Degradacao termica e catalitica da borra oleosa de Petroleo com materiais nanoestruturados al-mcm-41 e AL-SBA-15

Aiming to reduce and reuse waste oil from oily sludge generated in large volumes by the oil industry, types of nanostructured materials Al-MCM-41 and Al-SBA-15, with ratios of Si / Al = 50, were synthesized , and calcined solids used as catalysts in the degradation of oily sludge thermocatalytic oil from oilfield Canto do Amaro, in the state of Rio Grande do Norte. Samples of nanostructured materials were characterized by thermogravimetric analysis (TG / DTG), X-ray diffraction (XRD), scanning electron microscopy (SEM), absorption spectroscopy in the infrared Fourier transform (FT-IR) and adsorption nitrogen (BET). The characterization showed that the synthesized materials resulted in a catalyst nanostructure, and ordered pore diameter and surface area according to existing literature. The oily sludge sample was characterized by determining the API gravity and sulfur content and SARA analysis (saturates, aromatics, resins and asphaltenes). The results showed a material equivalent to the average oil with API gravity of 26.1, a low sulfur content and considerable amount of resins and asphaltenes, presented above in the literature. The thermal and catalytic degradation of the oily sludge oil was performed from room temperature to 870 ° C in the ratios of heating of 5, 10 and 20 ° C min-1. The curves generated by TG / DTG showed a more accelerated degradation of oily sludge when it introduced the nanostructured materials. These results were confirmed by activation energy calculated by the method of Flynn-Wall, in the presence of catalysts reduced energy, in particular in the range of cracking, showing the process efficiency, mainly for extraction of lightweight materials of composition of oily sludge, such as diesel and gasoline

Determinação da idade dental de crianças brasileiras nordestinas: novos valores de conversão de maturidade dental para população específica

Since Demirjian's system of estimating dental maturity was first described, many researchers from different countries have tested its accuracy among diverse populations. Some of these studies have pointed out a need to determine population-specific standards. In Brazil, the Northeast region is the one that most suffers the negative impact of exodus, specially related to the increase of abandoned children in the cities. The aim of this study was to test the accuracy of Demirjian's system for assessing the dental maturity of northeastern Brazilian children, so as to present a scale for maturity score conversion into dental age developed specifically for this population. This could be used for forensic, anthropological and legal matters, and also as a model for other countries attempting to formulate their own conversion scales. Panoramic radiographs of 1,491 children (821 females and 670 males), aged 7 to 13 years, from Ceará state, northeast Brazil, were assessed by a single observer to determine dental age (DA) according to Demirjian's system. The mean percentage of intra-observer agreement was 86.6%, with a mean Cohen's Kappa coefficient of 0.67 (substantial agreement). The DA was compared by paired t-test to subjects' chronological age (CA). The differences between CA and DA in all age groups were statistically significant (p<0.0001), demonstrating a great advancement in DA among Brazilians. Scatter plots were drawn for both genders, and the data were fitted to a growth curve, y = 100/ (1 + e-a(x b)). Graphs corresponding to the 50th percentile curves were produced. A table with new values for the conversion of maturity score into dental age for northeastern Brazilian children is presented. The great advancement in DA, as obtained by Demirjian's system in this population, justified the determination of specific scores for dental maturity assessment

Identificação e avaliação de propriedades de polissacarídeos sulfatados de diferentes fontes naturais que possibilitem sua aplicabilidade biotecnológica

Sulfated polysaccharides (SP) are widely distributed in animals and seaweeds tissues. These polymers have been studied in light of their important pharmacological activities, such as anticoagulant, antioxidant, antitumoral, anti-inflammatory, and antiviral properties. On other hand, SP potential to synthesize biomaterials like as nanoparticules has not yet been explored. In addition, to date, SP have only been found in six plants and all inhabit saline environments. However, the SP pharmacological plant activities have not been carrying out. Furthermore, there are no reports of SP in freshwater plants. Thus, do SP from marine plants show pharmacological activity? Do freshwater plants actually synthesize SP? Is it possible to synthesize nanoparticles using SP from seaweed? In order to understand this question, this Thesis was divided into tree chapters. In the first chapter a sulfated polysaccharide (SPSG) was successfully isolated from marine plant Halodule wrightii. The data presented here showed that the SPSG is a 11 kDa sulfated heterogalactan contains glucose and xylose. Several assays suggested that the SPSG possessed remarkable antioxidant properties in different in vitro assays and an outstanding anticoagulant activity 2.5-fold higher than that of heparin Clexane® in the aPTT test; in the next chapter using different tools such as chemical and histological analyses, energy-dispersive X-ray analysis (EDXA), gel electrophoresis and infra-red spectroscopy we confirm the presence of sulfated polysaccharides in freshwater plants for the first time. Moreover, we also demonstrate that SP extracted from E. crassipes root has potential as an anticoagulant compound; and in last chapter a fucan, a sulfated polysaccharide, extracted from the brown seaweed was chemically modified by grafting hexadecylamine to the polymer hydrophilic backbone. The resulting modified material (SNFuc) formed nanosized particles. The degree of substitution for hydrophobic chains of 1H NMR was approximately 93%. SNFfuc-TBa125 in aqueous media had a mean diameter of 123 nm and zeta potential of -38.3 ± 0.74 mV, measured bydynamic light scattering. Tumor-cell (HepG2, 786, H-S5) proliferation was inhibited by 2.0 43.7% at SNFuc concentrations of 0.05 0.5 mg/ mL and RAEC non-tumor cell line proliferation displayed inhibition of 8.0 22.0%. On the other hand, nanogel improved CHO and RAW non-tumor cell line proliferation in the same concentration range. Flow cytometric analysis revealed that this fucan nanogel inhibited 786 cell proliferation through caspase and caspaseindependent mechanisms. In addition, SNFuc blocks 786 cell passages in the S and G2-M phases of the cell cycle

Caracterização de superfícies de titânio modificado por oxidação à plasma

Recent years have seen a significant growth in surface modifications in titanium implants, resulting in shorter healing times in regions with low bone density. Among the different techniques, subtraction by chemical agents to increase oxidation has been applied for surface treatment of dental implants. However, this technique is generally unable to remove undesirable oxides, formed spontaneously during machining of titanium parts, raising costs due to additional decontamination stages. In order to solve this problem, the present study used plasma as an energy source to both remove these oxides and oxidize the titanium surface. In this respect, Ti disks were treated by hollow cathode discharge, using a variable DC power supply and vacuum system. Samples were previously submitted to a cleaning process using an atmosphere of Ar, H2 and a mixture of both, for 20 and 60 min. The most efficient cleaning condition was used for oxidation in a mixture of argon (60%) and oxygen (40%) until reaching a pressure of 2.2 mbar for 60 min at 500°C. Surfaces were characterized by scanning electron microscopy (SEM), X-ray diffraction (XRD), atomic force microscopy (AFM), adhesion and cell proliferation. SEM showed less cell spreading and a larger number of projections orfilopodia in the treated samples compared to the control sample. AFM revealed surface defects in the treated samples, with varied geometry between peaks and valleys. Biological assays showed no significant difference in cell adhesion between treated surfaces and the control. With respect to cell proliferation, the treated surface exhibited improved performance when compared to the control sample. We concluded that the process was efficient in removing primary oxides as well as in oxidizing titanium surfaces

Micropartículas de poli (ácido lático-co-ácido glicólico) obtidas por spray drying para a liberação prolongada de metotrexato

Methotrexate (MTX) is a drug used in the chemotherapy of some kind of cancers, autoimmune diseases and non inflammatory resistant to corticosteroids uveits. However, the rapid plasmatic elimination limits its therapeutic success, which leads to administration of high doses to maintain the therapeutic levels in the target tissues, occurring potential side effects. The aim of this study was to obtain spray dried biodegradable poly-lactic acid co-glycolic acid (PLGA) microparticles containing MTX. Thus, suitable amounts of MTX and PLGA were dissolved in appropriate solvent system to obtain solutions at different ratios drug/polymer (10, 20, 30 and 50% m/m). The physicochemical characterizing included the quantitative analysis of the drug using a validate UV-VIS spectrophotometry method, scanning electron microscopy (SEM), infrared spectrophotometry (IR), thermal analyses and X-ray diffraction analysis. The in vitro release studies were carried out in a thermostatized phosphate buffer pH 7.4 (0.05 M KH2PO4) medium at 37°C ± 0.2 °C. The in vitro release date was subjected to different kinetics release models. The MTX-loaded PLGA microparticles showed a spherical shape with smooth surface and high level of entrapped drug. The encapsulation efficiency was greater then 80%. IR spectroscopy showed that there was no chemical bond between the compounds, suggesting just the possible occurrence of hydrogen bound interactions. The thermal analyses and X-ray diffraction analysis shown that MTX is homogeneously dispersed inside polymeric matrix, with a prevalent amorphous state or in a stable molecular dispersion. The in vitro release studies confirmed the sustained release for distinct MTX-loaded PLGA microparticles. The involved drug release mechanism was non Fickian diffusion, which was confirmed by Kornmeyer-Peppas kinetic model. The experimental results demonstrated that the MTX-loaded PLGA microparticles were successfully obtained by spray drying and its potential as prolonged drug release system.

Preparação e carcterização de complexos multicomponentes contendo ciclodextrinas e benznidazol

The benznidazole (BNZ) is the only alternative for Chagas disease treatment in Brazil. This drug has low solubility, which restricts its dissolution rate. Thus, the present work aimed to study the BNZ interactions in binary systems with beta cyclodextrin (β-CD) and hydroxypropyl-beta cyclodextrin (HP-β-CD), in order to increase the apparent aqueous solubility of drug. The influence of seven hydrophilic polymers, triethanolamine (TEA) and 1-methyl-2- pyrrolidone (NMP) in benznidazole apparent aqueous solubility, as well as the formation of inclusion complexes was also investigated. The interactions in solution were predicted and investigated using phase solubility diagram methodology, nuclear magnetic resonance of protons (RMN) and molecular modeling. Complexes were obtained in solid phase by spray drying and physicochemical characterization included the UV-Vis spectrophotometric spectroscopy in the infrared region, scanning electron microscopy, X-ray diffraction and dissolution drug test from the different systems. The increment on apparent aqueous solubility of drug was achieved with a linear type (AL) in presence of both cyclodextrins at different pH values. The hydrophilic polymers and 1-methyl-2-pyrrolidone contributes to the formation of inclusion complexes, while the triethanolamine decreased the complex stability constant (Kc). The log-linear model applied for solubility diagrams revealed that both triethanolamine and 1-methyl-2-pyrrolidone showed an action cosolvent (both solvents) and complexing (1-methyl-2-pyrrolidone). The best results were obtained with complexes involving 1-methyl-2-pyrrolidone and hydroxypropylbeta- cyclodextrin, with an increased of benznidazole solubility in 27.9 and 9.4 times, respectively. The complexes effectiveness was proven by dissolution tests, in which the ternary complexes and physical mixtures involving 1-methyl- 2-pyrrolidone and both cyclodextrins investigated showed better results, showing the potential use as novel pharmaceutical ingredient, that leads to increased benznidazole bioavailability

Avaliação da argila atapulgita para potencial uso como excipiente farmacêutico em formas sólidas

Clays are natural materials that have great potential for use as excipients for solid dosage forms. Palygorskite is a type of clay that has hydrophilic properties as well as a large surface area, which could contribute to the dissolution of drugs. Thus, the present study aims to evaluate the use of palygorskite clay, from Piaui (Northeast region of Brazil), as a pharmaceutical excipient for solid dosage forms, using rifampicin and isoniazid as the model drugs. The former is a poorly soluble drug often associated with isoniazid for tuberculosis treatment. Palygorskite was characterized by X-ray diffraction (XRD), X-ray fluorescence (XRF), particle size, transmission electron microscopy (TEM), scanning electron microscopy (SEM) and specific surface area (BET). The rheological and technological properties of palygorskite were determined and compared to those of talc, magnesium stearate and Aersosil 200. Mixtures between drugs and palygorskite were analyzed by differential scanning calorimetry (DSC), thermogravimetric analysis (TG) combined with thermal analysis (DTA) and Fourier Transform Infrared Spectroscopy (FT-IR), where the results were compared with those of the individual compounds. In addition, dissolution studies of solid dispersions and capsules containing the drugs, mixed with either palygorskite or a mixture of talc and magnesium stearate, were performed. The results showed that palygorskite has small particles with a high surface area. Its rheological characteristics were better than those of others commonly used glidants and lubricants. There was no interaction between palygorskite and the drugs (rifampicin and isoniazid). Among the dispersions studied, the mixture with palygorskite (5%) showed the highest drug dissolution when compared to other excipients. The dissolution of the rifampicin capsules containing palygosrkite was faster in higher concentrations. However, these differences were statistically different only in the first minutes of the dissolution experiment. The dissolution profile of isoniazid was also statistically different on the initial part of the experiment. The formulations prepared with isoniazid and palygorskite showed higher drug dissolution, but it was in descending order of concentration. According to these results, the palygorskite clay used in this study has great potential for application as an excipient for solid dosage forms

Obtenção e caracterização de complexos de inclusão binários e ternários com praziquantel

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior

Preparação e caracterização de complexos multicomponentes contendo ciclodextrinas com metotrexato

Conselho Nacional de Desenvolvimento Científico e Tecnológico

Micropartículas de poli (ácido láctico)/ poloxámero obtids por spray drying para liberação modificada de metotrexatro

New drug delivery systems have been used to increase chemotherapy efficacy due the possible drug resistance of cancer cells. Poly (lactic acid) (PLA) microparticles are able to reduce toxicity and prolong methotrexate (MTX) release. In addition, the use of PLA/poloxamer polymer blends can improve drug release due to changes in the interaction of particles with biological surfaces. The aim of this study was developing spray dried biodegradable MTX-loaded microparticles and evaluate PLA interactions with different kinds of Pluronic® (PLUF127 and PLUF68) in order to modulate drug release. The variables included different drug:polymer (1:10, 1:4.5, 1:3) and polymer:copolymer ratios (25:75, 50:50, 75:25). The precision and accuracy of spray drying method was confirmed assessing drug loading into particles (75.0- 101.3%). The MTX/PLA microparticles showed spherical shape with an apparently smooth surface, which was dependent on the PLU ratio used into blends particles. XRD and thermal analysis demonstrated that the drug was homogeneously dispersed into polymer matrix, whereas the miscibility among components was dependent on the used polymer:copolymer ratio. No new drug- polymer bond was identified by FTIR analysis. The in vitro performance of MTX-loaded PLA microparticles demonstrated an extended-release profile fitted using Korsmeyer- Peppas kinetic model. The PLU accelerated drug release rate possible due PLU leached in the matrix. Nevertheless, drug release studies carried out in cell culture demonstrated the ability of PLU modulating drug release from blend microparticles. This effect was confirmed by cytotoxicity observed according to the amount of drug released as a function of time. Thus, studied PLU was able to improve the performance of spray dried MTX-loaded PLA microparticles, which can be successfully used as carries for modulated drug delivery with potential in vivo application

Estudo do perfil térmico de fornos do tipo "caipira" utilizados pelo setor de cerâmica vermelha em parelhas na região Seridó-RN

The present study aimed to characterize the thermal profile of wood fired oven used by the red ceramic industry in Parelhas, in the Seridó region/RN, aiming to propose structural interventions that can contribute to increasing productivity and product quality, optimize wood consumption and mitigate existing losses during the burning process. The study was conducted at Cerâmica Esperança in the city of Parelhas -RN, Brazil, during the period from August 2012 to September 2013. Four treatments were performed with three replicates, ie, with, a total of 12 experimental units (burnings). In the first stage 4 treatments were performed with three replicates, totaling 12 experimental units (firings). In the second stage 2 treatments were performed with three replications, totaling 6 experimental units (firings). The physical characteristics of the wood were analyzed using standard NBR 11941 and NBR 7190 for basic density and moisture, respectively. The clay was used as a reference parameter for distinguishing treatments. For both the analysis and characterization was carried out using techniques of fluorescence X (XRF) rays, X-ray diffraction (XRD) analysis, particle size analysis (FA). In the first and second stages were monitored: the time during the firing process, the amount of wood used at each firing, the number of parts enfornadas for subsequent determination of the percentages of losses, but also product quality. To characterize the thermal profile of the oven, we measured the temperature at 15 points scored in the surface charge put into the oven. Measurements were taken every 30 minutes from preheat until the end of burning, using a pyrometer laser sight sighting from preheating until the end of burning. In the second step 12 metal cylinders distributed on the oven walls, and the cylinder end walls 8 of the furnace 2 and rollers on each side walls are installed equidistant to 17 cm from the soil and the surface 30 of the wall are installed. The cylinders distributed on the front were placed 50 cm above the furnace, and the base of the oven 20 cm distant from the ground. 10 also thermocouples were installed, and five thermocouples distributed 1.77 cm above the combustion chambers, and one thermocouple on each side, and three thermocouples in front of the oven. We carried out the measurements of the temperatures every 1 hour during the burning two hours in cooling the cylinders with a pyrometer and thermocouples for dattaloger. These were fixed with depth of 30 cm from the wall. After statistical analysis it was found that: the thermal profile of the furnace surface and at different heights was heterogeneous; and the ranges of density and moisture content of wood are within recommended for use as an energy source standards. We conclude that even at low temperatures reached during firing there was a significant production of good quality products, this is due to high concentrations of iron oxide and potassium oxide found in clay, which lowers the melting point of the piece. The average burn time for each step varied 650-2100 minutes wood consumption was on average 20 m3, product quality was on average 16% of first quality, 70% second, third and 5% to 10% loss . The distance between the wire and the surface of the oven was a significant parameter for all treatments, but with different variations, meaning that the wire should not be so generic and unique form, used as a criterion for completion of the burn process. The central part of the furnace was the area that reached higher temperature, and in a unified manner, with the highest concentration of top quality products. The ideal temperature curve, which provided the highest quality of ceramic products was achieved in the central part of the furnace

Variabilidade espacial de atributos mineralógicos de um latossolo sob diferentes formas do relevo: I - mineralogia da fração argila

A distribuição dos minerais da fração argila depende de condições pedoambientais específicas. O estudo das relações entre atributos desses minerais e locais específicos de sua ocorrência na paisagem torna-se importante para o entendimento das relações entre a mineralogia e os demais atributos do solo. Este trabalho teve como objetivo avaliar os atributos cristalográficos, as razões Gt/(Gt+Hm) e Ct/(Ct+Gb) dos minerais da fração argila (hematita, goethita, caulinita e gibbsita) e o padrão de distribuição espacial destes em um Latossolo Vermelho eutroférrico sob cultivo de cana-de-açúcar há mais de 30 anos, com colheita no sistema cana crua. As amostras de solo foram coletadas nos pontos de cruzamento de uma malha, georreferenciados, com intervalos regulares de 10 m, e dimensão de 100 x 100 m, na profundidade de 0,2-0,4 m, totalizando 119 pontos, em uma área de 1 ha. As amostras de solos foram analisadas quimicamente. Posteriormente, a fração argila foi submetida à difração de raios X. Foram feitas as análises estatísticas e geoestatísticas dos atributos cristalográficos dos minerais analisados. Mapas de krigagem foram realizados para a visualização da variabilidade espacial dos atributos. Todos os atributos estudados apresentaram dependência espacial, e os atributos mineralógicos apresentaram-se relacionados com variações das formas do relevo. A gibbsita apresentou o maior diâmetro médio do cristal (DMC) entre os minerais da fração argila estudados, e a goethita foi o mineral que apresentou a maior variação do DMC e da largura à meia altura. Os maiores valores do DMC da goethita, hematita e gibbsita foram encontrados no compartimento II, caracterizado por uma área côncavo-convexa.

Mineralogy of the clay fraction of Alfisols in two slope curvatures: III - spatial variability

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Variabilidade espacial de atributos mineralógicos de um latossolo sob diferentes formas do relevo: II - correlação espacial entre mineralogia e agregados

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Relações solo-paisagem em uma litosseqüência arenito-basalto na região de Pereira Barreto, SP

Os objetivos deste trabalho foram estudar as relações solo-paisagem em uma litosseqüência de transição arenito-basalto e verificar a similaridade dos limites de superfícies geomórficas mapeados no campo com os limites mapeados a partir de técnicas geoestatísticas. Foi realizado o mapeamento de uma área de 530 ha, utilizando-se equipamento de GPS, e em seguida elaborou-se o Modelo de Elevação Digital, que possibilitou o estabelecimento da transeção de 2.100 m a partir do topo. Ao longo da transeção, o terreno foi estaqueado a intervalos regulares de 50 m, nos quais foram realizadas medidas da altitude para confecção do perfil altimétrico. As superfícies geomórficas foram identificadas e delimitadas conforme critérios topográficos e estratigráficos, com base em intensas investigações de campo. Coletaram-se amostras de solo em pontos laterais em 67 locais, nas superfícies geomórficas identificadas, nas profundidades de 0,0-0,25 m e 0,80-1,00 m. Além disso, foram abertas trincheiras nos segmentos de vertente inseridos nas superfícies geomórficas mapeadas. As amostras coletadas foram analisadas quanto a densidade do solo, textura, Ca2+, K+, Mg2+, SB, CTC, V, pH (água e KCl), SiO2, Al2O3 e Fe2O3 (ataque por H2SO4), óxidos de Fe livres extraído com ditionito-citrato-bicarbonato e ferro mal cristalizado extraídos com oxalato de amônio. A fração argila desferrificada foi analisada por difração de raios X. A compartimentação da paisagem em superfícies geomórficas e a identificação do material de origem mostraram-se bastante eficientes para entendimento da variação dos atributos do solo. A análise individual desses atributos por meio de estatística univariada auxiliou na discriminação das três superfícies geomórficas. O uso de técnicas de geoestatística permitiu a confirmação de que mesmo os atributos do solo apresentaram limites próximos aos das superfícies geomórficas.