Membrana de alumina anódica: comportamento da microestrutura e estudo das propriedades ópticas após tratamento térmico

Thin commercial aluminum electrolytic and passed through reactions was obtained with anodic alumina membranes nanopores. These materials have applications in areas recognized electronic, biomedical, chemical and biological weapons, especially in obtaining nanostructures using these membranes as a substrate or template for processing nanowires, nanodots and nanofibers for applications noble. Previous studies showed that the membranes that have undergone heat treatment temperature to 1300° C underwent changes in morphology, crystal structure and optical properties. This aim, this thesis, a study of the heat treatment of porous anodic alumina membranes, in order to obtain and to characterize the behavior changes structures during the crystallization process of the membranes, at temperatures ranging between 300 and 1700° C. It was therefore necessary to mount a system formed by a tubular furnace resistive alumina tube and controlled environment, applying flux with special blend of Ag-87% and 13% N2, in which argon had the role of carrying out the oxygen nitrogen system and induce the closing of the pores during the densification of the membrane. The duration of heat treatment ranged from 60 to 15 minutes, at temperatures from 300 to 1700° C respectively. With the heat treatment occurred: a drastic reduction of porosity, grain growth and increased translucency of the membrane. For the characterization of the membranes were analyzed properties: Physical - thermogravimetric, X-ray diffraction, BET surface area; morphological - SEM, EDS through compositional and, optical absorbance, and transmittance in the UV-VIS, and FTIR. The results using the SEM showed that crystallization has occurred, densification and significant changes in membrane structure, as well as obtaining microtube, the BET analysis showed a decrease in specific surface area of the membranes has to 44.381 m2.g-1 to less than 1.8 m2.g-1 and in the analysis of transmittance and absorbance was found a value of 16.5% in the range of 800 nm, characteristic of the near infrared and FTIR have confirmed the molecular groups of the material. Thus, one can say that the membranes were mixed characteristics and properties which qualify for use in gas filtration system, as well as applications in the range of optical wavelength of the infra-red, and as a substrate of nanomaterials. This requires the continuation and deepening of additional study

Construção de um aparato experimental para monitoramento in situ da deposição de filmes finos de titânio por magnetron sputtering

The technique of surface coating using magnetron sputtering is one of the most widely used in the surface engineering, for its versatility in obtaining different films as well as in the micro / nanometric thickness control. Among the various process parameters, those related to the active species of the plasma are of the most fundamental importance in the mechanism and kinetics of deposition. In order to identify the active species of the plasma, parameters such as gas flow, pressure and density of electric power were varied during titanium coating on glass substrate. By flowing argon gas of 10, 20, 30, 40 and 50 sccm (cubic centimeters per minute) for each gas flow a sequential scan of the electric current of 0.10, 0.20, 0.30, 0.40 , 0.50 A. The maximum value of 0.50 A was chosen based both on literature data and on limitations of the equipment. The monitoring of plasma species present during the deposition was carried out in situ by the technique of optical emission spectroscopy (OES) through the spectrometer Ocean Optics USB2000 Series. For this purpose, an apparatus was developed to adapt the OES inside the plasma reactor to stay positioned closest to the target. The radiations emitted by the species were detected by an optical fiber placed behind the glass substrate and their intensities as a function of wavelength were, displayed on a monitor screen. The acquisition time for each condition of the plain parameters was related to the minima of spectral lines intensities due to the film formed on the substrate. The intensities of different emission lines of argon and titanium were then analyzed as a function of time, to determine the active species and estimate the thickness of the deposited films. After the deposition, the coated glasses thin films were characterized by optical transmittance through an infrared laser. It was found that the thickness and deposition rate determined by in situ analysis were consistent with the results obtained by laser transmittance

Redução aluminotérmica do óxido de tântalo usando uma tocha de plasma como ignitor

In this work was used a plasma torch of non transferred arc with argon as work gas, using a power supply with maximum DC current of 250 A and voltage of 30 V to activate the plasma and keep it switched on. The flame temperature was characterized by optical emission spectroscopy, through Boltzmann-plot-method. The torch has been used like igniter in the aluminothermic reduction of the mixture tantalum oxide and aluminum, seeking to obtain metallic tantalum. In heating of the reagents only one particle will be considered to study interactions between plasma-particle, seeking to determinate its fusion and residence time. The early powders were characterized by laser granulometry, scanning electron microscopy (SEM) and X-ray diffraction analysis. The final product of this reaction was characterized by SEM and X-ray diffraction. Crystallite size was calculated by the Scherrer equation and microdeformation was determined using Willamsom-Hall graph. With Rietveld method was possible to quantify the percentile in weight of the products obtained in the aluminothermic reaction. Semi-quantitative chemical analysis (EDS) confirmed the presence of metallic tantalum and Al2O3 as products of the reduction. As was waited the particle size of the metallic tantalum produced, presents values in nanometric scale due the short cooling time of those particles during the process

Novo método para estimativa do gradiente de fratura para poços de petróleo

The development of oil wells drilling requires additional cares mainly if the drilling is in offshore ultra deep water with low overburden pressure gradients which cause low fracture gradients and, consequently, difficult the well drilling by the reduction of the operational window. To minimize, in the well planning phases, the difficulties faced by the drilling in those sceneries, indirect models are used to estimate fracture gradient that foresees approximate values for leakoff tests. These models generate curves of geopressures that allow detailed analysis of the pressure behavior for the whole well. Most of these models are based on the Terzaghi equation, just differentiating in the determination of the values of rock tension coefficient. This work proposes an alternative method for prediction of fracture pressure gradient based on a geometric correlation that relates the pressure gradients proportionally for a given depth and extrapolates it for the whole well depth, meaning that theses parameters vary in a fixed proportion. The model is based on the application of analytical proportion segments corresponding to the differential pressure related to the rock tension. The study shows that the proposed analytical proportion segments reaches values of fracture gradient with good agreement with those available for leakoff tests in the field area. The obtained results were compared with twelve different indirect models for fracture pressure gradient prediction based on the compacting effect. For this, a software was developed using Matlab language. The comparison was also made varying the water depth from zero (onshore wellbores) to 1500 meters. The leakoff tests are also used to compare the different methods including the one proposed in this work. The presented work gives good results for error analysis compared to other methods and, due to its simplicity, justify its possible application

Nova técnica para obtenção de fraturas com altíssima condutividade em poços de petróleo

Increase hydrocarbons production is the main goal of the oilwell industry worldwide. Hydraulic fracturing is often applied to achieve this goal due to a combination of attractive aspects including easiness and low operational costs associated with fast and highly economical response. Conventional fracturing usually involves high-flowing high-pressure pumping of a viscous fluid responsible for opening the fracture in the hydrocarbon producing rock. The thickness of the fracture should be enough to assure the penetration of the particles of a solid proppant into the rock. The proppant is driven into the target formation by a carrier fluid. After pumping, all fluids are filtered through the faces of the fracture and penetrate the rock. The proppant remains in the fracture holding it open and assuring high hydraulic conductivity. The present study proposes a different approach for hydraulic fracturing. Fractures with infinity conductivity are formed and used to further improve the production of highly permeable formations as well as to produce long fractures in naturally fractured formations. Naturally open fractures with infinite conductivity are usually encountered. They can be observed in rock outcrops and core plugs, or noticed by the total loss of circulation during drilling (even with low density fluids), image profiles, pumping tests (Mini-Frac and Mini Fall Off), and injection tests below fracturing pressure, whose flow is higher than expected for radial Darcian ones. Naturally occurring fractures are kept open by randomly shaped and placed supporting points, able to hold the faces of the fracture separate even under typical closing pressures. The approach presented herein generates infinite conductivity canal held open by artificially created parallel supporting areas positioned both horizontally and vertically. The size of these areas is designed to hold the permeable zones open supported by the impermeable areas. The England & Green equation was used to theoretically prove that the fracture can be held open by such artificially created set of horizontal parallel supporting areas. To assess the benefits of fractures characterized by infinite conductivity, an overall comparison with finite conductivity fractures was carried out using a series of parameters including fracture pressure loss and dimensionless conductivity as a function of flow production, FOI folds of increase, flow production and cumulative production as a function of time, and finally plots of net present value and productivity index

Metodologia para avaliação de cinemática de partículas gasosas em fluidos de viscosidade variável com o tempo e sua aplicação na construção de poços de petróleo

Many challenges have been presented in petroleum industry. One of them is the preventing of fluids influx during drilling and cementing. Gas migration can occur as result of pressure imbalance inside the well when well pressure becomes lower than gas zone pressure and in cementing operation this occurs during cement slurry transition period (solid to fluid). In this work it was developed a methodology to evaluate gas migration during drilling and cementing operations. It was considered gel strength concept and through experimental tests determined gas migration initial time. A mechanistic model was developed to obtain equation that evaluates bubble displacement through the fluid while it gels. Being a time-dependant behavior, dynamic rheological measurements were made to evaluate viscosity along the time. For drilling fluids analyzed it was verified that it is desirable fast and non-progressive gelation in order to reduce gas migration without affect operational window (difference between pore and fracture pressure). For cement slurries analyzed, the most appropriate is that remains fluid for more time below critical gel strength, maintaining hydrostatic pressure above gas zone pressure, and after that gels quickly, reducing gas migration. The model developed simulates previously operational conditions and allow changes in operational and fluids design to obtain a safer condition for well construction

Diversidade de espécies e ecologia da comunidade de lagartos de um fragmento de Mata Atlântica no nordeste do Brasil

Neste estudo foram investigadas a diversidade, a composição, e as diferenças no uso do espaço (hábitat e microhábitat) e do alimento em uma comunidade de lagartos habitantes da serapilheira de um fragmento de Mata Atlântica, do Estado de Alagoas, Brasil. Para a observação e/ou coleta dos espécimes, foram utilizados os métodos de busca ativa e armadilhas de queda (pit-fall traps) sem cerca-guia. Para análises de diversidade e da existência de diferenças de diversidade entre os hábitats e microhábitats, utilizou-se o índice de Shannon. A largura dos nichos espacial (hábitat e microhábitat) e alimentar foi avaliada, utilizando-se o índice de diversidade de Simpson. A similaridade entre as áreas foi averiguada utilizando-se o índice de Jaccard. Para avaliar o grau de sobreposição quanto ao uso do espaço (hábitats e microhábitats) e do alimento pelas espécies, foi utilizada uma versão da equação de MarcArthur & Levis. Foram obtidas vinte e três espécies de lagartos, pertencentes a nove famílias; destas, dezenove foram obtidas no interior da mata e nove na borda. Para o interior da mata as espécies mais abundantes foram Kentropyx calcarata, Dryadosaura nordestina, Enyalius catenatus e Gymnodactylus darwinii. Na borda da mata as espécies mais abundantes foram Tropidurus hispidus, T. semitaeniatus, Ophiodes striatus e Ameiva ameiva. Quanto à utilização dos recursos, os resultados mostraram que espécies filogeneticamente próximas nem sempre utilizam de maneira semelhante os recursos disponíveis. A dieta em geral foi composta por artrópodes. Tropidurus hispidus e T. semitaeniatus se mostraram especialistas no consumo de Himenoptera (Formicidae), que estiverem presentes em 100% dos seus estômagos. Ophiodes striatus teve como principal alimento caramujos (Gastropoda) e aranhas com 60% cada; sendo Gastropoda mais abundante para esta espécie

Estimativa da área foliar do antúrio com o uso de funções de regressão

O presente trabalho teve como objetivo determinar quais variáveis dimensionais da folha são mais adequadas para utilização na estimativa da área foliar do antúrio (Anthurium andraeanum), cv. Apalai, por meio de equação de regressão linear, e comparar o desempenho de diferentes funções de regressão obtidas com o uso de aprendizado de máquina (AM). A variável que melhor estimou a área foliar foi o produto das dimensões lineares (comprimento e largura), CxL, sendo a equação proposta Af = 0.9672 *C x L, com coeficiente de determinação (R²) de 0,99. Verificou-se, também, com o uso de AM, que as funções lineares são mais adequadas para a estimação da área foliar dessa espécie vegetal.

Modelo matemático para predição do VO2máx em cicloergômetro baseado na análise dos gases expirados

Existem diversas equações para predição do VO2máx a partir de variáveis dentro do teste ergométrico em vários ergômetros, no entanto equação semelhante utilizando os limiares ventilatórios na ergoespirometria em teste sub-máximo no cicloergômetro não está disponível. O objetivo do presente estudo foi avaliar a precisão de modelos de predição do VO2máx com base em indicadores de esforço sub-máximo. Neste sentido foram testados em protocolo incremental máximo no cicloergômetro 7.877 voluntários, sendo 4640 indivíduos do sexo feminino e 3147 do sexo masculino, todos saudáveis não atletas, com idades acima de 20 anos, divididos randomicamente em dois grupos: A de estimação e B de validação. A partir das variáveis independentes massa corporal (MC) em kg, carga de trabalho no limiar 2 (WL2) e freqüência cardíaca no limiar 2 (FCL2) foi possível construir um modelo de regressão linear múltipla para predição do VO2máx. Os resultados demonstram que em indivíduos saudáveis não atletas de ambos os sexos é possível predizer o VO2máx com um erro mínimo (EPE = 1,00%) a partir de indicadores submáximos obtidos em teste incremental. O caráter multidisciplinar do trabalho pôde ser caracterizado pelo emprego de técnicas que envolveram pneumologia, educação física, fisiologia e estatística

Estado nutricional antropométrico, composição corporal e pressão arterial em adolescentes

Os objetivos deste trabalho foram: (1) estimar as prevalências de excesso de peso e de gordura corporal, obesidade central e pressão arterial elevada (PAE) em adolescentes beneficiários do Programa Nacional de Alimentação Escolar (PNAE) da rede municipal de ensino de Natal-RN; (2) verificar a associação entre variáveis antropométricas e de composição corporal com a pressão arterial, a maturação sexual e a história familiar positiva de fatores de risco para doença cardiovascular (FRDCV); (3) comparar dois padrões de referência para classificação do excesso de peso em adolescentes; e (4) propor equações preditivas de massa gorda (MG) e massa livre de gordura (MLG) baseadas nos perímetros corporais. Trata-se de um estudo transversal, com 526 adolescentes beneficiários do PNAE, em Natal, Brasil. O tamanho da população de estudo foi definido por amostragem aleatória, em dois estágios, e ponderada segundo número de alunos de cada escola. No primeiro estudo, o excesso de peso foi determinado por Índice de Massa Corporal (IMC), a gordura corporal estimada por dobras cutâneas e a obesidade central por perímetro abdominal. A pressão arterial elevada foi classificada conforme a American Academy of Pediatrics. As prevalências foram apresentadas em valores relativos e efeito do desenho. Realizou-se uma análise fatorial para sintetizar o conjunto de variáveis antropométricas visando identificar fatores comuns. Extraíram-se dois fatores: (1) padrão excesso de adiposidade e (2) padrão adiposidade central elevada. Para avaliar a associação entre os padrões de adiposidade corporal com pressão arterial elevada, faixa etária, maturação sexual e história familiar de FRDCV utilizou-se a Razão de Chances e respectivo intervalo de confiança de 95% e regressão logística. No segundo estudo, calculou-se a sensibilidade e a especificidade do excesso de peso classificado segundo o IOTF e a World Health Organization WHO em relação ao excesso de adiposidade corporal; e a estatística Kappa para medir a concordância entre os dois padrões de referência. No terceiro estudo, foram elaborados modelos preditivos de MG e MLG com base em nove perímetros corporais, utilizando a bioimpedância Byodinamics 450 como padrão de referência. Para tanto foram selecionados 218 adolescentes eutróficos, segundo o IMC a partir do estudo transversal. As equações foram estimadas por regressão linear múltipla, considerando a idade e os perímetros corporais. Os resultados apontaram que 14,1% dos meninos e 15,7% das meninas tinham excesso de peso; 15,3% dos meninos e 11,6% das meninas tinham excesso de gordura corporal e dentre os meninos 14,3% tinham pressão arterial elevada e as meninas, 21,4%. Todos os efeitos do desenho foram inferiores a 2,5%. Nos meninos, o padrão excesso de adiposidade foi associado à história familiar positiva de FRDCV (ORajust=2,60; 1,09-6,22), maturação sexual (ORajust=2,92; 1,04-8,22) e PAE (ORajust=3,66; 1,34-9,94). Os meninos com 12 anos e mais apresentaram 6,1 vezes mais chance de apresentar padrão adiposidade central elevada do que os adolescentes com 10 a 11 anos (IC95% 2,32-16,04), assim como os púberes apresentaram 3,2 vezes este mesmo padrão em relação aos pré-púberes (IC95%1,14-8,85). A partir da comparação entre os dois padrões de referencia de classificação do excesso de peso por meio do IMC, observou-se que a sensibilidade foi de 79,3% para o critério IOTF e de 88,9% para WHO e a especificidade foi de 94,7% e 89,9%, respectivamente. O nível de concordância foi maior para o critério IOTF (Kappa=0,70 x Kappa=0,64). Em relação à construção das equações preditivas de gordura corporal, do total de 106 meninos e 112 meninas, foram desenvolvidas duas equações para estimar MG e duas para MLG, considerando o sexo. No sexo masculino, a equação para estimar a MG incluiu as variáveis idade, punho, quadril e perímetro abdominal (R2=0,552; AIC=416,04) e MLG, idade, punho e antebraço (R2=0,869; AIC=578,24). Enquanto que no feminino, MG foi estimada pelas variáveis punho, perímetro do abdômen, do quadril, da coxa proximal e da panturrilha (R2=0,838; AIC=415,36); e a MLG por idade, punho, perímetro do abdômen, do quadril e da panturrilha (R2=0,878; AIC=512,48). Conclui-se que os adolescentes tinham elevada prevalência de excesso de adiposidade corporal e de pressão arterial elevada. Tanto o padrão excesso de adiposidade quanto adiposidade central elevada constituem-se em padrões de risco. O padrão excesso de adiposidade foi associado à pressão arterial, história familiar positiva de FRDCV e maturação sexual em meninos. O critério IOTF mostrou-se menos sensível, mais específico, com maior nível de concordância e maior probabilidade de identificar corretamente o excesso de gordura corporal nos adolescentes avaliados. Quatro equações foram desenvolvidas para a estimativa da MG e MLG em adolescentes. As equações desenvolvidas para estimar a MG no sexo feminino e MLG para ambos os sexos apresentaram valores elevados de coeficiente de determinação ajustados e, portanto, são as preferenciais. Este estudo foi realizado com a participação de equipe multidisciplinar composta por professores da área de Nutrição, Endocrinologia Pediátrica, Estatística, Educação Física, discentes do Curso de Graduação em Nutrição e residentes em Pediatria

Faecal bacteria in Perna perna (Linnaeus, 1758) (Mollusca: Bivalvia) for biomonitoring coastal waters and seafood quality

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

Influência da hereditariedade nas capacidades motoras, na aptidão física e antropometria

Conselho Nacional de Desenvolvimento Científico e Tecnológico

Avaliação de um método de cromatografia em fase gasosa head space e estudo da estabilidade do etanol em amostras de sangue

The ethanol is the most overused psychoactive drug over the world; this fact makes it one of the main substances required in toxicological exams nowadays. The development of an analytical method, adaptation or implementation of a method known, involves a process of validation that estimates its efficiency in the laboratory routine and credibility of the method. The stability is defined as the ability of the sample of material to keep the initial value of a quantitative measure for a defined period within specific limits when stored under defined conditions. This study aimed to evaluate the method of Gas chromatography and study the stability of ethanol in blood samples, considering the variables time and temperature of storage, and the presence of preservative and, with that check if the conditions of conservation and storage used in this study maintain the quality of the sample and preserve the originally amount of analyte present. Blood samples were collected from 10 volunteers to evaluate the method and to study the stability of ethanol. For the evaluation of the method, part of the samples was added to known concentrations of ethanol. In the study of stability, the other side of the pool of blood was placed in two containers: one containing the preservative sodium fluoride 1% and the anticoagulant heparin and the other only heparin, was added ethanol at a concentration of 0.6 g/L, fractionated in two bottles, one being stored at 4ºC (refrigerator) and another at -20ºC (freezer), the tests were performed on the same day (time zero) and after 1, 3, 7, 14, 30 and 60 days of storage. The assessment found the difference in results during storage in relation to time zero. It used the technique of headspace associated with gas chromatography with the FID and capillary column with stationary phase of polyethylene. The best analysis of chromatographic conditions were: temperature of 50ºC (column), 150ºC (jet) and 250ºC (detector), with retention time for ethanol from 9.107 ± 0.026 and the tercbutanol (internal standard) of 8.170 ± 0.081 minutes, the ethanol being separated properly from acetaldehyde, acetone, methanol and 2-propanol, which are potential interfering in the determination of ethanol. The technique showed linearity in the concentration range of 0.01 and 3.2 g/L (0.8051 x + y = 0.6196; r2 = 0.999). The calibration curve showed the following equation of the line: y = x 0.7542 + 0.6545, with a linear correlation coefficient equal to 0.996. The average recovery was 100.2%, the coefficients of variation of accuracy and inter intra test showed values of up to 7.3%, the limit of detection and quantification was 0.01 g/L and showed coefficient of variation within the allowed. The analytical method evaluated in this study proved to be fast, efficient and practical, given the objective of this work satisfactorily. The study of stability has less than 20% difference in the response obtained under the conditions of storage and stipulated period, compared with the response obtained at time zero and at the significance level of 5%, no statistical difference in the concentration of ethanol was observed between analysis. The results reinforce the reliability of the method of gas chromatography and blood samples in search of ethanol, either in the toxicological, forensic, social or clinic

Controle de qualidade físico-químico e biodisponibilidade relativa em ratos de suspensões orais de naproxeno sódico obtidas de farmácias de manipulação na cidade do Natal RN

Compounded medicines have been reported by the ANVISA due to decreased of the therapeutic response or toxicity of these formulations. The aim of this work was to investigate the physicochemical quality control among naproxen sodium oral suspensions 25 mg/mL obtained from six compounding pharmacies (A, B, C, D, E and F) and the manufactured suspension (R). In the quality control test, the tests of pH, content, homogeneity, volume and physical and organoleptic characteristics were performed according to the Brazilian Pharmacopoeia. The analytical method for determination of naproxen in suspensions was validate. This method showed excellent precision, accuracy, linearity and specificity. In the content test the suspensions B, C and E showed lower value and the F suspension showed a high value of the content. The products C and E were disapproved in the description of the physical and organoleptic characteristics test. In the pH test, three suspensions were outside specifications (C, E and F). Only the products R, A and D showed satisfactory results in these tests and therefore they were approved for relative bioavailability test. The R, A and D suspensions were orally administered to Wistar rats and the blood samples were taken at time intervals of 10, 20, 40, 60 min, 3, 4, 6, 24 and 48 h. The plasma samples were immediately stored at 80 ºC until analysis of HPLC. The bioanalytical method validation showed specificity, linearity (R2 0.9987), precision, accuracy, good recovery and stability. The chromatographic conditions were: flow rate of 1.2 mL.min-1 with a mobile phase of acetonitrile : sodium phosphate buffer pH 4.0 (50:50, v/v) at 280 nm, using a C18 column. The confidence interval of 90% for the Cmax and AUCt ratio was within the range of 80 - 125% proposed by the FDA. Only one suspension, obtained from the compounding pharmacy D, was considered bioequivalent to the rate of absorption under the conditions proposed by this study. Thus, the results indicate the need for strict supervision from the relevant authorities to ensure the patient safety and the quality of compounded drugs by pharmacies

Fator de visão do céu e intensidade de ilhas de calor na escala do pedestre

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