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

Distribuição do sistema radicular da goiabeira 'Rica' produzida a partir de estaquia herbácea

O conhecimento da distribuição do sistema radicular de plantas, principalmente de perenes, não é muito estudado, devido a inúmeros fatores, dentre os quais, a dificuldade inerente ao método de amostragem. A presente pesquisa objetivou conhecer o sistema radicular da goiabeira através do método de escavação. Utilizando jatos de água, retirou-se a terra até um volume de 10 m³ (5x5x0,4m), subdivididos em paralelepípedos de 0,1 m³ (0,5x0,5x0,4m), expondo o sistema radical da goiabeira 'Rica'. Verificou-se um vigoroso sistema radicular sem a caracterização da raiz principal e com distribuição homogênea, grande número de raízes primárias, proporcionado pela adequada formação de mudas, através de estaquia herbácea.

Desenho e Construção de um protótipo gerador de jato de plasma frio a pressão atmosférica para aplicações biomédicas

Research for better performance materials in biomedical applications are constants. Thus recent studies aimed at the development of new techniques for modification of surfaces. The low pressure plasma has been highlighted for its versatility and for being environmentally friendly, achieving good results in the modification of physic chemical properties of materials. However, it is requires an expensive vacuum system and cannot able to generate superficial changes in specific regions. Furthermore, it is limits their use in polymeric materials and sensitive terms due to high process temperatures. Therefore, new techniques capable of generating cold plasma at atmospheric pressure (APPJ) were created. In order to perform surface treatments on biomaterials in specific regions was built a prototype capable of generating a cold plasma jet. The prototype plasma generator consists of a high voltage source, a support arm, sample port and a nozzle through which the ionized argon. The device was formed to a dielectric tube and two electrodes. This work was varied some parameters such as position between electrodes, voltage and electrical frequency to verify the behavior of glow discharges. The disc of titanium was polished and there was a surface modification. The power consumed, length, intensity and surface modifications of titanium were analyzed. The energy consumed during the discharges was observed by the Lissajous figure method. To check the length of the jets was realized with Image Pro Plus software. The modifications of the titanium surfaces were observed by optical microscopy (OM ) and atomic force microscopy (AFM ). The study showed that variations of the parameters such as voltage, frequency and geometric position between the electrodes influence the formation of the plasma jet. It was concluded that the plasma jet near room temperature and atmospheric pressure was able to cause modifications in titanium surface

Deposição e distribuição de calda de pulverização em plantas de feijoeiro (Phaseolus vulgaris) e capim-braquiária (Brachiaria decumbens)

Com o objetivo de avaliar a deposição e distribuição de solução traçante em plantas de feijoeiro e capim-braquiária, foi conduzido experimento no NuPAM-FCA/ UNESP, campus de Botucatu-SP, utilizando um simulador de pulverização em ambiente controlado. Os tratamentos utilizados foram: bico jato plano XR Teejet (XR110.02VS) + surfactante Aterbane BR (0,5% v/v); bico jato cônico Conejet (TXVK-4) + surfactante Aterbane BR (0,5% v/v); bico jato plano XR Teejet (XR110.02VS); e bico jato cônico Conejet (TXVK-4). em todos os tratamentos foi aplicada uma solução de NaCl (0,5% p/v) + corante Poliglow laranja (0,5% p/v) + mancozeb (0,5% p/v). As unidades experimentais constituíram-se de vasos com duas plantas-alvo de capim-braquiária posicionadas sob uma planta-alvo de feijoeiro. A visualização da distribuição das gotas nas folhas de capim-braquiária foi efetuada com auxílio de luz negra, e o depósito da calda na superfície das plantas foi quantificado através da condutividade elétrica da solução aplicada e coletada por meio de lavagem de ambos os alvos. Os bicos de pulverização, jato plano (XR Teejet) e cônico (Conejet), não apresentaram diferença no depósito nos folíolos totais de feijoeiro quando submetidos a mesma condição de calda de pulverização. No entanto, o bico jato plano XR Teejet (XR110.02VS) e o bico jato cônico Conejet (TXVK-4) proporcionaram aumento de 67,1 e 61,5% na deposição da calda em relação a área foliar e 106,4 e 66,9% para matéria seca, respectivamente, em relação ao bico jato plano XR Teejet (XR110.02VS) + surfactante Aterbane BR (0,5% v/v) e ao bico jato cônico Conejet (TXVK-4) + surfactante Aterbane BR (0,5% v/v). Para o capim-braquiária, o bico cônico Conejet proporcionou deposição superior e distribuição mais uniforme em relação ao jato plano XR Teejet.

Depósitos de calda de pulverização nas faces adaxial e abaxial de folhas de Eichhornia crassipes dispostas em diferentes ângulos

Estudos foram conduzidos com o objetivo de avaliar os depósitos de gotas pulverizadas através de dois tipos de pontas sobre as faces adaxial e abaxial de folhas de Eichhornia crassipes dispostas em diferentes ângulos. No primeiro estudo, os tratamentos foram dispostos no esquema fatorial 2x4x7: dois tipos de pontas (TX12 e XR11002VS), quatro ângulos verticais (0º, 30º, 60º e 90º) e sete ângulos horizontais (0º, 15º, 30º, 45º, 60º, 75º e 90º). No ângulo vertical de 90º a lâmina foliar foi posicionada paralelamente ao sentido de deslocamento do jato de pulverização; e no ângulo horizontal de 90º a folha foi posicionada perpendicularmente ao plano do solo. Como traçadores, foram utilizadas soluções de 1.000 ppm do corante Azul FDC-1 e 3.500 ppm do corante Amarelo Tartrasina para as pontas tipo leque e cone, respectivamente. No segundo estudo, os tratamentos foram dispostos no esquema fatorial 2x2x3: dois tipos de pontas (TX12 e XR11002VS), dois tipos de calda (com e sem Aterbane BR a 0,5%) e três ângulos horizontais (0º, 45º e 90º). Adotou-se o ângulo vertical de 90º como padrão para todos os tratamentos. Soluções de 1.000 ppm do corante Azul FDC-1 e 3.500 ppm do corante Amarelo Tartrasina foram utilizadas como traçadores para a calda com e sem surfatante, respectivamente. Os resultados do primeiro estudo revelaram que os depósitos observados em toda a folha e na face adaxial das lâminas foliares de aguapé diminuíram à medida que se aumentou a angulação vertical, independentemente da ponta utilizada. Os menores depósitos sempre estiveram relacionados ao ângulo vertical de 90º, independentemente do ângulo horizontal utilizado. Não foi detectado nenhum depósito na face abaxial das folhas de aguapé em todas as combinações dos fatores estudados. No segundo estudo também foram observados os mesmos decréscimos no volume de calda depositado em toda a folha e na face adaxial à medida que se aumentou a angulação vertical das lâminas foliares. As duas pontas proporcionaram depósitos nulos na face abaxial quando o surfatante não foi utilizado; entretanto, a adição do surfatante à calda incrementou significativamente os depósitos nesta face da folha do aguapé.

Modelos analíticos para rádio fontes extragalácticas

The great majority of analytical models for extragalactic radio sources suppose self-similarity and can be classified into three types: I, II and III. We have developed a model that represents a generalization of most models found in the literature and showed that these three types are particular cases. The model assumes that the area of the head of the jet varies with the jet size according to a power law and the jet luminosity is a function of time. As it is usually done, the basic hypothesis is that there is an equilibrium between the pressure exerted both by the head of the jet and the cocoon walls and the ram pressure of the ambient medium. The equilibrium equations and energy conservation equation allow us to express the size and width of the source and the pressure in the cocoon as a power law and find the respective exponents. All these assumptions can be used to calculate the evolution of the source size, width and radio luminosity. This can then be compared with the observed width-size relation for radio lobes and the power-size (P-D) diagram of both compact (GPS and CSS) and extended sources from the 3CR catalogue. In this work we introduce two important improvement as compared with a previous work: (1)We have put together a larger sample of both compact and extended radio sources

Modelos auto-similares para rádio fontes extragalácticas.

This work is a detailed study of self-similar models for the expansion of extragalactic radio sources. A review is made of the definitions of AGN, the unified model is discussed and the main characteristics of double radio sources are examined. Three classification schemes are outlined and the self-similar models found in the literature are studied in detail. A self-similar model is proposed that represents a generalization of the models found in the literature. In this model, the area of the head of the jet varies with the size of the jet with a power law with an exponent γ. The atmosphere has a variable density that may or may not be spherically symmetric and it is taken into account the time variation of the cinematic luminosity of the jet according to a power law with an exponent h. It is possible to show that models Type I, II and III are particular cases of the general model and one also discusses the evolution of the sources radio luminosity. One compares the evolutionary curves of the general model with the particular cases and with the observational data in a P-D diagram. The results show that the model allows a better agreement with the observations depending on the appropriate choice of the model parameters.

Evolução de Rádio Fontes Duplas Extragalácticas

Double radio sources have been studied since the discovery of extragalactic radio sources in the decade of 1930. Since then, several numerical studies and analytical models have been proposed seeking a better understanding of the physical phenomena that determines the origin and evolution of such objects. In this thesis, we intended to study the evolution problem of the double radio sources in two fronts: in the ¯rst we have developed an analytical self-similar model that represents a generalization of most models found in the literature and solve some existent problems related to the jet head evolution. We deal with this problem using samples of hot spot sizes to ¯nd a power law relation between the jet head dimension and the source length. Using our model, we were able to draw the evolution curves of the double sources in a PD diagram for both compact sources (GPS and CSS) and extended sources of the 3CR catalogue. We have alson developed a computation tool that allows us to generate synthetic radio maps of the double sources. The objective is to determine the principal physical parameters of those objects by comparing synthetic and observed radio maps. In the second front, we used numeric simulations to study the interaction of the extra- galactic jets with the environment. We simulated situations where the jet propagates in a medium with high density contrast gas clouds capable to block the jet forward motion, forming the distorted structures observed in the morphology of real sources. We have also analyzed the situation in which the jet changes its propagation direction due to a change of the source main axis, creating the X-shaped sources. The comparison between our simulations and the real double radio sources, enable us to determine the values of the main physical parameters responsible for the distortions observed in those objects

Desenvolvimento e caracterização de dispositivos para reposição de filmes finos por descarga em cátodo oco

In the present work we use a plasma jet system with a hollow cathode to deposit thin TiO2 films on silicon substrates as alternative at sol-gel, PECVD, dip-coating e magnetron sputtering techniques. The cylindrical cathode, made from pure titanium, can be negatively polarized between 0 e 1200 V and supports an electrical current of up to 1 A. An Ar/O2 mixture, with a total flux of 20 sccm and an O2 percentage ranging between 0 and 30%, is passed through a cylindrical hole machined in the cathode. The plasma parameters and your influence on the properties of deposited TiO2 films and their deposition rate was studied. When discharge occurs, titanium atoms are sputtered/evaporated. They are transported by the jet and deposited on the Si substrates located on the substrate holder facing the plasma jet system at a distance ranging between10 and 50 mm from the cathode. The working pressure was 10-3 mbar and the deposition time was 10 -60 min. Deposited films were characterized by scanning electron microscopy and atomic force microscopy to check the film uniformity and morphology and by X-ray diffraction to analyze qualitatively the phases present. Also it is presented the new dispositive denominate ionizing cage, derived from the active screen plasma nitriding (ASPN), but based in hollow cathode effect, recently developed. In this process, the sample was involved in a cage, in which the cathodic potential was applied. The samples were placed on an insulator substrate holder, remaining in a floating potential, and then it was treated in reactive plasma in hollow cathode regime. Moreover, the edge effect was completely eliminated, since the plasma was formed on the cage and not directly onto the samples and uniformity layer was getting in all sampl

A combination of implicit and adaptative upwind tools for the numerical solution of incompressible free surface flows

This paper is concerned with the numerical solutions of time dependent two-dimensional incompressible flows. By using the primitive variables of velocity and pressure, the Navier-Stokes and mass conservation equations are solved by a semi-implicit finite difference projection method. A new bounded higher order upwind convection scheme is employed to deal with the non-linear (advective) terms. The procedure is an adaptation of the GENSMAC (J. Comput. Phys. 1994; 110: 171-186) methodology for calculating confined and free surface fluid flows at both low and high Reynolds numbers. The calculations were performed by using the 2D version of the Freeflow simulation system (J. Comp. Visual. Science 2000; 2:199-210). In order to demonstrate the capabilities of the numerical method, various test cases are presented. These are the fully developed flow in a channel, the flow over a backward facing step, the die-swell problem, the broken dam flow, and an impinging jet onto a flat plate. The numerical results compare favourably with the experimental data and the analytical solutions. Copyright (c) 2006 John Wiley & Sons, Ltd.

Evaluation of a bounded high order upwind scheme for 3D incompressible free surface flow computations

fit the context of normalized variable formulation (NVF) of Leonard and total variation diminishing (TVD) constraints of Harten. this paper presents an extension of it previous work by the authors for solving unsteady incompressible flow problems. The main contributions of the paper are threefold. First, it presents the results of the development and implementation of a bounded high order upwind adaptative QUICKEST scheme in the 3D robust code (Freeflow), for the numerical solution of the full incompressible Navier-Stokes equations. Second, it reports numerical simulation results for 1D hock tube problem, 2D impinging jet and 2D/3D broken clam flows. Furthermore, these results are compared with existing analytical and experimental data. and third, it presents the application of the numerical method for solving 3D free surface flow problems. (C) 2007 IMACS. Published by Elsevier B.V. All rights reserved,

Assessment of a high-order finite difference upwind scheme for the simulation of convection-diffusion problems

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

Studies on the cooling minimum quantity and conventional cooling at hardened steels in grinding process

The purpose of this work is to explain the concept of cutting fluids reasonable usage through the fluid minimum quantity in grinding processes. on that purpose, the development of a new nozzle and an own and adequate methodology should be required in order to obtain good results and compare them to the conventional methods. The analysis of the grinding wheel/cutting fluid performance was accomplished from the following input parameters: flow rate variation by nozzle diameter changes (three diameters values: 3mm, 4mm and 5mm), besides the conventional round nozzle already within the machine. Integral oil and a synthetic emulsion were used as cutting fluids and a conventional grinding wheel was employed. The workpieces were made of steel VC 131, tempered and quenched with 60HRc. Thus, as the flow rate and the nozzle diameter changes, keeping steady fluid jet velocity (equal to cutting velocity), attempted to find the best machining conditions, with the purpose to obtain a decrease on the cutting fluid volume, taking into consideration the analysis of the process output variables such as cutting strength, cutting specific energy, grinding wheel wear and surface roughness. It was verified that the 3mm diameter optimized nozzle and the integral oil, in general, was the best combination among all proposed.

Improving minimum quantity lubrication in CBN grinding using compressed air wheel cleaning

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

Cerâmicas avançadas no processo de retificação cilíndrica externa de mergulho utilizando a técnica da mínima quantidade de lubrificação (MQL) com rebolos diamantados

Nas últimas duas décadas, as cerâmicas avançadas têm sido exaustivamente utilizadas em aplicações na indústria devido às suas propriedades de elevada resistência ao desgaste e dureza. Entretanto, ainda se tem um alto custo agregado ao acabamento da peça. Esse acabamento geralmente é feito pelo processo de retificação, único processo economicamente viável que produz superfícies de elevada qualidade e precisão geométrica. Nesse contexto, as empresas vêm buscando a otimização no processo de retificação como, por exemplo, a redução do fluxo de fluido de corte utilizado, o que também visa atender exigências mundiais de preservação ambiental. Desta forma, este projeto pretendeu explorar a técnica da Mínima Quantidade de Lubrificação (MQL) na retificação cilíndrica externa de mergulho em cerâmicas com rebolos diamantados. Foram utilizados dois métodos de refrigeração: o convencional e o MQL, com três avanços de corte para cada caso. Foram usados um bocal convencional e um bocal para o MQL, tendo este um uniformizador de saída do jato. Foram analisadas como variáveis de saída: a emissão acústica, relação G, aspecto da superfície via microscopia eletrônica de varredura (MEV), rugosidade e circularidade. Assim, embora a refrigeração convencional ainda apresente os melhores resultados em comparação com a refrigeração com MQL, esta última pode atender os requisitos necessários para diversas aplicações, em especial quando utilizadas baixas espessuras equivalentes de corte (h eq). Além disso, a técnica de MQL possui a vantagem de gerar um menor impacto ambiental em comparação com a lubrificação convencional, devido ao uso mínimo de fluido de corte cujo descarte é cada vez mais regulamentado e custoso.