241 resultados para Análise Térmica. TG-DSC. Hormônios Bioidênticos. Estradiol e Estriol
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Foi desenvolvido um método para detectar e quantificar misturas de corantes em sucos artificiais em pó fabricados no Brasil, de diferentes marcas e sabores. Foram estudados 6 corantes artificiais: amarelo tartrazina, amarelo crepúsculo, vermelho ponceau 4R, vermelho bordeaux S, vermelho 40 e azul brilhante presentes de forma unitária ou em misturas nos sucos com sabores laranja, tangerina, maracujá, abacaxi, limão e uva. A identificação dos corantes nas amostras foi feita através da comparação com os espectros dos padrões, utilizando-se a análise por infravermelho médio e pelos respectivos valores de absorção máxima nos comprimentos de onda relativos aos padrões e valores de referência na literatura. Também foram estudados os perfis de decomposição térmica por termogravimetria, termogravimetria derivada e calorimetria diferencial exploratória dos corantes e dos sucos em pó, sendo determinados os teores de umidade, de matéria orgânica e de cinzas. O teor de umidade encontrado não ultrapassou 4% para todas as amostras de suco analisadas. Com relação ao teor de matéria orgânica obteve-se para 57% dos sucos analisados um teor médio de 51,3% e para 43% das outras amostras obteve-se uma média de 67,2 %. Os resultados obtidos para o teor de cinzas indicaram que 29% das amostras apresentaram um teor de 26,7% para esse parâmetro enquanto 71% das amostras apresentaram um teor de cinzas de 46,4%. Os resultados obtidos por análise térmica mostraram-se adequados considerando-se que para obter os resultados pelo método tradicional há um investimento maior de tempo, de pessoal envolvido e de material, além da proteção ao meio ambiente. Para a análise por espectroscopia de absorção molecular foi proposta uma equação simplificada para a determinação de cada corante na mistura utilizando-se a lei de Beer. Para validação, empregou-se a espectroscopia de absorção molecular no visível, onde foi investigada a influência dos interferentes (TiO2 e açúcar) presentes nas amostras de sucos, os testes de fotodegradação e a avaliação do efeito do pH. Para quantificação tomou-se como referência 512 amostras sintéticas contendo um e dois corantes (1,5625 a 25,000 mg L-1) para obtenção das curvas analíticas que foram aplicadas à análise dos sucos em pó. Os resultados indicaram que o teor máximo do amarelo crepúsculo foi encontrado nos sucos com os sabores laranja, tangerina e manga que correspondeu a 25,6% da ingestão diária aceitável (para ser ultrapassada corresponderia a ingestão de 4 copos). O teor máximo encontrado para o amarelo tartrazina nos sucos foi para o sabor maracujá que correspondeu a 8,5% da ingestão diária aceitável, (para ser alcançado corresponderia a ingestão de 12 copos). O método proposto foi testado e validado com sucesso para amostras de sucos em pó sendo de simples execução e de rapidez na obtenção dos resultados
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Bifunctional catalysts based on zircon oxide modified by tungsten (W = 10, 15 and 20 %) and by molybdenum oxide (Mo= 10, 15 e 20 %) containg platinum (Pt = 1%) were prepared by the polymeric precursor method. For comparison, catalysts the tungsten base was also prepared by the impregnation method. After calcinations at 600, 700 and 800 ºC, the catalysts were characterized by X-ray diffraction, fourier-transform infrared spectroscopy, thermogravimetric and differential thermal analysis, nitrogen adsorption and scanning electron microscopy. The profile of metals reduction was determined by temperature programmed reduction. The synthesized catalysts were tested in n-heptane isomerization. X-ray diffractogram of the Pt/WOx-ZrO2 and Pt/MoOx-ZrO2 catalysts revealed the presence of tetragonal ZrO2 and platinum metallic phases in all calcined samples. Diffraction peaks due WO3 and ZrO2 monoclinic also were observed in some samples of the Pt/WOx-ZrO2 catalysts. In the Pt/MoOx-ZrO2 catalysts also were observed diffraction peaks due ZrO2 monoclinic and Zr(MoO4)2 oxide. These phases contained on Pt/WOx-ZrO2 and Pt/MoOx-ZrO2 catalysts varied in accordance with the W or Mo loading and in accordance with the calcination temperature. The infrared spectra showed absorption bands due O-W-O and W=O bonds in the Pt/WOx-ZrO2 catalysts and due O-Mo-O, Mo=O and Mo-O bonds in the Pt/MoOx-ZrO2 catalysts. Specific surface area for Pt/WOx-ZrO2 catalysts varied from 30-160 m2 g-1 and for the Pt/MoOx-ZrO2 catalysts varied from 10-120 m2 g-1. The metals loading (W or Mo) and the calcination temperature influence directly in the specific surface area of the samples. The reduction profile of Pt/WOx-ZrO2 catalysts showed two peaks at lower temperatures, which are attributed to platinum reduction. The reduction of WOx species was evidenced by two reduction peak at high temperatures. In the case of Pt/MoOx-ZrO2 catalysts, the reduction profile showed three reduction events, which are attributed to reduction of MoOx species deposited on the support and in some samples one of the peak is related to the reduction of Zr(MoO4)2 oxide. Pt/WOx-ZrO2 catalysts were active in the n-heptane isomerization with high selectivity to 3-methyl-hexane, 2,3- dimethyl-pentane, 2-methyl-hexane among other branched hydrocarbons. The Pt/MoOx-ZrO2 catalysts practically didn't present activity for the n-heptane isomerization, generating mainly products originating from the catalytic cracking
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The improved performance of hydraulic binders, the base of Portland cement, consists in the careful selection and application of materials that promote greater durability and reduced maintenance costs There is a wide variety of chemical additives used in Portland cement slurries for cementing oil wells. These are designed to work in temperatures below 0 ° C (frozen areas of land) to 300 ° C (thermal recovery wells and geothermal); pressure ranges near ambient pressure (in shallow wells) to greater than 200 MPa (in deep wells). Thus, additives make possible the adaptation of the cement slurries for application under various conditions. Among the materials used in Portland cement slurry, for oil wells, the materials with nanometer scale have been applied with good results. The nanossílica, formed by a dispersion of SiO2 particles, in the nanometer scale, when used in cement systems improves the plastic characteristics and mechanical properties of the hardened material. This dispersion is used commercially as filler material, modifier of rheological properties and / or in recovery processes construction. It is also used in many product formulations such as paints, plastics, synthetic rubbers, adhesives, sealants and insulating materials Based on the above, this study aims to evaluate the performance of nanossílica as extender additive and improver of the performance of cement slurries subjected to low temperatures (5 ° C ± 3 ° C) for application to early stages of marine oil wells. Cement slurries were formulated, with densities 11.0;12.0 and 13.0 ppg, and concentrations of 0; 0.5, 1.0 and 1.5%. The cement slurries were subjected to cold temperatures (5 ° C ± 3 ° C), and its evaluation performed by tests rheological stability, free water and compressive strength in accordance with the procedures set by API SPEC 10A. Thermal characterization tests (TG / DTA) and crystallographic (XRD) were also performed. The use of nanossílica promoted reduction of 30% of the volume of free water and increased compression resistance value of 54.2% with respect to the default cement slurry. Therefore, nanossílica presented as a promising material for use in cement slurries used in the early stages of low-temperature oil wells
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The Cu-Al2O3 composite ceramic combines the phase of alumina, which is extremely hard and durable, yet very brittle, to metallic copper phase high ductility and high fracture toughness. These characteristics make this material a strong candidate for use as a cutting tool. Al2O3-Cu composite powders nanocrystalline and high homogeneity can be produced by high energy milling, as well as dense and better mechanical structures can be obtained by liquid phase sintering. This work investigates the effect of high-energy milling the dispersion phase Al2O3, Cu, and the influence of the content of Cu in the formation of Cu-Al2O3 composite particles. A planetary mill Pulverisatte 7 high energy was used to perform the experiments grinding. Al2O3 powder and Cu in the proportion of 5, 10 and 15% by weight of Cu were placed in a container for grinding with balls of hard metal and ethyl alcohol. A mass ratio of balls to powder of 1:5 was used. All powders were milled to 100 hours, and powder samples were collected after 2, 10, 20, 50 and 70 hours of grinding. Composite powders with compact cylindrical shape of 8 mm diameter were pressed and sintered in uniaxial matrix resistive furnace to 1200, 1300 to 1350 °C for 60 minutes under an atmosphere of argon and hydrogen. The heating rate used was 10°C/min. The powders and structures of the sintered bodies were characterized by XRD, SEM and EDS. Analysis TG, DSC and particle size were also used to characterize the milled powders, as well as dilatometry was used to observe the contraction of the sintered bodies. The density of the green and sintered bodies was measured using the geometric method (mass / volume). Vickers microhardness with a load of 500 g for 10 s were performed on sintered structures. The Cu-Al2O3 composite with 5% copper density reached 61% of theoretical density and a hardness of 129 HV when sintered at 1300 ° C for 1h. In contrast, lower densities (59 and 51% of the theoretical density) and hardness (110 HV and 105) were achieved when the copper content increases to 10 and 15%.
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In this study we evaluated the capacity removal of PAHs in an oily solution between the bentonite hydrofobized with linseed oil and paraffin with natural bentonite. Analyses of natural bentonite and hydrofobized were made by the characterization techniques: (1) Thermogravimetric Analysis (TGA), which aimed to evaluate the thermal events due to mass loss, both associated with the exit of moisture and decomposition of clay as due to hidrofobizante loss agent. (2) Analysis of X-ray diffraction (XRD) in order to determine the mineralogical phases that make up the structure of clay and (3) Spectrophotometry in the infrared region used to characterize the functional groups of both the matrix mineral (bentonite) and the hidrofobizantes agents (linseed oil and paraffin). We used a factorial design 24 with the following factors; hidrofobizante, percent hidrofobizante, adsorption time and volume of the oily solution. Analyzing the factorial design 24 was seen that none of the factors apparently was more important than the others and, as all responses showed significant values in relation to the ability of oil removal was not possible to evaluate a difference in the degree of efficiency the two hidrofobizantes. For the new study compared the efficiency of the modified clay, with each hidrofobizante separately in relation to their natural form. As such, there are four new factorial designs 23 using natural bentonite as a differentiating factor. The factors used were bentonite (with and without hydrophobization), exposure time of the adsorbent material to the oily solution and volume of an oily solution, trying to interpret how these factors could influence the process of purifying water contaminated with PAHs. Was employed as a technique for obtaining responses to fluorescence spectroscopy, as already known from literature that PAHs, for presenting combined chains due to condensation of the aromatic rings fluoresce quite similar when excited in the ultraviolet region and as an auxiliary technique to gas chromatography / mass spectrometry (GC-MS) used for the analysis of PAHs in order to complement the study of fluorescence spectroscopy, since the spectroscopic method only allows you an idea of total number of fluorescent species contained in the oil soluble. The result shows an excellent adsorption of PAHs and other fluorescent species assigned to the main effect of the first factor, hydrophobization for the first planning 23 BNTL 5%, for 93% the sixth stop in the second test (+-+),factorial design 23 BNTL 10%, the fourth test (++-) with 94.5% the third factorial design 23 BNTP 5%, the second test (+--) with 91% and the fourth and final planning 23 BNTP 10%, the last test ( + + +) with 88%. Compared with adsorption of bentonite in its natural form. This work also shows the maximum adsorption of each hidrofobizante
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The advancement of nanotechnology in the synthesis and characterisation of nanoparticles (NP's) has played an important role in the development of new technologies for various applications of nano-scale materials that have unique properties. The scientific development in the last decades in the field of nanotechnology has sought ceaselessly, the discovery of new materials for the most diverse applications, such as biomedical areas, chemical, optical, mechanical and textiles. The high bactericidal efficiency of metallic nanoparticles (Au and Ag), among other metals is well known, due to its ability to act in the DNA of fungi, viruses and bacteria, interrupting the process of cellular respiration, making them important means of study, in addition to its ability to protect UVA and UVB. The present work has as its main objective the implementation of an innovative method in the impregnation of nanoparticles of gold in textile substrate, functionalized with chitosan, by a dyeing process by exhaustion, with the control of temperature, time and velocity, thus obtaining microbial characteristics and UV protection. The exhausted substrates with colloidal solutions of NPAu's presented the colours, lilac and red (soybean knits) due to their surface plasmon peak around 520-540 nm. The NPAu's were synthesized chemically, using sodium citrate as a reducing agent and stabilizer. The material was previously cationised with chitosan, a natural polyelectrolyte, with the purpose of functionalising it to enhance the adsorption of colloid, at concentrations of 5, 7, 10 and 20 % of the bonding agent on the weight of the material (OWM). It was also observed, through an experimental design 23 , with 3 central points, which was the best process of exhaustion of the substrates, using the following factors: Time (min.), temperature (OC) and concentration of the colloid (%), having as a response to variable K/S (ABSORBÂNCIA/ Kubelka-Munk) of the fibres. Furthermore, it was evidenced as the best response, the following parameters: concentration 100%, temperature 70 ºC and time 30 minutes. The substrate with NPAu was characterised by XRD; thermal analysis using TGA; microstructural study using SEM/EDS and STEM, thus showing the NP on the surface of the substrate confirming the presence of the metal. The substrates showed higher washing fastness, antibacterial properties and UV radiation protection.
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The hormone administration by the oral route is frequently related with different many side effects. The aim of this study was to evaluate the safety and efficacy of a new product intended to transdermal hormone replacement nanostructured (TRHN) therapy, based on a patented under No. US 2013/0123220A1 formulation. This formulation was able to restore serum levels of estradiol (0.1%) + estradiol (0.25%) in 122 postmenopausal women with a mean age of 56.88 (± 6.27). The assessment is part of a longitudinal prospective study. Clinical parameters, including the degree of satisfaction with symptom relief, serum concentrations of estradiol, weight, blood pressure, were compared between the beginning and the end of treatment. The findings show that BIOLIPÍDEO B2® was safe and effective in restoring hormonal serum levels without side effects. The satisfaction with treatment was 92%. Serum concentrations of estradiol was significantly higher after treatment (p <0.05). Weight and systolic and diastolic blood pressure showed no significant differences (p> 0.05) during treatment. No vaginal bleeding was observed. Evaluation of bilateral breast mammography treatment found normal results in all women. This study shows for the first time the effectiveness of a transdermal formulation nanostructured in the transdermal delivery of estradiol and estriol measured in vivo using Confocal Raman Spectroscopy. The formulation of BIOLIPÍDEO/B2® is safe and effective in restoring serum estradiol levels and alleviates menopausal symptoms. The formulation can serve as a good choice for hormone replacement therapy to protect against post-menopausal symptoms.
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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior - CAPES
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The PSFC (Pr0.5Sr0.5Fe1-xCuxO3-δ) is a new mixed oxide perovskite and has been studied and evaluated the cathode materials for intermediate temperature solid oxide fuel cells (IT-SOFCs), mainly due to its good compatibility with the electrolyte (CGO) and its high ionic conductivity and electronic in intermediate temperature. In this work, PSFC powders with two different compositions (Pr0,5Sr0,5Fe0,8Cu0,2O3- PSFC5582 and Pr0,5Sr0,5Fe0,6Cu0,4O3-PSFC5564) were synthesized by the citrate method using a new route. The powders obtained were characterized by thermal analysis (Differential Scanning Calorimetry and Thermogravimetry), and the material calcined at 800, 900 and 1000 °C for 5h were analyzed by X-ray diffractometry (XRD), with the Rietveld refinement of the diffraction data and dilatometry. PSFC5582 composite films were obtained by screen printing of powder calcined at 1000 °C. The films were deposited on substrate ceria doped with gadolinia (CGO) and then sintered at 1050 °C for 2h. The electrochemical performance of the electrodes was evaluated by impedance spectroscopy and the interface electrode/electrolyte was observed by scanning electron microscopy (SEM). The specific resistance area (ASR) was 0.44 Ω.cm² at 800 °C, slightly lower than those reported in the literature for cathodes containing cobalt. The thermal expansion coefficients of both the PSFC compositions were obtained and varied between 13 and 15 x 10-6 °C-1 , in a temperature range of 200 to 650 °C, demonstrating the good thermal compatibility of cathodes with Ce0,9Gd0,1O1,95 electrolytes (CET = 12 x 10-6 °C).
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Composite NiO-C0.9Gd0.1O1.95 (NiO-GDC), one of the materials most used for the manufacture of anodes of Cells Solid Oxide Fuel (SOFC) currently, were obtained by a chemical route which consists in mixing the precursor solution of NiO and CGO phases obtained previously by the Pechini method. The nanopowders as-obtained were characterized by thermal analysis techniques (thermogravimetry and Differential Scanning Calorimetry) and calcined materials were evaluated by X-ray diffraction (XRD). Samples sintered between 1400 and 1500 ° C for 4 h were characterized by Archimedes method. The effects of the composition on the microstructure and electrical properties (conductivity and activation energy) of the composites sintered at 1500 ° C were investigated by electron microscopy and impedance spectroscopy (between 300 and 650 ° C in air). The refinement of the XRD data indicated that the powders are ultrafine and the crystallite size of the CGO phase decreases with increasing content of NiO. Similarly, the crystallite of the NiO phase tends to decrease with increasing concentration of CGO, especially above 50 wt % CGO. Analysis by Archimedes shows a variation in relative density due to the NiO content. Densities above 95% were obtained in samples containing from 50 wt % NiO and sintered between 1450 and 1500 °C. The results of microscopy and impedance spectroscopy indicate that from 30-40 wt.% NiO there is an increase in the number of contacts NiO - NiO, activating the electronic conduction mechanism which governs the process of conducting at low temperatures (300 - 500 °C). On the other hand, with increasing the measuring temperature the mobility of oxygen vacancies becomes larger than that of the electronic holes of NiO, as a result, the high temperature conductivity (500-650 ° C) in composites containing up to 30-40 wt.% of NiO is lower than that of CGO. Variations in activation energy confirm change of conduction mechanism with the increase of the NiO content. The composite containing 50 wt. % of each phase shows conductivity of 19 mS/cm at 650 °C (slightly higher than 13 mS/cm found for CGO) and activation energy of 0.49 eV.
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Chitosan is a polymer biocompatibility and biodegradability widely used in drug delivery systems. The co-crosslinking of chitosan with sodium sulfate and genipin, to form particulate systems is related of making them more resistant to acidic pH and to modulate the release kinetics for the oral route. Triamcinolone is a glucocorticoid with anti-inflammatory and immunosuppressive actions. The nanoparticles were prepared by co-crosslinking and characterized for particle size, PDI, zeta potential, crosslinking degree, encapsulation rate, morphology, infrared spectroscopy, thermal analysis, release kinetics and cells studies. The nanoparticles were prepared initially without genipin with sodium sulphate and the particles parameters were monitored in function of different ratio of drug / polymer, different concentrations of sodium sulfate and polysorbate 80 and the drip mode of crosslinkers on polymers. After optimizing conditions, the chosen system parameters without genipin included mean diameter of 312.20 ± 5.70 nm, PDI 0.342 ± 0.013 and zeta potential of 20.18 ± 2.28 mV. The genipin was introduced into the system analyzing different concentrations (0.5, 1.0 and 2.0 mM) and crosslinking times (3, 6, 12 and 24 h). Evaluating crosslinking time with genipin (0.5 mM) it was showed that varying the genipin reaction time the systems size ranged from 235.1 to 334.4 nm, the PDI from 0.321 to 0.392 and zeta potential 20.92 to 30.39 mV. The crosslinking degree that coud vary from 14 to 30 %. Nanoparticles without genipina, 6 h and 24 h crosslinking time were dried by spray-drying method. Analysis by scanning electron micrograph (SEM) revealed that the microparticles showed spherical morphology. The encapsulation rate was 75 ± 2.3 % using validated HPLC methodology. The infrared analysis showed chemical interactions between the components of the formulation. Thermal analysis showed that systems with a higher degree of crosslinking had a higher thermal stability. On release kinetics, increasing the degree of crosslinking was able to decrease the concentration and rate of release of triamcinolone. In studies with liver cancer cells (HepG2) and colon (HT-29), the microparticulate prepared with triamcinolone and 24 h of crosslinking with genipin showed a potential for antitumor activity in hepatic cell line HepG2. Therefore, a new delivery system for triamcinolone on polymeric nanoparticles of chitosan cocrosslinked with genipin and sodium sulfate was obtained with hepatic antitumor potential.
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The reduction in energy consumption is the main requirement to be satisfied in refrigeration and air conditioning by mechanical vapor compression system. In automotive system isn´t different. Thermal analyses in these systems are crucial for a better performance in automotive air conditioner. This work aims to evaluate the conditions of use of R134A refrigerant (used in vehicles) and compare with R437A (alternative refrigerant), varying the speed of the electric fan in the evaporator. All tests were performed in automotive air conditioning unit ATR600, simulating the thermal conditions of the system. The equipment is instrumented for data acquisition temperature, condensation and evaporation pressures and electrical power consumed to determine the coefficient of performance of the cycle. The system was tested under rotations of 800, 1600 and 2400 rpm with constant load of R- 134a. It occurred with the same conditions with R437A. Both recommended by the manufacturer. The results show that the best system performance occurs in the rotation of 800 RPM for both refrigerants.
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Surface defects on steel parts borne costs of smelting industries due to the need of rework. Sand molds are frequently used in foundry industries and largely responsible for providing surface defects. This study aims to optimize the levels of the molding process variables to minimize the occurrence of surface defects in steel castings in silica sand molds chemically linked by cold cure process. The methodology used the experimental design with split plot, being considered in the study the resin percentage factors in the mold formulation, addition of iron oxide, type of paint, the paint application method, amount of ink layers, use of hot air along the lines and waiting time of the mold before casting. They were analyzed as response variables erosion defects, sand inclusion, penetration, porosity and surface finish. Tensile strength tests were performed to evaluate the influence of factors on mechanical parameters and the microstructural parameters were carried out the analysis of X-ray diffraction, scanning electron microscopy (SEM) and thermal analysis (TG / DSC / dilatometry). The results elucidate that for the faulty erosion, the only significant factor with a 95% confidence level was the type of ink and the ink alumina-based superior results obtained. For the sand inclusion of defect, there were three significant factors, with best results obtained with alumina-based paint and spray applied using hot air in the mold before casting the metal. For the defect penetration, there were four significant factors, the best results being achieved with 0.8% of resin and addition of iron oxide in the molding formulation, the paint being applied by brush and standby time of 24 hours before leak. For the defect porosity with a 95% confidence level, no significant factors. For the defect surface finish, the best results were achieved with the 0.8% formulation of the resin in the mold and application of the paint brush. To obtain the levels of the factors that optimize all defects simultaneously, we performed a weighted average of the results of each type of fault, concluding that the best levels of the factors were: 0.8% resin and addition of iron oxide in the formulation of the template, application of two coats of paint applied with a brush or spray, using hot air in the mold before casting and 24 hours of waiting ready the mold before casting. These levels of the optimized factors were used in an experiment to confirm that ratified the results, helping to reduce rework and consequently reducing costs of cast steel parts.
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DUTRA, Ricardo Peixoto Suassuna ; SILVA, Jaquelígia Brito da ; MORAES, Márcio Luiz Varela Nogueira de ; NASCIMENTO, R. M. ; GOMES, Uilame Umbelino ; PASKOCIMAS, Carlos Alberto . Avaliação da potencialidade de argilas do Rio Grande do Norte. Cerâmica Industrial, v. 13, p. 47-50, 2008.
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The natural gas is an alternative source of energy which is found underground in porous and permeable rocks and being associated or not to the oil. Its basic composition includes methane, other hydrocarbon and compounds such as carbon dioxide, nitrogen, sulphidric gas, mercaptans, water and solid particles. In this work, the dolomite mineral, a double carbonate of calcium and magnesium whose the chemical formula is CaMg(CO3)2, was evaluated as adsorbent material. The material was characterized by granulometric analysis, X-ray fluorescence, X-ray diffraction, thermogravimetric analysis, differential thermal analysis, specific surface area, porosity, scanning electronic microscopy and infrared spectroscopy. Then the material was functionalized with diethanolamine (dolomite+diethanolamine) and diisopropylamine (dolomite+diisopropylamine). The results indicated that the adsorbents presented appropriate physiochemical characteristics for H2S adsorption. The adsorption tests were accomplished in a system coupled to a gas chromatograph and the H2S monitoring in the output of the system was accomplished by a pulsed flame photometric detector (PFPD). The adsorbents presented a significant adsorption capacity. Among the analyzed adsorbents, the dolomite+diethanolamine presented the best capacity of adsorption. The breakthrough curves obtained proved the efficiency of this process