Desenvolvimento e validação de método analítico para determinação de WE010, WE014 e WE017

The synthetic guanylhydrazones WE010 (3,5-di-tert-butil-4-hidroxibenzaldehyde-guanylhydrazone), WE014 (4-bifenilcarboxialdehydeguanylhydrazone) and WE017 (3,4-diclorobenzaldehydeguanylhydrazone) showed high cytotoxic activity in terms of percentage inhibition of cancer cells growth. However, further progress in the development of these drug candidates requires precise and convenient methods for their qualitative and quantitative analyses. The aim of this study was to develop and validate High Performance Liquid Chromatography with diode-array detection (HPLC-DAD) and Ultra Fast Liquid Chromatography with diode-array detection (UFLC-DAD) methods suitable for as simultaneous as isolated determination of studied guanylhydrazones, based on the optimization of chromatographic parameters and obtaining reduced detection times. The chromatographic analyses of analytes by HPLC were performed on C18 ACE analytical column (150 mm x 4.6 mm), with a particle size of 5.0 μm. Among all the conditions assayed, the best results of separation were obtained with a mixture of methanol:water (60:40, v/v) as the mobile phase at a flow rate 1.5mL/min and pH of 3.5 adjusted at acetic acid. The UFLC method was developed by experimetal desing techniques in order to find optimal chromatographic analytical conditions, which were achieved on XR-ODS analytical column (50 mm x 3.0 mm), with a particle size of 2,2 μm, maintained at 25 ºC. The mobile phase was consisted of methanol:water (65:35, v/v) with 0.1% triethylamine (TEA) and pH of 3.5 adjusted at acetic acid, at a flow rate 0.5 mL/min. The procedure were validated following evaluating parameters such as specificity, linearity, limits of detection (LD) and quantification (LQ), precision, accuracy and robustness, giving results within the acceptable range. Although the UFLC method shows better sensitivity (lower values of LD and LQ), robustness (lower rates of relative standard deviation) and minimize spending time and solvent, both developed methods were adequately applied to the analysis of guanylhydrazones molecules, may be used in routine of quality control laboratories. Keywords: guanylhydrazones, HPLC/DAD, UFLC/DAD, validation of analitical method

Determinação dos parâmetros do controlador preditivo generalizado com função de pesos variante no tempo através de algoritmos genéticos

The predictive control technique has gotten, on the last years, greater number of adepts in reason of the easiness of adjustment of its parameters, of the exceeding of its concepts for multi-input/multi-output (MIMO) systems, of nonlinear models of processes could be linearised around a operating point, so can clearly be used in the controller, and mainly, as being the only methodology that can take into consideration, during the project of the controller, the limitations of the control signals and output of the process. The time varying weighting generalized predictive control (TGPC), studied in this work, is one more an alternative to the several existing predictive controls, characterizing itself as an modification of the generalized predictive control (GPC), where it is used a reference model, calculated in accordance with parameters of project previously established by the designer, and the application of a new function criterion, that when minimized offers the best parameters to the controller. It is used technique of the genetic algorithms to minimize of the function criterion proposed and searches to demonstrate the robustness of the TGPC through the application of performance, stability and robustness criterions. To compare achieves results of the TGPC controller, the GCP and proportional, integral and derivative (PID) controllers are used, where whole the techniques applied to stable, unstable and of non-minimum phase plants. The simulated examples become fulfilled with the use of MATLAB tool. It is verified that, the alterations implemented in TGPC, allow the evidence of the efficiency of this algorithm

Determinação de Chaveamento para Recomposição do Serviço em Redes de Distribuição de Energia Elétrica em Média Tensão Através de Métodos Baseado em Parâmetros de Sensibilidade

The reconfiguration of a distribution network is a change in its topology, aiming to provide specific operation conditions of the network, by changing the status of its switches. It can be performed regardless of any system anomaly. The service restoration is a particular case of reconfiguration and should be performed whenever there is a network failure or whenever one or more sections of a feeder have been taken out of service for maintenance. In such cases, loads that are supplied through lines sections that are downstream of portions removed for maintenance may be supplied by the closing of switches to the others feeders. By classical methods of reconfiguration, several switches may be required beyond those used to perform the restoration service. This includes switching feeders in the same substation or for substations that do not have any direct connection to the faulted feeder. These operations can cause discomfort, losses and dissatisfaction among consumers, as well as a negative reputation for the energy company. The purpose of this thesis is to develop a heuristic for reconfiguration of a distribution network, upon the occurrence of a failure in this network, making the switching only for feeders directly involved in this specific failed segment, considering that the switching applied is related exclusively to the isolation of failed sections and bars, as well as to supply electricity to the islands generated by the condition, with significant reduction in the number of applications of load flows, due to the use of sensitivity parameters for determining voltages and currents estimated on bars and lines of the feeders directly involved with that failed segment. A comparison between this process and classical methods is performed for different test networks from the literature about networks reconfiguration

Um método para determinação da profundidade combinando visão estéreo e autocalibração para aplicação em robótica móvel

This work proposes a method to determine the depth of objects in a scene using a combination between stereo vision and self-calibration techniques. Determining the rel- ative distance between visualized objects and a robot, with a stereo head, it is possible to navigate in unknown environments. Stereo vision techniques supply a depth measure by the combination of two or more images from the same scene. To achieve a depth estimates of the in scene objects a reconstruction of this scene geometry is necessary. For such reconstruction the relationship between the three-dimensional world coordi- nates and the two-dimensional images coordinates is necessary. Through the achievement of the cameras intrinsic parameters it is possible to make this coordinates systems relationship. These parameters can be gotten through geometric camera calibration, which, generally is made by a correlation between image characteristics of a calibration pattern with know dimensions. The cameras self-calibration allows the achievement of their intrinsic parameters without using a known calibration pattern, being possible their calculation and alteration during the displacement of the robot in an unknown environment. In this work a self-calibration method based in the three-dimensional polar coordinates to represent image features is presented. This representation is determined by the relationship between images features and horizontal and vertical opening cameras angles. Using the polar coordinates it is possible to geometrically reconstruct the scene. Through the proposed techniques combination it is possible to calculate a scene objects depth estimate, allowing the robot navigation in an unknown environment

Análise de antenas de microfita em rampa com múltiplas camadas dielétricas

The present work deals with the ana1ysis of microstrip patch antennas printed on tapered dielectric substrates. We investigate the influence ofthe substrate height variations on the properties of configurations such as microstrip patch antennas, microstrip patch antennas with overlay and suspendeô microstrip patch antennas. The dielectric substrates can be isotropic or anisotropic ones. This accurate analysis is based on the full-wave formulation. It is carried out initially for the determination of the impedance matrix, through the use of the spectral¬domain immitance approach. We use a model based on a segmentation of the considered line into uniform microstrip line subsections. Normalized phase constants and characteristic impedances are obtained by means of the Galerkin numerical technique. Then, the cascaded combination of the uniform microstrip subsections are analyzed through an interactive procedure. Numerical results are presented for the input reflection coefficient, voltage standing wave ratio, resonant frequency, and radiation pattems ofthe E_plane and H-plane diagrams. It is found that the variations in the substrate height profile produce a great influence on the bandwidth of microstrip antennas. This procedure gives bandwidth improvements without altering considerably the resonant frequency. Furthermore, the tapered microstrip antenna can be used as a lightweight altemative for bandwidth control and to eXtend the use of microstiip antenna technology to a wider variety of applications. Finally, suggestions for the continuity of this work are presented

Sistema inteligente para determinação das direções de chegada de múltiplos sinais em arranjos de antenas

This dissertation presents a new proposal for the Direction of Arrival (DOA) detection problem for more than one signal inciding simultaneously on an antennas array with linear or planar geometry by using intelligent algorithms. The DOA estimator is developed by using techniques of Conventional Beam-forming (CBF), Blind Source Separation (BSS), and the neural estimator MRBF (Modular Structure of Radial Basis Functions). The developed MRBF estimator has its capacity extended due to the interaction with the BSS technique. The BSS makes an estimation of the steering vectors of the multiple plane waves that reach the array in the same frequency, that means, obtains to separate mixed signals without information a priori. The technique developed in this work makes possible to identify the multiple sources directions and to identify and to exclude interference sources

Estudo da estimativa da incerteza de medição para determinação do BS&W e da vazão aplicado no laboratório de avaliação de medição do petróleo

The considered work presents the procedure for evaluation of the uncertainty related to the calibration of flow measurers and to BS&W. It is about a new method of measurement purposed by the conceptual project of the laboratory LAMP, at Universidade Federal do Rio Grande do Norte, that intends to determine the conventional true value of the BS&W from the total height of the liquid column in the auditor tank, hydrostatic pressure exerted by the liquid column, local gravity, specific mass of the water and the specific mass of the oil, and, to determine the flow, from total height of liquid column and transfer time. The calibration uses a automatized system of monitoration and data acquisition of some necessary largnesses to determine of flow and BS&W, allowing a better trustworthiness of through measurements

Estudo das propriedades termofísicas com variação da expansibilidade de compósito desenvolvido com matriz PUR-NOP e carga funcional de argilomineral

In this study were conducted experimental procedures for determination of variation of the expandability of rigid polyurethane foam (PUR) from a natural oil polyol (NOP), specifically the Castor oil plant, Ricinus communis, pure and additions of the vermiculite in phase dispersed in different percentage within a range from 0% to 20%, mass replacement. From the information acquired, were defined the parameters for production of bodies of test, plates obtained through controlled expansion, with the final volume fixed. Initially, the plates were subjected to thermal performance tests and evaluated the temperature profiles, to later be extracted samples duly prepared in accordance with the conditions required for each test. Was proceeded then the measurement of the coefficient of thermal conductivity, volumetric capacity heat and thermal diffusivity. The findings values were compared with the results obtained in the tests of thermal performance, contributing to validation of the same. Ultimately, it was investigated the influence that changes in physical-chemical structure of the material had exerted on the variation of thermophysical quantities through gas pycnometry, scanning electron microscopy (SEM) combined with energy dispersive X-ray fluorescence spectroscopy (EDXRF), infrared spectroscopy using Fourier transform (FTIR), thermogravimetric analysis (TGA) and differential thermal analysis (DTA). Based on the results obtained was possible to demonstrate that all load percentage analyzed promoted an increase in the potential expansion (PE) of the resin. In production of the plates, the composites with density near at the free expansion presented high contraction during the cure, being the of higher density adopted as definitive standard. In the thermal performance tests, the heating and cooling curves of the different composites had presented symmetry and values very close for lines of the temperature. The results obtained for the thermophysical properties of composites, showed little difference in respect of pure foam. The percentage of open pores and irregularities in the morphology of the composites were proportionate to the increment of vermiculite. In the interaction between the matrix and dispersed phase, there were no chemical transformations in the region of interface and new compounds were not generated. The composites of PUR-NOP and vermiculite presented thermal insulating properties near the foam pure and percentage significantly less plastic in its composition, to the formulation with 10% of load

Análise tribológica das malhas multifuncionais obtidas por multicamadas

The present work consists in the analysis of tribologycal properties of basic and multifunctional knitted fabrics. This knowledge has fundamental importance for the textile industry since it can quantify, in an objective way, the tactil. The fabrics used were characterized by friction and mechanical tests for determining the viscoelastic region, wear resistance and friction coefficient of the fabrics used. The stress-strain curve was obtained by the method Kawabata, KES-FB1. Wear tests performed with the aid of equipment Martindale. The measurement of friction coefficient, two methods were used and analyzed comparatively. The first was a method already established worldwide known as KES-FB4 and the second was an innovative method called FRICTORQ, developed by the University of Minho. These two methods were compared taking into account the relative motion between the tribologycal pairs are different from each method. While the first motion is translational, the second is rotational. It was formal that the knitted had a multifunctional fabrics tribologycal performance which was better than the basic knitted fabrics, as the viscoelastic region, was laager highlighting a multifunctional structure, with greater wear resistance mainly on the back side of the knitted fabrics and lower friction coefficient. Performing a comparative analysis between two methods used to measure the friction coefficient, it was formal that both methods were consistent in terms of results. In operational terms, the FRICTORQ showed ease of operation and increased reproducibility of results

Painéis-sanduíche com núcleo de EPS reciclado: metodologia de execução e determinação de propriedades termofísicas

New materials made from industrial wastes have been studied as an alternative to traditional fabrication processes in building and civil engineering. These materials are produced considering some issues like: cost, efficiency and reduction of nvironmental damage. Specifically in cases of materials destined to dwellings in low latitude regions, like Brazilian Northeast, efficiency is related to mechanical and thermal resistance. Thus, when thermal insulation and energetic efficiency are aimed, it s important to increase thermal resistance without depletion of mechanical properties. This research was conducted on a construction element made of two plates of cement mortar, interspersed with a plate of recycled expanded polystyrene (EPS). This component, widely known as sandwich-panel, is commonly manufactured with commercial EPS whose substitution was proposed in this study. For this purpose it was applied a detailed methodology that defines parameters to a rational batching of the elements that constitute the nucleus. Samples of recycled EPS were made in two different values of apparent specific mass (ρ = 65 kg/m³; ρ = 130 kg/m³) and submitted to the Quick-Line 30TM that is a thermophysical properties analyzer. Based on the results of thermal conductivity, thermal capacity and thermal diffusivity obtained, it was possible to assure that recycled EPS has thermal insulation characteristics that qualify it to replace commercial EPS in building and civil engineering industry

Análise teórico-experimental do coeficiente de perfomance (COP) de um sistema de refrigeração por jato-compressão

The use of waste heat of energy conversion equipment to produce a cooling effect, consists currently in a very interesting way of efficiency improvement of energy systems. The present research has as intention the theoretical and experimental study of a new intermittent refrigeration system ejector cycle characteristics, with use of waste heat. Initially, was doing a bibliographical survey about the vapor ejector refrigeration system technology. In the following stage was doing a simulation of the corresponding thermodynamic cycle, with preliminarily intention to evaluate the performance of the system for different refrigerants fluids. On the basis of the results of the simulation were selected the refrigerant fluid and developed an experimental group of benches of the refrigeration system considered, where pressure and temperature sensory had been inserted in strategical points of the refrigeration archetype and connected to a computerized data acquisition system for measure the refrigerant fluid properties in the thermodynamic cycle. The test results obtained show good agreement with the literature

Avaliação do comportamento tribológico de compósitos poliéster/fibra de vidro utilizando resíduos de poliéster/fibra de vidro e carbonato de cálcio como carga

The use of composite materials and alternative is being increased every day, as it becomes more widespread awareness that the use of renewable and not harmful to the environment is part of a new environmentally friendly model. Since its waste (primarily fiberglass) can not be easily recycled by the difficulty that still exists in this process, since they have two phases mixed, a polymeric matrix thermoset difficult to recycle because it is infusible and phase of fiber reinforcements. Thermoset matrix composites like Polyester + fiberglass pose a threat due to excessive discharge. Aiming to minimize this problem, aimed to reuse the composite Polyester + fiber glass, through the wastes obtained by the grinding of knifes and balls. These residues were incorporated into the new composite Polyester/Fiberglass for hot compression mold and compared tribological to composites with filler CaCO3, generally used as filler, targeting a partial replacement of CaCO3 by such waste. The composites were characterized by thermal analysis (TGA, DSC and DMA), by the surface integrity (roughness determination, contact angle and surface energy), mechanical properties (hardness) and tribological tests (wear and coefficient of dynamic friction) in order to evaluate the effect of loads and characterize these materials for applications that can take, in the tribological point of view since waste Polyester + fiberglass has great potential for replacement of CaCO3

Determinação experimental e modelagem termodinâmica do ponto de turbidez de sistemas aquosos com tensoativos nonilfenolpolietoxilados

The nonionic surfactants are composed of substances whose molecules in solution, does not ionize. The solubility of these surfactants in water due to the presence of functional groups that have strong affinity for water. When these surfactants are heated is the formation of two liquid phases, evidenced by the phenomenon of turbidity. This study was aimed to determine the experimental temperature and turbidity nonilfenolpoliethoxyled subsequently perform a thermodynamic modeling, considering the models of Flory-Huggins and the empirical solid-liquid equilibrium (SLE). The method used for determining the turbidity point was the visual method (Inoue et al., 2008). The experimental methodology consisted of preparing synthetic solutions of 0,25%, 0,5%, 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 12,5%, 15%, 17% and 20% by weight of surfactant. The nonionic surfactants used according to their degree of ethoxylation (9.5, 10, 11, 12 and 13). During the experiments the solutions were homogenized and the bath temperature was gradually increased while the turbidity of the solution temperature was checked visually Inoue et al. (2003). These temperature data of turbidity were used to feed the models evaluated and obtain thermodynamic parameters for systems of surfactants nonilfenolpoliethoxyled. Then the models can be used in phase separation processes, facilitating the extraction of organic solvents, therefore serve as quantitative and qualitative parameters. It was observed that the solidliquid equilibrium model (ESL) was best represented the experimental data.

Determinação de dados de equilíbrio líquido-vapor a altas pressões para sistemas de hidrocarbonetos assimétricos

Crude oil is a complex liquid mixture of organic and inorganic compounds that are dominated by hydrocarbons. It is a mixture of alkanes from the simplest to more complex aromatic compounds that are present derivatives such as gasoline, diesel, alcohol, kerosene, naphtha, etc.. These derivatives are extracted from any oil, however, only with a very high quality, in other words, when the content of hydrocarbons of low molecular weight is high means that production of these compounds is feasible. The American Petroleum Institute (API) developed a classification system for the various types of oil. In Brazil, the quality of most of the oil taken from wells is very low, so it is necessary to generate new technology to develop best practices for refining in order to produce petroleum products of higher commercial value. Therefore, it is necessary to study the thermodynamic equilibrium properties of its derivative compounds of interest. This dissertation aims to determine vapor-liquid equilibrium (VLE) data for the systems Phenilcyclohexane - CO2, and Cyclohexane - Phenilcyclohexane - CO2 at high pressure and temperatures between 30 to 70oC. Furthermore, comparisons between measured VLE experimental data from this work and from the literature in relation to the Peng- Robinson molecular thermodynamic model, using a simulation program SPECS IVCSEP v5.60 and two adjustable interaction parameters, have been performed for modeling and simulation purposes. Finally, the developed apparatus for determination of phase equilibrium data at high pressures is presented

Recuperação e purificação de quitosanases usando adsorção em leito expandido com streamline DEAE com modelagem e simulação usando redes neurais

Expanded Bed Adsorption (EBA) is an integrative process that combines concepts of chromatography and fluidization of solids. The many parameters involved and their synergistic effects complicate the optimization of the process. Fortunately, some mathematical tools have been developed in order to guide the investigation of the EBA system. In this work the application of experimental design, phenomenological modeling and artificial neural networks (ANN) in understanding chitosanases adsorption on ion exchange resin Streamline® DEAE have been investigated. The strain Paenibacillus ehimensis NRRL B-23118 was used for chitosanase production. EBA experiments were carried out using a column of 2.6 cm inner diameter with 30.0 cm in height that was coupled to a peristaltic pump. At the bottom of the column there was a distributor of glass beads having a height of 3.0 cm. Assays for residence time distribution (RTD) revelead a high degree of mixing, however, the Richardson-Zaki coefficients showed that the column was on the threshold of stability. Isotherm models fitted the adsorption equilibrium data in the presence of lyotropic salts. The results of experiment design indicated that the ionic strength and superficial velocity are important to the recovery and purity of chitosanases. The molecular mass of the two chitosanases were approximately 23 kDa and 52 kDa as estimated by SDS-PAGE. The phenomenological modeling was aimed to describe the operations in batch and column chromatography. The simulations were performed in Microsoft Visual Studio. The kinetic rate constant model set to kinetic curves efficiently under conditions of initial enzyme activity 0.232, 0.142 e 0.079 UA/mL. The simulated breakthrough curves showed some differences with experimental data, especially regarding the slope. Sensitivity tests of the model on the surface velocity, axial dispersion and initial concentration showed agreement with the literature. The neural network was constructed in MATLAB and Neural Network Toolbox. The cross-validation was used to improve the ability of generalization. The parameters of ANN were improved to obtain the settings 6-6 (enzyme activity) and 9-6 (total protein), as well as tansig transfer function and Levenberg-Marquardt training algorithm. The neural Carlos Eduardo de Araújo Padilha dezembro/2013 9 networks simulations, including all the steps of cycle, showed good agreement with experimental data, with a correlation coefficient of approximately 0.974. The effects of input variables on profiles of the stages of loading, washing and elution were consistent with the literature