16 resultados para Metodologias de calibração

em Universidade Federal do Rio Grande do Norte(UFRN)


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In this work a pyrometer using the classic model of Kimball-Hobbs was developed, tested and calibrated. The solar radiation is verified through the temperature difference between the sensible elements covered by absorbing (black) and reflecting (white) pigmentations of the incoming radiation. The photoacoustic technique was used to optimize the choice of the pigments. Methodologies associated with linearity, thermo-variation, sensibility, response time and distance are also presented. To correctly classify the results, the international standard ISO 9060 as well as indicative parameters of World Meteorological Organization (WMO) are used. In addition a system of data acquisition of two channels with 12 bits, constructed during the this time, was used to measure the global solar radiation on the ground by the pyrometer and also by another pyrometer certified in the case of Keep & zonen. The results statistically show, through the hypothesis test presented here, that both equipments find population average with 95% of correctness

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PAHs (Polycyclic Aromatic Hydrocarbons) are a group of organic substances which receive considerable attention because of the carcinogenic and mutagenic properties of some of them. It is therefore important to determine the PAHs in different environmental matrices. Several studies have shown the use of gas chromatography coupled to mass spectrometry as a technique for quantification of PAHs by presenting excellent detection limits. This study aimed to develop an analytical methodology for the determination of 16 PAHs listed by the USEPA, test two methods for extraction of PAHs in water from a 23 factorial design, quantify them through the analytical technique coupled to gas chromatography mass spectrometry (GC/MS) using the method developed, and finally apply the results in chemometrics. The sample was synthesized and subjected to tests of the 23 factorial design, which has the factors: the type of extraction technique (ultrasound and digester), the ratio solvent / sample (1:1 and 1:3) and the type of solvent (dichloromethane / hexane and acetone / dichloromethane). The responses of eight combinations of the factorial design were obtained from the quantification by external calibration in GC/MS. The quantification method was developed from an optimized adaptation of the USEPA Method 8270. We used the full scan mode as a way of acquiring the mass spectra of 16 PAHs. The time in which the samples were subjected to ultrasound was fixed at 10 min and held an investigation to establish the conditions of power and time in the digester. We had the best response in the investigation of the digester power of 100 watts and the time of six minutes. The factorial design of liquid-liquid extraction showed that the most representative factors were: the use of the digester as extraction technique, the ratio solvent / sample 1:1 and the use of a 1:1 mixture of dichloromethane / hexane as a solvent more suitable. These results showed that the 1:1 mixture of dichloromethane / hexane is an excellent mixture to recover the extraction of PAHs an aqueous sample using the microwave digester. The optimization of the method of separation, identification and quantification of PAHs in the GC/MS was valid for 16 PAHs present in each chromatogram of the samples

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Instrumentation is a tool of fundamental importance for research in several areas of human knowledge. Research projects are often unfeasible when data cannot be obtained due to lack of instruments, especially due to impor ting difficulties and the high costs there associated. Thus, in order to collaborate with the enhancement of a national technology, a multiband hand - held sun p hotometer (FSM - 4) was developed to operate in the 500 nm, 670 nm, 870 nm and 940 nm bands. In the 500 nm, 670 nm and 870 nm bands aerosols are monitored for evaluation of the AOD (Aerosol Optical Depth), and the PWC (Precipitable Water Column) is evaluated in the 940 nm band. For the development of the mech anical and electronic parts for the FSM - 4, th e materials and componen ts should combine low cost and quality of the data collected. The calibration process utilized the Langley method (ML) and Modified Langley Method (MLM). These methods are usually applied at high altitudes in order to provide atmosp heric optical stability. This condition however can be found in low height sites as shown in the research by Liu et al. (2010). Thus, for calibration of the FSM - 4, we investigated the atmospher ic optical stability utilizing the ML and MLM at a site in the cit y of Caicó / RN, located in the s emiarid region in northeastern Brazil. This site lies in a region far aw ay from large urban centers and activities generating anthropogenic atmospheric pollution. Data for calibration of the prototype were collected usin g the FSM - 4 in two separate operations during the dry season, one in December 2012 and another in September 2013. The methodologies showed optical atmospheric instability in the studied region through the dispersion of the values obtained for the calibrati on constant. This dispersion is affected by the variability of AOD and PWC during the appl ication of the above mentioned methods . As an alternative to the descr ibed sun photometer calibration , a short study was performed using the sun photometer worldwide network AERONET/NASA (AERsol RObotic NETwork – US Space Agency), installed in Petrolina / PE in Brazil. Data were collected for three days utilizing the AERONET instruments and the FSM - 4, operating simultaneously on the same site. By way of the ML and MLM techniques, convergent test values were obtained for the calibration constants, despite the low amount of data collected. This calibration transfer methodology proved to be a viable alternative to the FSM - 4 calibration .

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Due to the appreciation of family farming by the Brazilian Federal Government, the Technical Assistance and Rural Extension was induced to restructure and act in a more participative way, culminating in the National Policy of Technical Assistance and Rural Extension (PNATER), changing the profile of technology transfer and knowledge (diffusionism) for an action that uses participatory methodologies focused on exchange of knowledge between farmers and technicians. The process of discussion of the trends of ATER brought the New ATER , with the recognition of agroecology as the main guidance. This research aimed to analyze methods of public ATER developed by institutions of Rio Grande do Norte, under the guidance of New ATER. The research is qualitative. Secondary data were collected through documental research and literature. Primary data were collected through a set of interviews applied to representatives of public institutions ATER, namely EMATER-RN, Diaconia and AACC and representatives of organizations that receive public ATER. The research showed the difficulties of EMATER-RN in implementing of New ATER due to lack of infrastructure and low adherence of the new form of technical assistance and rural extension. It was shown also that the AACC and Diaconia act with ATER through projects with implementation deadlines set, often interrupting ATER while communities are still in need of assistance

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Produced water is characterized as one of the most common wastes generated during exploration and production of oil. This work aims to develop methodologies based on comparative statistical processes of hydrogeochemical analysis of production zones in order to minimize types of high-cost interventions to perform identification test fluids - TIF. For the study, 27 samples were collected from five different production zones were measured a total of 50 chemical species. After the chemical analysis was applied the statistical data, using the R Statistical Software, version 2.11.1. Statistical analysis was performed in three steps. In the first stage, the objective was to investigate the behavior of chemical species under study in each area of production through the descriptive graphical analysis. The second step was to identify a function that classify production zones from each sample, using discriminant analysis. In the training stage, the rate of correct classification function of discriminant analysis was 85.19%. The next stage of processing of the data used for Principal Component Analysis, by reducing the number of variables obtained from the linear combination of chemical species, try to improve the discriminant function obtained in the second stage and increase the discrimination power of the data, but the result was not satisfactory. In Profile Analysis curves were obtained for each production area, based on the characteristics of the chemical species present in each zone. With this study it was possible to develop a method using hydrochemistry and statistical analysis that can be used to distinguish the water produced in mature fields of oil, so that it is possible to identify the zone of production that is contributing to the excessive elevation of the water volume.

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Since the beginning of the National Program for Production and Use of Biodiesel in Brazil, in 2004, different raw materials were evaluated for biodiesel production, trying to combine the agricultural diversity of the country to the desire to reduce production coasts. To determine the chemical composition of biodiesel produced from common vegetables oils, international methods have been used widely in Brazil. However, for analyzing biodiesel samples produced from some alternative raw materials analytical problems have been detected. That was the case of biodiesel from castor oil. Due the need to overcome these problems, new methodologies were developed using different chromatographic columns, standards and quantitative methods. The priority was simplifying the equipment configuration, realizing faster analyses, reducing the costs and facilitating the routine of biodiesel research and production laboratories. For quantifying free glycerin, the ethylene glycol was used in instead of 1,2,4-butanetriol, without loss of quality results. The ethylene glycol is a cheaper and easier standard. For methanol analyses the headspace was not used and the cost of the equipment used was lower. A detailed determination of the esters helped the deeper knowledge of the biodiesel composition. The report of the experiments and conclusions of the research that resulted in the development of alternative methods for quality control of the composition of the biodiesel produced in Brazil, a country with considerable variability of species in agriculture, are the goals of this thesis and are reported in the following pages

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Successive curricular changes that occurred in professional education altered pedagogical practices, and these practices being developed by means of integrating projects, at Centro Federal de Educação Tecnológica de Sergipe (CEFET-SE), between 2001 and 2003, originated some questions which became the study object of this thesis. We search for theoretical support mainly in GEPEM research (GEPEM/UFRN) works and practices in order to analyze elements that emerged from this pedagogical practice. To do so, we take as main reference the research of qualitative approach. We developed documents analysis, interviews, considering three aspects: the scenery where these changes took place, the conception and implementation of the Integrating Projects for what, we ask support in pedagogy of projects studies and principles of interdisciplinary, and contextualization as curriculum structuring elements. This research brought out some difficulties, conflicts and possible consensus in developing the methodological strategies for the Projects. In this process of coexistence of the traditional and the new, of an unavoidable distance between what was thought and what was effectively done, elements for a new pedagogical practice emerged. This could be noticed in terms of participative work, formative moments, teacher s autonomy related to the pedagogical work. A new door could be open to the possibilities of taking conscience of accepting the differences and oneself autoexperimentation. These are the possibilities that make men, not being mere information deposit, can dialog and transform, producing his existence by this means. In the present case, the existence of being teacher, the build himself in the time of possibilities

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In Brazil the theme quality in public construction has been widely discussed in the early 1990s, with the creation of the Brazilian Program of Quality and Productivity for the Habitat (PBQP-H) which is strongly influenced by the wave of studies on issues of quality in the world, such as the ISO 9000. Over the years, other approaches have emerged and been consolidated, evolving from market and customer´s needs. An example is the Six Sigma methodology. This study aims to examine the Six Sigma, ISO 9000 and PBQP-H methodologies, noting the common elements, differences, gaps and how the methods are complementary, so that with the ongoing work, proposed initiatives can be developed to improve the quality that enables its application in public construction. Still aiming to optimize the deployment of the proposed initiatives, it was performed an analysis of ISO 9001 and PBPQ-H certifications in Brazil and in the state of Rio Grande do Norte, with respect to the construction industry and a case study to identify the factors that influence the adoption of initiatives to improve quality, and check if the selected construction company is prepared to implement the proposed initiatives. This research is characterized as exploratory and applied, with literature review and a case study. The data collection instrument was a questionnaire and the statistical analysis used a multidimensional scaling method. The conclusion is that the methodologies are compatible and complementary, and their integration could potentialize the goals set. It was identified that the state of Rio Grande do Norte has a few number of certifications in construction. Nine initiatives are proposed for implementation at construction companies. In the case study it was found that the studied company would be able to implement the suggestions proposed and the requirement for certification by clients and funding institutions influence the adoption of quality improvement initiatives. This result confirms the literature which states that top management support is crucial for the successful implementation of quality methodologies

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The exponential growth in the applications of radio frequency (RF) is accompanied by great challenges as more efficient use of spectrum as in the design of new architectures for multi-standard receivers or software defined radio (SDR) . The key challenge in designing architecture of the software defined radio is the implementation of a wide-band receiver, reconfigurable, low cost, low power consumption, higher level of integration and flexibility. As a new solution of SDR design, a direct demodulator architecture, based on fiveport technology, or multi-port demodulator, has been proposed. However, the use of the five-port as a direct-conversion receiver requires an I/Q calibration (or regeneration) procedure in order to generate the in-phase (I) and quadrature (Q) components of the transmitted baseband signal. In this work, we propose to evaluate the performance of a blind calibration technique without additional knowledge about training or pilot sequences of the transmitted signal based on independent component analysis for the regeneration of I/Q five-port downconversion, by exploiting the information on the statistical properties of the three output signals

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The continuous development of instruments and equipment used as tools or torque measurement in the industry is demanding more accurate techniques in the use of this kind instrumentation, including development of metrological characteristics in torque measurement. The same happens with the needs in calibration services. There is a diversity of methods of hand torque tools in the market with different measuring range but without complaining with technical standards in terms of requirements of quality and reliability. However, actually there is no choice of a torque measuring standard that fulfils, with low cost, the needs for the calibration of hand torque tools in a large number of ranges. The objective of this thesis is to show the development and evaluation of a torque measuring standard device with a conception to allow the calibration of hand torque tools with three levels of torque with an single instrument, promoting reduction of costs and time in the calibration, also offering reliability for the evaluation of torque measuring instrument. To attend the demand in the calibration of hand torque tools it is necessary that the calibration laboratories have a big collection of torque measuring standards, to fulfills the needs of the costumer, what is very costly. The development of this type of torque measuring standard revealed a viable technique and economically making possible the calibration of hand torque tools in different nominal ranges through a single measurement system versatile, efficient and of easy operation

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This work is combined with the potential of the technique of near infrared spectroscopy - NIR and chemometrics order to determine the content of diclofenac tablets, without destruction of the sample, to which was used as the reference method, ultraviolet spectroscopy, which is one of the official methods. In the construction of multivariate calibration models has been studied several types of pre-processing of NIR spectral data, such as scatter correction, first derivative. The regression method used in the construction of calibration models is the PLS (partial least squares) using NIR spectroscopic data of a set of 90 tablets were divided into two sets (calibration and prediction). 54 were used in the calibration samples and the prediction was used 36, since the calibration method used was crossvalidation method (full cross-validation) that eliminates the need for a validation set. The evaluation of the models was done by observing the values of correlation coefficient R 2 and RMSEC mean square error (calibration error) and RMSEP (forecast error). As the forecast values estimated for the remaining 36 samples, which the results were consistent with the values obtained by UV spectroscopy

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In this work, the quantitative analysis of glucose, triglycerides and cholesterol (total and HDL) in both rat and human blood plasma was performed without any kind of pretreatment of samples, by using near infrared spectroscopy (NIR) combined with multivariate methods. For this purpose, different techniques and algorithms used to pre-process data, to select variables and to build multivariate regression models were compared between each other, such as partial least squares regression (PLS), non linear regression by artificial neural networks, interval partial least squares regression (iPLS), genetic algorithm (GA), successive projections algorithm (SPA), amongst others. Related to the determinations of rat blood plasma samples, the variables selection algorithms showed satisfactory results both for the correlation coefficients (R²) and for the values of root mean square error of prediction (RMSEP) for the three analytes, especially for triglycerides and cholesterol-HDL. The RMSEP values for glucose, triglycerides and cholesterol-HDL obtained through the best PLS model were 6.08, 16.07 e 2.03 mg dL-1, respectively. In the other case, for the determinations in human blood plasma, the predictions obtained by the PLS models provided unsatisfactory results with non linear tendency and presence of bias. Then, the ANN regression was applied as an alternative to PLS, considering its ability of modeling data from non linear systems. The root mean square error of monitoring (RMSEM) for glucose, triglycerides and total cholesterol, for the best ANN models, were 13.20, 10.31 e 12.35 mg dL-1, respectively. Statistical tests (F and t) suggest that NIR spectroscopy combined with multivariate regression methods (PLS and ANN) are capable to quantify the analytes (glucose, triglycerides and cholesterol) even when they are present in highly complex biological fluids, such as blood plasma

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This work aims to detect polycyclic aromatic hydrocarbons (PAHs) through optimized analytical techniques, such as gas chromatography with flame-ionisation detector (CGFID), gas chromatography coupled to mass spectrometry (CGMS), Fluorescence Spectroscopy of Molecular and Purpot of oils and greases (POG). Apply to chemometrics, Factorial Planning 23, in the preparation of samples by liquid-liquid extraction. The sample preparation was used for liquid-liquid extraction and factors in this sample was used for the application of factorial planning 23, such as the use of ultrasound, solvents (dichloromethane, hexane and chloroform) and ratio of solvent / synthetic sample. These factors were assigned two types of levels: positive and negative. It was used to form the cube to better analyze the answers. The responses of the eight combinations were obtained in reading the spectrofluorimetric. The optimization of equipment were used, and they served in the HPA's identification of the samples collected in Rio Potengi. The optimization of the equipment was observed every 16's and PAH in the samples was found that the HPA's came from contamination of the Rio Potengi. The contamination comes through organic household waste, hospital waste, and among other contamination that comes from industries that are installed around the River The factorial design of high validity, it was observed a more effective sample preparation. The factorial design of liquid-liquid extraction showed a way to spend less solvent in less time using an ideal solvent, but also a way to extract more analyte from the matrix itself is water. In planning a smaller form factor extraction was the use of ultrasound, the ratio 1:3 corresponding to a solvent and sample 3 and the best solvent was dichloromethane who presented a viable extraction, not discarding the possibility of using also the hexane. The chloroform and may be toxic not had a good extraction

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Due to the appreciation of family farming by the Brazilian Federal Government, the Technical Assistance and Rural Extension was induced to restructure and act in a more participative way, culminating in the National Policy of Technical Assistance and Rural Extension (PNATER), changing the profile of technology transfer and knowledge (diffusionism) for an action that uses participatory methodologies focused on exchange of knowledge between farmers and technicians. The process of discussion of the trends of ATER brought the New ATER , with the recognition of agroecology as the main guidance. This research aimed to analyze methods of public ATER developed by institutions of Rio Grande do Norte, under the guidance of New ATER. The research is qualitative. Secondary data were collected through documental research and literature. Primary data were collected through a set of interviews applied to representatives of public institutions ATER, namely EMATER-RN, Diaconia and AACC and representatives of organizations that receive public ATER. The research showed the difficulties of EMATER-RN in implementing of New ATER due to lack of infrastructure and low adherence of the new form of technical assistance and rural extension. It was shown also that the AACC and Diaconia act with ATER through projects with implementation deadlines set, often interrupting ATER while communities are still in need of assistance

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Produced water is characterized as one of the most common wastes generated during exploration and production of oil. This work aims to develop methodologies based on comparative statistical processes of hydrogeochemical analysis of production zones in order to minimize types of high-cost interventions to perform identification test fluids - TIF. For the study, 27 samples were collected from five different production zones were measured a total of 50 chemical species. After the chemical analysis was applied the statistical data, using the R Statistical Software, version 2.11.1. Statistical analysis was performed in three steps. In the first stage, the objective was to investigate the behavior of chemical species under study in each area of production through the descriptive graphical analysis. The second step was to identify a function that classify production zones from each sample, using discriminant analysis. In the training stage, the rate of correct classification function of discriminant analysis was 85.19%. The next stage of processing of the data used for Principal Component Analysis, by reducing the number of variables obtained from the linear combination of chemical species, try to improve the discriminant function obtained in the second stage and increase the discrimination power of the data, but the result was not satisfactory. In Profile Analysis curves were obtained for each production area, based on the characteristics of the chemical species present in each zone. With this study it was possible to develop a method using hydrochemistry and statistical analysis that can be used to distinguish the water produced in mature fields of oil, so that it is possible to identify the zone of production that is contributing to the excessive elevation of the water volume.