de raios X (DRX) e a ressonância magnética nuclear (RMN) foram às técnicas utilizadas na caracterização das formas polimórficas. A maioria das amostras obtidas pelas técnicas de cristalização consistiam de misturas de formas cristalinas, contendo, por vezes, formas metaestáveis e formas amorfas. Identificaram-se duas formas cristalinas como polimorfos da loratadina, cujas curvas DSC mostrou interconversão entre ambas. / The preparation, characterization and thermal behavior of the crystalline forms of the antihistamine loratadine has been developed. The selection of loratadine as an object of study results from its pharmacological interest. Loratadine is the International Common Denomination (ICD) given to ethyl 4-(8-chloro-5,6-dihydro-11H-benzo [5,6] cyclohepta[1,2-b]pyridin-11-ylidene)-1-piperidinecarboxylate, a potent anti-allergic and anti-histamincs, tricyclic, non-sedating long acting. Crystalline forms were prepared and studied for the identification of polymorphic forms. The solvents used in preparing the solutions were: ethanol, acetonitrile, isopropyl alcohol, acetone, methyl alcohol, isopropyl ether, methyl tert-butyl ether, toluene, chloroform. The crystallization was performed by evaporating the solvent at different temperatures. The differential scanning calorimetry (DSC), thermogravimetry and derivative thermogravimetry (TG/DTG), differential thermal analysis (DTA), X-ray diffraction (XRD) and nuclear magnetic resonance (NMR) techniques were used to characterize the polymorphic forms. Most of the samples obtained by the crystallization were mixtures of crystalline forms, containing sometimes forms metastable and amorphous forms. It was identified as two crystalline polymorphic forms of loratadine, whose DSC curves demonstrated that they are interconvertable.

Conselho Nacional de Desenvolvimento Científico e Tecnológico / In this work were obtained of Cu1-xMxO (M = Fe, Ni, Al e Zn, for 0 ≤ x ≤ 0,1 samples, using the co-precipitation method. These samples were studied using different techniques of characterization structural and magnetic. X-ray diffraction (XRD) results added to the Rietveld refinement analysis of the x-ray powder diffraction data shows that all samples present monoclinic the same structure of CuO with space group C2/c. The magnetization measurements as function of temperature (MvsT) show a fast suppress of TN for Fe-doped CuO samples, in contrast with (Ni, Zn and Al)-doped CuO. Synchrotron radiation XRD data at low temperature performed with show that the Cu0,9Fe0,1O and Cu0,9Ni0,1O samples present slow changes in the cell parameters, which it can be associated with the magnetic transition. Although the X-ray absorption (XAS) measurements performed in Cu K-edge show a variation in the density of unoccupied state in the p sublevel, appreciable changes in the local structure of these ions ban not be confirmed. On the other hand, measurements at the doping K and L2,3-edges confirm the existence of Ni2+ ions and oxygen vacancies and/or defect in your structure, already measurements performed in Cu0,9Fe0,1O sample shown the presence of Fe+2/Fe+3 mixed valence. / Neste trabalho foram obtidas amostras de Cu1-xMxO (M = Fe, Ni, Al e Zn) usando o método químico de co-precipitação. Estas amostras foram estudadas por diferentes técnicas de caracterização estrutural e magnética. Resultados de difração de raios X (DRX) associados às análises de refinamento Rietveld confirmam que todas as amostras de CuO dopadas com Fe, Ni, Al e Zn apresentaram estrutura cristalina similar a estrutura monoclínica do CuO puro, pertencente ao grupo espacial C2/c. As medidas de magnetização em função da temperatura (MvsT) mostram uma rápida supressão da temperatura de Néel (TN) de 210 K para 65 K, na amostras de CuO dopadas com 10% de Fe, em contraste com os sistema dopado com Ni, Zn e Al. Resultados de DRX em baixa temperatura usando radiação síncrotron indicam suaves alterações no parâmetro de rede das amostras de Cu0,9Fe0,1O e Cu0,9Ni0,1O, os quais podem estar associados com a transição magnética. Embora as medidas de absorção de raios X realizadas na borda K do Cu, antes e depois da TN, mostrarem uma variação na densidade de estado desocupado no subnível p, não se verificaram mudanças apreciáveis na estrutura local destes íons. Por outro lado, as medidas de absorção na borda K e L2,3 do dopante confirmam a existência de íons de Ni com estado de oxidação +2 e vacância de oxigênio e/ou defeitos na estrutura monoclínica do CuO dopado com Ni. Já nas medidas realizadas na amostra de Cu0,9Fe0,1O mostra a presença de valência mista de Fe+2/Fe+3 neste composto.