23 resultados para Reprodutibilidade


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Two pillaring methods were tested to synthesize pillared clays containing mixed Al/Co pillars. Using the first method, based on the traditional procedure, were obtained materials containing different Co concentrations: 10, 25, 50, 75 and 100 % of Co in the pillaring solution. Just the experiments with low concentrations (10 and 25 % of Co) has formed pillared clays, whereas the sample with 25 % of cobalt showed best results compared with the one obtained just using Al as pillaring agent (basal spacing higher than 18 Å and surface area bigger than 300 m²/g). The 27Al NMR results pointed out the formation of mixed Al/Co pillars due to decreased between the intensities of AlVI/AlIV signals, indicating that the AlIV content decreased while Co content increased, suggesting the isomorphic substitution of Al atoms for Co in the Keggin ion structure (pillaring agent). For the samples containing 75 and 100 % of cobalt, it was verified the formation of others materials, which could be identified as hydrotalcite like compounds. The second pillarization method was named mixed layers, because the objective was to intercalate clay layers with hydrotalcite layers. Thus, after calcination, the hydrotalcite layers would dehydroxylate, resulting just in the metals oxides, intercalated between the clay sheets, thus generating, a pillared clay. For this purpose, were tested 4 synthesis procedures: physical mixture, mixture in water, ionic exchange under reflux and in situ synthesis. Of these, the method which showed the best results was the in situ synthesis, in which basal spacings of 14 Å (after calcination) were obtained, indicating that the samples are intercalated with metal oxides (Mg and Al). This procedure was reproduced with a Co-Al LDH (layered double hydroxide) and similar results were obtained, testifying the method reproducibility

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The processing of heavy oil produced in Brazil is an emergency action and a strategic plan to obtain self-sufficiency and economic surpluses. Seen in these terms, it is indispensable to invest in research to obtain new catalysts for obtaining light fraction of hydrocarbons from heavy fractions of petroleum. This dissertation for the degree of Doctor of Philosophy reports the materials preparation that combine the high catalytic activity of zeolites with the greater accessibility of the mesoporosity, more particularly the HZSM-5/MCM-41 hybrid, done by synthesis processes with less environmental impact than conventional ones. Innovative methodologies were developed for the synthesis of micro-mesoporous hybrid material by dual templating mechanism and from crystalline zeolitic aluminosilicate in the absence of organic template. The synthesis of hybrid with pore bimodal distribution took place from one-single organic directing agent aimed to eliminate the use of organic templates, acids of any kind or organic solvents like templating agent of crystalline zeolitic aluminosilicate together with temperature-programmed microwave-assisted, making the experimental procedures of preparation most practical and easy, with good reproducibility and low cost. The study about crystalline zeolitic aluminosilicate in the absence of organic template, especially MFI type, is based on use of H2O and Na+ cation playing a structural directing role in place of an organic template. Advanced characterization techniques such as X-Ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), Scanning Electron Microscopy (SEM), Highresolution Transmission Electron Microscopy (HRTEM), Adsorption of N2 and CO2, kinetic studies by Thermogravimetric Analysis (TGA) and Pyrolysis coupled to Gas Chromatography/Mass Spectrometry (Pyrolysis-GC/MS) were employed in order to evaluate the synthesized materials. Achieve the proposed objectives, has made available a set of new methodologies for the synthesis of zeolite and hybrid micro-mesoporous material, these suitable for catalytic pyrolysis of heavy oils aimed at producing light fraction

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Ceramic pigments that own mainly the spinel structure AB2O4 are becoming a matter of great scientific and technological interest due to the ability of accommodate different cations in its structure, allowing different dopings and thus obtaining different colors. Studies on ceramic pigments currently are being directed to the development of stable and pigments obtained at low temperatures and with greater reproducibility. This work aims at the use of inorganic pigments for applications in ceramic tiles, investigating the influence of doping and calcination temperature on the coloring pigments and ceramic glazes. the based pigments of CoCr2O4, CoAl2O4, Co0,8Zn0,2Cr2O4 and Co0,8Zn0,2Al2O4 were synthesized by a chemical route using commercial gelatin as organic precursor. The materials were characterized by thermogravimetric analysis (TG), X-ray diffraction (XRD), infrared spectroscopy (FTIR) spectroscopy scanning electron microscopy (SEM) in the UVVisible region and colorimetry. The results confirmed the feasibility of synthesis used, the route presented pigments crystal structures and the desired phases were obtained from 500 °C with increased crystallinity and the crystallite size. The pigments have hues ranging from green to violet according to their doping and calcination temperatures.

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OBJETIVO: Analizar limitaciones del estudio de fluorosis dentaria en pesquisas transversales. MÉTODOS: Se utilizaron datos de estudios de de Condiciones de Salud Bucal de la Población Brasileña (SBBrasil 2003) y de la Investigación Nacional de la Salud Bucal (SBBrasil 2010). La estimativa de tendencia epidemiológica de la fluorosis en la población de 12 años, aspectos de la confiabilidad de los datos, así como la precisión de las estimativas, fueron evaluadas en estas dos investigaciones. La distribución de la prevalencia de la fluorosis fue hecha de acuerdo con los dominios de estudio (capitales y regiones) y el año estudiado. Se expresaron también los intervalos de confianza (IC95%) para la prevalencia simple (sin considerar las fases de la gravedad). RESULTADOS: La prevalencia de la fluorosis dentaria presentó una variación considerable, de 0 a 61% en 2003 y de 0 a 59% en 2010. Se observaron inconsistencias en los datos en términos individuales (por año y por dominio) y en el comportamiento de la tendencia. Considerando la expectativa de prevalencia y los datos disponibles en las dos investigaciones, el tamaño mínimo de la muestra debería ser de 1.500 individuos para obtener intervalos de 3,4% y 6,6% de confianza, considerando un coeficiente de variación mínimo de 15%. Dada la subjetividad en la naturaleza de su clasificación, exámenes de fluorosis dentaria pueden presentar más variación de los realizados para otras condiciones de salud bucal. El poder para establecer diferencias entre los dominios del estudio con la muestra de SBBrasil 2010 es bastante limitado. CONCLUSIONES: No fue posible analizar la tendencia de la fluorosis dentaria en Brasil con base en los estudios de 2003 y 2010; esos datos son sólo indicadores exploratorios de la prevalencia de la fluorosis. La comparación se hace imposible por el hecho de haber sido utilizado modelos de análisis diferentes en las dos pesquisas. La investigación de la fluorosis dentaria en pesquisas de base poblacional no es viable técnica y económicamente, la realización de estudios epidemiológicos localizados con plan de muestreo es más adecuada.

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Epidemiological surveys are important for obtaining information on the prevalence and etiology of mouth diseases, since the data collected permit health actions to be planned, performed, and assessed. Methodological uniformity is necessary, however, to maintain reproductibility, validity, and reliability, and to allow national and international comparisons. The initiative of the World Health Organization (WHO) as an advisor in ongoing surveys has been extremely useful, stimulating standardization in all countries. In 1991, a Portuguese version of the 1987 third edition of Oral Health Surveys - basic methods, an instruction manual for performing epidemiological surveys, was published and became a reference for many parts of Brazil and the World. The present analysis found conflicting points in relation to the sample size, calibration of the examiners, and criteria for evaluating oral health and treatment needs. In conclusion, due to the dynamic characteristics of scientific knowledge and, considering the regional differences in relation to the development of oral diseases, we recommend that proposals for standardizing surveys be checked periodically. Other important issues may have not been detected in this analysis, urging a thorough discussion within the dentistry community as a whole.

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Epidemiological surveys are important for obtaining information on the prevalence and etiology of mouth diseases, since the data collected permit health actions to be planned, performed, and assessed. Methodological uniformity is necessary, however, to maintain reproductibility, validity, and reliability, and to allow national and international comparisons. The initiative of the World Health Organization (WHO) as an advisor in ongoing surveys has been extremely useful, stimulating standardization in all countries. In 1991, a Portuguese version of the 1987 third edition of Oral Health Surveys - basic methods, an instruction manual for performing epidemiological surveys, was published and became a reference for many parts of Brazil and the World. The present analysis found conflicting points in relation to the sample size, calibration of the examiners, and criteria for evaluating oral health and treatment needs. In conclusion, due to the dynamic characteristics of scientific knowledge and, considering the regional differences in relation to the development of oral diseases, we recommend that proposals for standardizing surveys be checked periodically. Other important issues may have not been detected in this analysis, urging a thorough discussion within the dentistry community as a whole.

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The worldwide concern regarding the use of sustainable energy and preserving the environment are determining factors in the search for resources and alternative sources of energy and therefore fuel less aggressive nature. In response to these difficulties Biodiesel has emerged as a good solution because it is produced from renewable sources, produces burns cleaner and is easily reproducible. This work was synthesized with biodiesel oil, sunflower via homogeneous catalysis in the presence of KOH, with and without the use of BHT and subsequently added to the blends BX (a proportion of biodiesel X = 5, 10, 15 and 20 %). Atmospheric distillation of the analysis, performed in blends with and without BHT were collected residue generated by each sample and performed a study heat from the thermogravimetric analysis at a heating rate of 10 °C*min-1, nitrogen atmosphere and heating to 600 °C. According to the specifications of Resolution N 7/2008 for biodiesel, it was found that the synthesized material was in accordance with the specifications. For blends showed that the samples are in accordance with the Resolution of ANP N 42/2009. From the TG / DTG curves of the samples of biodiesel, blends and waste can be seen that these show a single loss of thermal decomposition concerning constituents present in each sample. The blends without BHT with ratios of 5%, 10% and 15% biodiesel showed a lower amount of waste (1,07%; 1,09% e 1,10%) to mineral diesel (1,15%). Therefore, it is concluded that the addition of biodiesel with diesel mineral can improve some physico-chemical parameters, but also, depending on the added amount, decreasing the amount of waste generated. This fact is of great importance because the carbonaceous residue can cause problems in mechanical equipment and parts for vehicles, causing more frequent maintenance, and this is not desirable

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The growing world demand for energy supplied by fossil fuels, a major contributor to the emission of pollutants into the atmosphere and causing environmental problems, has been encouraging governments and international organizations to reflect and encourage the use of alternative renewable sources. Among these new possibilities deserves attention biodiesel, fuel cleaner and easy to reproduce. The study of new technologies involving that source is necessary. From this context, the paper aims at analyzing the thermal stability by thermogravimetric analysis, of the waste generated from atmospheric distillation of mixtures with ratios of 5, 10, 15 and 20% palm biodiesel in diesel with and without addition of BHT antioxidant. It was synthesized biodiesel through palm oil, via homogeneous catalysis in the presence of KOH, with and without the use of BHT and subsequently added to the diesel common indoor type (S1800) from a gas station BR. The diesel was already added with 5% biodiesel, and thus the proportions used for these blends were subtracted from the existing ratio in diesel fuel, resulting in the following proportions palm oil biodiesel: 0% (B5), 5% (B10), 10 % (B15) and 15% (B20). From atmospheric distillation analysis, performed in mixtures with and without BHT were collected residue generated by each sample and performed a thermal study from the thermogravimetric analysis at a heating rate of 10 °C.min-1, nitrogen atmosphere and heating to 600 ° C. According to the specifications of Resolution No. 7/2008 for biodiesel, it was found that the material was synthesized in accordance with the specifications. For mixtures, it was noted that the samples were in accordance with the ANP Resolution No. 42/2009. Given the TG / DTG curves of the samples of waste mixtures with and without BHT antioxidant was able to observe that they showed a single stage of thermal decomposition attributed to decomposition of heavy hydrocarbons and esters and other heavier constituents of the waste sample weighed. The thermal behavior of residues from atmospheric distillation of mixtures of diesel / biodiesel is very important to understand how this affects the proper functioning of the engine. A large amount of waste can generate a high content of particulate material, coke formation and carbonaceous deposits in engine valves, compromising their performance