999 resultados para MEV-catodoluminescência


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Although there are a wide variety of additives that act in fresh state, to adjust the properties of cement, there is also a search by additions that improve the tenacity of the cement in the hardened state. This, in turn, can often be increased by inserting fibers, which act on the deflection of microcracks. This study aimed to use a microfiber glass wool (silica-based) as an additive reinforcing the cement matrix, improving the rupture tenacity, in order to prevent the propagation of microcracks in the cement sheath commonly found in oil wells submitted to high temperatures. The fibers were added at different concentrations, 2 to 5% (BWOC) and varied average sizes, grinding for 90 s, 180 s, 300 s, 600 s. The cement slurries were made with a density of 1,90 g/ cm3 (15,6 lb/gal), using Portland cement CPP- Special Class as the hydraulic binder and 40% silica flour. The characterization of the fiber was made by scanning electron microscopy (SEM), particle size by sieving, X-ray fluorescence (XRF), X-ray diffraction (XRD) and thermogravimetry (TG / DTG). Were performed technological tests set by the API (American Petroleum Institute) by rheology, stability, free water, compressive strength, as well as testing rupture energy, elastic modulus and permeability. The characterization results showed good thermal stability of the microfiber glass wool for application in oil wells submitted to steam injection and, also, that from the particle size data, it was possible to suggest that microfibers milled up to 300 s, are ideal to act as reinforcement to the cement slurries. The rheological parameters, there was committal of plastic viscosity when larger lengths were inserted of microfiber (F90). The values obtained by free water and stability were presented according to API. The mechanical properties, the incorporation of microfiber to the cement slurries gave better rupture tenacity, as compared to reference cement slurries. The values of compressive strength, elastic modulus and permeability have been maintained with respect to the reference cement slurries. Thus, cement slurries reinforced with microfiber glass wool can ensure good application for cementing oil wells submitted to steam injection, which requires control of microcracks, due to the thermal gradients

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In this study, it has been investigated the influence of silver film deposition onto 100% polyester woven and non-woven, on the survival of Escherichia coli and Staphylococcus aureus in contact with these surfaces. The treatment was performedin a chamber containing the working gas at low pressure (~ 10-2 mbar). Some process parameters such as as voltage: 470 V; pressure: 10-2 mbar; current : 0.40 A and gas flow: 6 and 10 cm3/min were kept constant. For the treatments with purêargon plasma using a flow of 6 and 10 cm3/min, different treatment times were evaluated, such as, 10 , 20, 30, 40, 50 and 60 minutes. Contact angle (sessile drop), measurements were used to determine the surface tension of the treated fabrics and its influence on the bacteria grow as weel as the possibilities of a biofilm formation. The formation of a silver film, as well as the amount of this element was verified byEDX technique. The topography was observed through scanning electron microscopy (SEM) to determine the size of silver grains formed on the surfaces of the fabric and assess homogeneity of treatment. The X-ray diffraction (XRD) was used to analyze the structure of silver film deposition. The woven fabric treatments enabled the formation of silver particulate films with particle size larger than the non-woven fabrics. With respect to bacterial growth, all fabrics were shown to be bactericidal for Staphylococcus aureus (S. aureus), while for the Escherichia coli (E. coli), the best results were found for the non-woven fabric (TNT) treated with a flow of 10 cm3/min to both bacteria

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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

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

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The aim of the present study was to assess the effectiveness and adverse effects on dental enamel caused by nightguard vital bleaching with 10% carbamide peroxide. This was accomplished through the interaction of researchers from different areas such as dentistry, materials engineering and physics. Fifty volunteers took part in the doubleblind randomized controlled clinical trial. They were allocated to an experimental group that used Opalescence PF 10% (OPA) and a control group that used a placebo gel (PLA). Fragments of human dental enamel from the vestibular surface of healthy premolars, extracted for orthodontic reasons, were fixed to the vestibular surface of the first upper molars of the volunteers for in situ observation. Bleaching was performed at night for 21 days. The observation periods included Baseline (BL), T0 (21 days), T30 (30 days after treatment) and T180 (180 days after treatment, only for the OPA group). Tooth color was assessed by comparing it with the Vita® scale and by the degree of satisfaction expressed by the volunteer. We also assessed adverse clinical effects, dental sensitivity and gingival bleeding. The study of adverse effects on enamel was conducted in vivo and in situ, using the DIAGNOdent® laser fluorescence device to detect mineral loss. Scanning electron microscopy (SEM) was used to check for superficial morphological alterations, energy dispersive spectrophotometry (EDS) to semiquantitatively assess chemical composition using the Ca/P ratio, and the x-ray diffraction (XRD) technique to observe alterations in enamel microstructure. The results showed that nightguard vital bleaching with 10% carbamide peroxide was effective in 96% of the cases, versus 8% for the PLA group. Dental sensitivity was present in 36% (9/25) of the cases. There was no significant association between gingival bleeding and the type of gel used (p = 1.00). In vivo laser fluorescence analysis showed no difference in values for the control group, whereas in the OPA group there was a statistically significant difference between baseline values in relation to the subsequent periods (p<0.01), with lower mean values for post-bleaching times. There was a significant difference between the groups for times T0 and T30. Micrographic analysis showed no enamel surface alterations related to the treatment performed. No significant alteration in Ca/P ratio was observed in the OPA group (p = 0.624) or in the PLA group (p = 0.462) for each of the observation periods, nor between the groups studied (p=0.102). The XRD pattern for both groups showed the presence of three-phase Hydroxyapatite according to JCPDS files (9-0432[Ca5(PO4)3(OH)], 18-0303[Ca3(PO4)2.xH2O] and 25-0166[Ca5(PO4)3(OH, Cl, F)]). No other peak associated to other phases was found, independent of the group analyzed, which reveals there was no disappearance, nucleation or phase transformation. Neither was there any alteration in peak pattern location. With the methodology and protocol used in this study, nightguard vital bleaching with 10% carbamide peroxide proved to be an effective and safe procedure for dental enamel

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Bacterial cellulose (BC) has a wide range of potential applications, namely as temporary substitute skin in the treatment of skin wounds, such as burns, ulcers and grafts. Surface properties determine the functional response of cells, an important factor for the successful development of biomaterials. This work evaluates the influence of bacterial cellulose surface treatment by plasma (BCP) on the cellular behavior and its genotoxicity potential. The modified surface was produced by plasma discharge in N2 and O2 atmosphere, and the roughness produced by ion bombardment characterized by scanning electron microscopy (SEM) and atomic force microscopy (AFM). Cell adhesion, viability and proliferation on BCP were analysed using crystal violet staining and the 3-[4,5-dimethylthiazol-2-yl]-2,5-diphenyl-tetrazolium (MTT) method. Genotoxicity was evaluated using the comet and cytokinesis block micronucleus assay. The results show that the plasma treatment changed surface roughness, producing an ideal cell attachment, evidenced by more elongated cell morphology and improved proliferation. The excellent biocompatibility of BCP was confirmed by genotoxicity tests, which showed no significant DNA damage. The BCP has therefore great potential as a new artificial implant

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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

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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.

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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

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior

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Conselho Nacional de Desenvolvimento Científico e Tecnológico

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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

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

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O fungo nematófago Monacrosporium robustum foi detectado, isolado e identificado pela primeira vez de solos do Brasil, em maio de 1999, no Laboratório de Nematologia do Departamento de Fitossanidade da Universidade Estadual Paulista (UNESP), Campus de Jaboticabal, São Paulo, tendo sido o potencial como agente de biocontrole do nematóide de cisto da soja, Heterodera glycines raça 3 observado ao microscópio eletrônico de varredura (MEV) (Maia & Santos, 1999). Na presente pesquisa, detalhes das estruturas de captura, tamanho, forma e septação dos conídios, bem como nematóides capturados pelo fungo foram documentados. Monacrosporium robustum produz micélio hialino, e as estruturas de captura são constituídas por ramificações adesivas, na forma de protuberâncias verticais que surgem das hifas, medindo, em média, 10 µm de comprimento e 5 µm de diâmetro. Uma substância gelatinosa desprende- se dessas estruturas, ao contato com o nematóide, aprisionando-o. Os conídios do fungo são hialinos, fusóides com dois ou quatro septos, às vezes, cinco. Conídios jovens são asseptados e piriformes. Sob condições de laboratório, esse fungo predou 100% dos ovos e dos juvenis de segundo estádio de H. glycines e formas ativas de Panagrellus sp., no período de 72 h da exposição desses nematóides ao fungo.

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Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)