Dispersões sólidas de sinvastatina: preparação, caracterização, no estado sólido utilizando técnicas emergentes e estudo de estabilidade

This thesis aimed to assess the increase in solubility of simvastatin (SINV) with solid dispersions using techniques such as kneading (MA), co-solvent evaporation (ES), melting carrier (FC) and spray dryer (SD). Soluplus (SOL), PEG 6000 (PEG), PVP K-30 (PVP) e sodium lauryl sulphate (LSS) were used as carriers. The solid dispersions containing PEG [PEG-2(SD)], Soluplus [SOL-2(MA)] and sodium lauryl sulphate [LSS-2(ES)] were presented with a greater increase in solubility (5.02, 5.60 and 5.43 times respectively); analyses by ANOVA between the three groups did not present significant difference (p<0.05). In the phase solubility study, the calculation of the Gibbs free energy (ΔG) revealed that the spontaneity of solubilisation of SINV occurred in the order SOL>PEG >PVP 75%>LSS, always 80%. The phase diagrams of PEG and LSS presented solubilization stoichiometry of type 1:1 (type AL). The diagrams with PVP and SOL tend to 1:2 stoichiometry (type AL + AP). The stability coefficients (Ks) of the phase diagrams revealed that the most stable reactions occurred with LSS and PVP. The solid dispersions were characterized by Fourier transform infrared (FTIR), differential scanning calorimetry (DSC), scanning electron microscopy (SEM), particle size distribution (PSD), near-infrared spectroscopy imaging (NIR-CI) and X-ray diffraction of the powder using the Topas software (PDRX-TOPAS). The solid dispersion PEG-2(SD) presented the greatest homogeneity and the lowest degree of crystallinity (18.2%). The accelerated stability study revealed that the solid dispersions are less stable than SINV, with PEG-2(SD) being the least stable, confirmed by FTIR and DSC. The analyses by PDRX-TOPAS revealed the amorphous character of the dispersions and the mechanism of increasing solubility

Superfícies geomórficas e atributos de Latossolos em uma seqüência Arenítico-Basáltica da região de Jaboticabal (SP)

Em um segmento de vertente com substrato de arenito em contato com basalto, regionalmente muito freqüente, pretendeu-se não só relacionar as superfícies geomórficas com os atributos físicos, químicos e mineralógicos dos Latossolos nelas encontrados, mas também testar métodos geoestatísticos para localização de limites dessas superfícies. Usando critérios geomorfológicos, três superfícies foram identificadas e topograficamente caracterizadas. Os solos foram amostrados, a intervalos regulares de 25 m, na profundidade de 0,6 a 0,8 m (topo do horizonte B), em uma transeção de 1.700 m perfazendo 109 pontos. Nas amostras, foram analisados: densidade de partículas, granulometria, CTC do solo, CTC da argila, Fe total da argila (ataque por H2SO4) e óxidos de Fe livres (por dissolução seletiva). A fração argila desferrificada foi analisada por difração de raios X. Com base na estratigrafia e variações do relevo local, foram identificadas e diferenciadas, no campo, três superfícies geomórficas. Analisaram-se também o perfil altimétrico e o modelo de elevação digital do terreno. Observou-se que as três diferentes superfícies estão bem relacionadas com os atributos físicos, químicos e mineralógicos dos seus respectivos solos. Na parte inferior desta vertente, superfície mais recente e sobre basalto, em Latossolo Vermelho eutroférrico típico, foram encontradas as maiores variabilidades da declividade, da argila e de Fe. As variações da inclinação do terreno, quando analisadas sistematicamente pelo split moving windows dissimilarity analysis (análise estatística de dissimilaridade, em segmentos móveis), mostraram que este método estatístico pode ser usado para ajudar a localizar os limites entre superfícies geomórficas. As variações dos solos da transeção, e arredores, mostraram-se relacionadas com idade, inclinação do terreno e litologia. O trabalho geomórfico detalhado forneceu importantes informações para subsidiar os trabalhos de levantamento de solos e de pedogênese.

Variação espacial da perda de solo por erosão em diferentes superfícies geomórficas

O objetivo deste trabalho foi estudar a influência das superfícies geomórficas na variação espacial da perda de solo por erosão na região de Pereira Barreto, São Paulo (SP). Os solos foram amostrados nos pontos de cruzamento de uma malha, georreferenciados, com intervalos de 350m, na profundidade de 0,0-0,2m, totalizando 67 pontos. Foram feitas determinações da composição granulométrica e do conteúdo de matéria orgânica. Foram avaliados os fatores de erosão locais, tais como erosividade (R), erodibilidade (K), fator topográfico (LS), uso e manejo (C), práticas conservacionistas (P), potencial natural de erosão (PNE), perda de solo com e sem práticas conservacionistas (A e *A), tolerância de perda de solo (T) e risco de erosão (RE). As variáveis A, PNE e RE apresentaram forte correlação espacial com o fator topográfico (LS), indicando a forte relação do relevo sobre os fatores de erosão. As perdas de solo (A e *A) apresentaram comportamento coerente com a conceituação de superfícies geomórficas, evidenciando as relações de dependência do processo erosivo do solo aos ambientes geomórficos.

Variabilidade espacial de atributos do solo e de fatores de erosão em diferentes pedoformas

As formas do relevo podem ser indicadores da variação dos atributos do solo, pois essa variabilidade é causada por pequenas alterações do declive que afetam os processos pedogenéticos bem como o transporte e o armazenamento de água no perfil do solo. O trabalho foi desenvolvido em Catanduva (SP), com o objetivo de caracterizar a variabilidade espacial de atributos do solo e fatores de erosão em diferentes pedoformas sob cultivo de cana-de-açúcar. de acordo com o modelo de Troeh classificou-se as formas do relevo em duas pedoformas, côncava e convexa. Com a utilização de um DGPS levantaram-se as cotas altimétricas, estabelecendo-se uma malha, com intervalos regulares de 50 m, com 270 pontos na pedoforma côncava e 353 pontos na pedoforma convexa, perfazendo um total de 623 pontos, coletados na profundidade de 0,0 - 0,2 m em uma área de 200 ha. em cada ponto da malha foram determinados os atributos químicos do solo, granulometria, espessura do solo e fatores de erosão locais, tais como erosividade (R), erodibilidade (K), fator topográfico (LS), uso e manejo (C), práticas conservacionistas (P), potencial natural de erosão (PNE), perda de solo (A) e risco de erosão (RE). Os dados foram avaliados primeiramente por uma análise estatística exploratória, calculando-se a média, mediana, variância, coeficiente de variação, coeficiente de assimetria, coeficiente de curtose e teste de normalidade. Posteriormente, a dependência espacial foi verificada por meio da técnica de geoestatística utilizando-se semivariogramas. As maiores perdas de solo, risco de erosão e potencial natural de erosão e menor espessura do solo ocorreram na pedoforma convexa, indicando forte dependência espacial com a forma do relevo. A pedoforma côncava proporcionou maior variabilidade espacial, demonstrando que a forma do relevo condiciona padrões diferenciados de variabilidade. A magnitude da variabilidade dos atributos do solo é mais influenciada pela forma do relevo que pela erosão. A espessura do horizonte A+E integrado com a forma do relevo é um indicador de processos erosivos para classe de Argissolos.

Estudo da formulação de massas cerâmicas provenientes da região do Seridó-RN para fabricação de telhas

This work has for objective study compared the characteristics and technological properties of ceramic bodies from the region of Seridó-RN. The region under study has identified 23 cities where they were 80 ceramics industries. To define the universe of search, there was a survey of pottery that are part of APL Seridó next to the IEL. The characteristics and operating conditions of ceramics industries of the region were identified through a socio-economic questionnaire applied locally, which addressed issues such as: profiles of companies, production process etc. The analysis of information collected from 24 companies identified in seven cities shows that the vast majority of industries is small, with family structure, obsolete equipment and labo, little qualified. Most of the pottery works with low technical knowledge, poor control of the production process and product technology. The raw collected were submitted to analysis of X ray diffraction, chemical composition, termical analysis, particle size distribution and plasticity. Then were produced five formulations and made by uniaxial pressure at 25 MPa for firing in temperatures varying from 850 to 1050 °C. The firing technological properties evaluated were: mass loss to fire, lineal shrinkage, apparent density, apparent porosity, water absorption and flexural strength (3 points). The results indicated that the raw materials from the region have significant similarities in the composition chemical and mineralogical. Furthermore, it indicates the possibility of the use of cycles of firing faster and efficient than the current, limited to some clay mass burning of certain conditions

Estudo e caracterização de matérias-primas para o desenvolvimento de blocos sílico-calcários

The types of products manufactured calcium silicate blocks are very diversified in its characteristics. They include accessory bricks, blocks, products in dense material, with or without reinforcements of hardware, great units in cellular material, and thermal insulating products. The elements calcium silicate are of great use in the prefabricated construction, being formed for dense masses and hardened by autoclaving. This work has for objective develop formulations that make possible the obtaining of calcium silicate blocks with characteristics that correspond the specifications technical, in the State of the Rio Grande of the North, in finality of obtaining technical viability for use in the civil construction. The work studied the availability raw materials from convenient for the production of calcium silicate blocks, and the effect of variations of the productive process on the developed products. The studied raw materials were: the quartz sand from the city of São Gonçalo do Amarante/RN, and two lime, a hydrated lime and a pure lime from the city of Governador Dix-Sept Rosado/RN. The raw materials collected were submitted a testes to particle size distribution, fluorescence of X rays, diffraction of X rays. Then were produced 8 formulations and made body-of-test by uniaxial pressing at 36 MPa, and cured for 7 hours at about 18 kgf/cm2 pressing and temperature of approximately 180 °C. The cure technological properties evaluated were: lineal shrinkage, apparent density, apparent porosity, water absorption, modulus of rupture flexural (3 points), resistance compression, phase analysis (XRD) and micromorphological analysis (SEM). From the results presented the technological properties, was possible say that utilization of hydrated lime becomes more viable its utilization in mass limestone silica, for manufacture of calcium silicate blocks

Estudo de formulação de massa para aplicação em placas cerâmicas

The sector of civil construction is strongly related to the red ceramic industry. This sector uses clay as raw material for manufacturing of various products such as ceramic plates. In this study, two types of clay called clay 1 and clay 2 were collected on deposit in Ielmo Marinho city (RN) and then characterized by thermogravimetric analysis (TG/DTG), differential thermal analysis (DTA), X-ray diffraction (XRD), X-ray fluorescence (XRF), rational analysis and particle size distribution and dilatometric analyses. Ceramic plates were manufactured by uniaxial pressing and by extrusion. The plates obtained by pressing were produced from the four formulations called 1, 2, 3 and 4, which presented, respectively, the following proportions by mass: 66.5% clay 1 and 33.5% clay 2, 50% clay 1 and 50% clay 2, 33.5% clay 1 and 66.5% clay 2, 25% clay 1 and 75% clay 2. After firing at 850, 950 and 1050 °C with heating rate of 10 °C/min and soaking time of 30 minutes, the following technological properties were determined: linear firing shrinkage, water absorption, apparent porosity, apparent specific mass and tensile strength (3 points). The formulation containing 25% clay 1 produced plates with most satisfactory results of water absorption and mechanical resistance, because of that it was chosen for manufacturing plates by extrusion. A single firing cycle was established for these plates, which took place as follow: heating rate of 2 °C/min up to 600 ºC with soaking time of 60 minutes, followed by heating using the same rate up to 1050 ºC with soaking time of 30 minutes. After this cycle, the same technological properties investigated in the plates obtained by pressing were determined. The results indicate (according to NRB 13818/1997) that the plates obtained by pressing from the mixture containing 25 wt% clay 1, after firing at 1050 °C, reach the specifications for semi-porous coating (BIIb). On the other hand, the plates obtained by extrusion were classified as semi-stoneware (group AIIa)

Formação de particulas submicrometricas de pmma por cristalização termica de solução polimérica

Polymer particles in the nanometer range are of fundamental interest today, especially when used as carrier systems in the controlled release of drugs, cosmetics and nutraceuticals, as well as in coating materials with magnetic properties. The main objective of the present study concerns the production of submicron particles of poly (methyl methacrylate) (PMMA) by crystallization of a polymer solution by thermally controlled cooling. In this work, PMMA solutions in ethanol and 1-propanol were prepared at different concentrations (1% to 5% by weight) and crystallized at different cooling rates (0.2 to 0.8 ° C / min) controlled linearly. Analysis of particle size distribution (DLS / CILAS) and scanning electron microscopy (SEM) were performed in order to evaluate the morphological characteristics of the produced particles. The results demonstrated that it is possible to obtain submicron polymer perfectly spherical particles using the technique discussed in this study. It was also observed that, depending on the cooling rate and the concentration of the polymer solution, it is possible to achieve high yield in the formation of submicron particles. In addition, preliminary tests were performed in order to verify the ability of this technique to form particulated carrier material with magnetic properties. The results showed that the developed technique can be an interesting alternative to obtain polymer particles with magnetic properties

Desenvolvimento de um secador spray para obtenção de pós finos de precursores de nióbio

This work presents a spray-dryer designed to oxalate-niobate precursors and suitable for the production of Niobium Carbide. The dryer was intended to produce powders of controlled particle size. First, the precursor is dissolved in water to produce a solution of known concentration and then it is atomized on the spray-dryer to produce the powder. This equipment consists of a 304 stainless steel chamber, 0.48 m x 1.9 m (diameter x length), with a conical shape at the lower portion, which is assembled on a vertical platform. The chamber is heated by three 4 kW electrical resistances. In this process, drying air is heated as it flows inside a serpentine surrounding the chamber, in contrary to more traditional processes in which the hot drying air is used to heat the component. The air enters the chamber at the same temperature of the chamber, thus avoiding adherence of particles on the internal surface. The low speed flow is concurrent, directed from the top to the bottom portion of the chamber. Powders are deposited on a 0.4 m diameter tray, which separates the cylindrical portion from the conical portion of the chamber. The humid air is discharged though a plug placed underneath the collecting tray. A factorial experimental planning was prepared to study the influence of five parameters (concentration, input flow, operation temperature, drying air flow and spray air flow) on the characteristics of the powders produced. Particle size distribution and shape were measured by laser granulometry and scanning electronic microscopy. Then, the powders are submitted to reaction in a CH4 / H2 atmosphere to compare the characteristics of spray-dried powders with powders synthetizided by conventional methods

Caracterização do lodo de lagoa anaeróbia tratando resíduos esgotados de tanques sépticos e fossas com vistas ao aproveitamento

The sludge generated in stabilization ponds can be designed for various purposes, among them we mention agricultural use, recovery of degraded areas and civil construction. The choice of these alternatives should be made based on qualitative and quantitative characteristics of the sludge. In this context, this study characterized the digested sludge from an anaerobic lagoon in Cidade do Natal/RN, which deals exclusively with residues of depleted septic tanks and pits. The sludge showed levels of macro and micronutrients that confirm its potential for agriculture, with 139.49 g.kg -1 organic matter, 15.40 g.kg-1 nitrogen and metal concentrations below those required by Resolution No. 375/06 of CONAMA, besides the absence of fecal coliform and less than 0.15 viable helminthes eggs/g, on average. The particle size distribution showed that most of the particles have a diameter similar to the sand, allowing the replacement of this input, for example. Analysis of the leachate and of the sludge solubilized classified as non-inert and non-hazardous according to NBR 10.004/04. The volume produced in three years of operation by the pond was 1903.50m³, equivalent to approximately 400 kg of dry sludge. Overall, the concentrations of the parameters were similar to literature, although none of them addresses sludge anaerobic pond treating sewer from septic tanks and pits.The sludgepresents technical feasibility to various types of use, however the cost of dewatering and especially with transport can derail it. It needs to be made a more thorough study of the costs to prove its economic viability

Europium luminescent polymeric microspheres fabricated by spray drying process

The spray drying method was used to prepare luminescent microspheres. These microspheres were prepared by spraying an aqueous solution of dextrin and an europium(III) complex with subsequent drying in a hot medium. The spray dried powder was characterized by scanning electron microscopy (SEM) and photoluminescence spectroscopy (PL). Particle size distribution was estimated from SEM images. The ultrasonic spray drying technique was successfully applied to yield a microparticulated and red luminescent powder composed by the [Eu(dpa)(3)](3-) stop (dpa = dipicolinic acid) complex incorporated in dextrin microspheres.

Structural and morphological characteristics of (Pb1-x Sr (x) )TiO3 powders obtained by polymeric precursor method

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Caracterização dos eletrocatalisadores LaMnO3, LaFeO3, LaFe0,2Mn0,8O3 E La0,5Fe0,5MnO3 preparados por autocombustão assistida por microondas para cátodos de células a combustível do tipo SOFC

Materials consisting of perovskite-type oxides (ABO3) have been developed in this work for applications in fuel cell cathodes of solid oxide type (SOFC). These ceramic materials are widely studied for this type of application because they have excellent electrical properties, conductivity and electrocatalytic. The oxides LaMnO3, LaFeO3, LaFe0.2Mn0.8O3 e La0.5Fe0.5MnO3 were synthesized by the method of microwave assisted combustion and after sintering at 800°C in order to obtain the desired phases. The powders were characterized by thermogravimetry (TG), X-ray diffraction (XRD), X-ray fluorescence (XRF), scanning electron microscopy (SEM) and voltammetric analysis (cyclic voltammetry and polarization curves). The results obtained by XRF technique showed that the microwave synthesis method was effective in obtaining doping oxides with values near stoichiometric. In general, powders were obtained with particle size less than 0.5 μm, having a porous structure and uniform particle size distribution. The particles showed spherical form, irregular and crowded of varying sizes, according to the analysis of SEM. The behavior of the oxides opposite the thermal stability was monitored by thermogravimetric curves (TG), which showed low weight loss values for all samples, especially those of manganese had its structure. By means of Xray diffraction of the samples sintered at 800°C was possible to observe the formation of powders having high levels of crystallinity. Furthermore, undesirable phases such as La2O3 and MnOx were not identified in the diffractograms. These phases block the transport of oxygen ions in the electrode/electrolyte interface, affecting the electrochemical activity of the system. The voltammetric analysis of the electrocatalysts LF-800, LM-800, LF2M8-800 e L5F5M-800 revealed that these materials are excellent electrical conductors, because it increased the passage of electrical current of the working electrode significantly. Best performance for the oxygen reduction reaction was observed with iron-rich structures, considering that the materials obtained have characteristics suitable for use in fuel cell cathodes of solid oxide type

Interações entre a carboximetilcelulose, carbonato de cálcio e bentonita: repercussões sobre as propriedades dos fluidos de perfuração aquosos

The role of carboxymethylcellulose (CMC) in association to calcium carbonate particles (CaCO3) in most water-based drilling fluids is to reduce the fluid loss to the surrounding formation. Another essential function is to provide rheological properties capable of maintaining in suspension the cuttings during drilling operation. Therefore, it is absolutely essential to correlate the polymer chemical structure (degree of substitution, molecular weight and distribution of substituent) with the physical-chemical properties of CaCO3, in order to obtain the better result at lower cost. Another important aspect refers to the clay hydration inhibitive properties of carboxymethylcellulose (CMC) in drilling fluids systems. The clay swelling promotes an undesirable damage that reduces the formation permeability and causes serious problems during the drilling operation. In this context, this thesis consists of two main parts. The first part refers to understanding of interactions CMC-CaCO3, as well as the corresponding effects on the fluid properties. The second part is related to understanding of mechanisms by which CMC adsorption occurs onto the clay surface, where, certainly, polymer chemical structure, ionic strength, molecular weight and its solvency in the medium are responsible to affect intrinsically the clay layers stabilization. Three samples of carboximetilcellulose with different molecular weight and degree of substitution (CMC A (9 x 104 gmol DS 0.7), CMC B (2.5 x 105 gmol DS 0.7) e CMC C (2.5 x 105 gmol DS 1.2)) and three samples of calcite with different average particle diameter and particle size distribution were used. The increase of CMC degree of substitution contributed to increase of polymer charge density and therefore, reduced its stability in brine, promoting the aggregation with the increase of filtrate volume. On the other hand, the increase of molecular weight promoted an increase of rheological properties with reduction of filtrate volume. Both effects are directly associated to hydrodynamic volume of polymer molecule in the medium. The granulometry of CaCO3 particles influenced not only the rheological properties, due to adsorption of polymers, but also the filtration properties. It was observed that the lower filtrate volume was obtained by using a CaCO3 sample of a low average size particle with wide dispersion in size. With regards to inhibition of clay swelling, the CMC performance was compared to other products often used (sodium chloride (NaCl), potassium chloride (KCl) and quaternary amine-based commercial inhibitor). The low molecular weight CMC (9 x 104 g/mol) showed slightly lower swelling degree compared to the high molecular weight (2.5 x 105 g/mol) along to 180 minutes. In parallel, it can be visualized by Scanning Electron Microscopy (SEM) that the high molecular weight CMC (2.5 x 105 g/mol e DS 0.7) promoted a reduction in pores formation and size of clay compared to low molecular weight CMC (9.0 x 104 g/mol e DS 0.7), after 1000 minutes in aqueous medium. This behavior was attributed to dynamic of interactions between clay and the hydrodynamic volume of CMC along the time, which is result of strong contribution of electrostatic interactions and hydrogen bounds between carboxylate groups and hydroxyls located along the polymer backbone and ionic and polar groups of clay surface. CMC adsorbs on clay surface promoting the skin formation , which is responsible to minimize the migration of water to porous medium. With the increase of degree of substitution, it was observed an increase of pores onto clay, suggesting that the higher charge density on polymer is responsible to decrease its flexibility and adsorption onto clay surface. The joint evaluation of these results indicate that high molecular weight is responsible to better results on control of rheological, filtration and clay swelling properties, however, the contrary effect is observed with the increase of degree of substitution. On its turn, the calcite presents better results of rheological and filtration properties with the decrease of average viii particle diameter and increase of particle size distribution. According to all properties evaluated, it has been obvious the interaction of CMC with the minerals (CaCO3 and clay) in the aqueous medium

Desenvolvimento de uma rota química alternativa de síntese de SrCo0,8Fe0,2O3- e LaNi0,3Co0,7O3- para aplicação na reação de oxidação do CO

This thesis focuses on the coprecipitation synthesis method for preparation of ceramic materials with perovskite structure, their characterization and application as catalytic material in the reaction of converting CO to CO2 developing a methodological alternative route of synthesis from the middle via oxalate coprecipitation material SrCo0,8Fe0,2O3-d. In order to check the influence of this method, it was also synthesized using a combined citrate - EDTA complexing method. The material was characterized by: X-ray diffraction (XRD), Rietveld refinement method, thermogravimetry and differential thermo analysis (TG / DTA), scanning (SEM) and transmission (TEM) electron microscopy, particle size distribution and surface analysis method BET. Both methods led to post-phase synthesis, with pH as a relevant parameter. The synthesis based on the method via oxalate coprecipitation among particles led to the crystalline phase as those obtained using a combined citrate - EDTA complexing method under the same conditions of heat treatment. The nature of the reagent used via oxalate coprecipitation method produced a material with approximately 80 % lower than the average size of crystallites. Moreover, the via oxalate coprecipitation method precursors obtained in the solid state at low temperature (~ 26 oC), shorter synthesis, greater thermal stability and a higher yield of around 90-95 %, maintaining the same order of magnitude the crystallite size that the combined citrate - EDTA complexing method. For purposes of comparing the catalytic properties of the material was also synthesized by the using a combined citrate - EDTA complexing method. The evaluation of catalytic materials SrCo0,8Fe0,2O3-d LaNi0,3Co0,7O3-d was accompanied on the oxidation of CO to CO2 using a stainless steel tubular reactor in the temperature range of 75-300 oC. The conversion CO gas was evaluated in both materials on the results shaved that the firm conversion was loves for the material LaNi0,3Co0,7O3-d