9 resultados para Reproducibility

em Universidade Federal do Rio Grande do Norte(UFRN)


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Investigations in the field of pharmaceutical analysis and quality control of medicines require analytical procedures with good perfomance characteristics. Calibration is one of the most important steps in chemical analysis, presenting direct relation to parameters such as linearity. This work consisted in the development of a new methodology to obtain calibration curves for drug analysis: the stationary cuvette one. It was compared to the currently used methodology, and possible sources of variation between them were evaluated. The results demonstrated that the proposed technique presented similar reproducibility compared to the traditional methodology. In addition to that, some advantages were observed, such as user-friendliness, cost-effectiveness, accuracy, precision and robustness. Therefore, the stationary cuvette methodology may be considered the best choice to obtain calibration curves for drug analyis by spectrophotometry

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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

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Considering the constant evolution of technology in growth and the need for production techniques in the ceramics area to move forward together, we sought in this study, the research and development of polymeric precursor method to obtain inorganic ceramic pigments. Method that provides quality to obtain the precursor powders of oxides and pigments at the same time, offers time and cost advantages, such as reproducibility, purity and low temperature heat treatment, control of stoichiometry. This work used chromium nitrate and iron nitrate as precursors. The synthesis is based on the dissolution of citric acid as a complexing agent, addition of metal oxides, such as ion chromophores; polymerization with ethylene glycol and doping with titanium oxide. Passing through precalcination, breakdown, thermal treatments at different temperatures of calcination (700 to 1100 oC), resulting in pigments: green for chromium oxide deposited on TiO2 (CrTiO3) and orange for iron oxide deposited on TiO2 ( FeTiO3). Noticing an increase of opacity with increasing temperature. Were performed thermal analysis (TG and ATD) in order to evaluate its thermodecomposition. The powders were also characterized by techniques such as XRD, revealing the formation of crystalline phases such as iron titanate (FeTiO3) and chrome titanate (CrTiO3), SEM, demonstrating formation of rounded particles for both oxides and Spectroscopy in the UV-Visible Region, verifying the potential variation and chromaticity os pigments. Thus, the synthesized oxides were within the requirements to be applied as pigments and shown to be possible to propose its use in ceramic materials

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The Wii Balance Board (WBB) began to be investigated as a low-cost alternative for assessing static balance in vertical posture. However, studies employed methodological procedures that did not eliminate result variability between the tests and equipment used. Objective: Determine the validity and reproducibility of the WBB as an instrument for assessing static balance in the vertical position, using simultaneous data analysis and superimposed equipment. Methods: This is an accuracy study of 29 healthy young individuals of both sexes aged 18 to 30 years. Subjects were assessed 24h apart (test-retest), using unipodal and bipodal support tests, with eyes closed and open. To that end the WBB was placed on top of a force platform (FP) and data (postural sway) were collected simultaneously on both devices. Validity and reproducibility were analyzed using the interclass correlation coefficient (ICC). Finally, Bland-Altman analysis was applied to assess agreement. Results: The sample was composed of 23 women and 6 men, with mean age of 24.2±6.3 years, 60.7±6.3 kg and 1.64±4.2 m. The validity of the WBB compared to the FP was excellent for all 4 tasks proposed (ICC = 0.93 0.98). The reproducibility analyzed by test-retest was excellent for the bipodal support tasks (ICC = 0.93-0.98) and only moderate for the unipodal support tests (ICC = 0.46 0.70). Graphic analysis exhibited good agreement between the devices, since most of the measures were within the limits of agreement. Conclusion: this study proved the validity and reproducibility of the Wii Balance Board as an instrument for assessing static balance in vertical posture, using simultaneous analysis with superimposed equipment. Thus, the WBB has been increasingly used by physical therapists and other health professionals in their clinical practice, as both a rehabilitation and assessment tool

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Currently, several psychological and non-psychological tests can be found in publishes without standardization on procedures set in different psychological areas, like intelligence, emotional states, attitudes, social skills, vocation, preferences and others. The computerized psychological testing is a extension of traditional testing psychological practices. However, it has own psychometrics qualities, either by its matching in a computerized environment or by the extension that can be developed in it. The current research, developed from a necessity to study process of validity and reliability on a computerized test, drew a methodological structure to provide parallel applications in numerous kinds of operational groups, evaluating the influences of the time and approach in the computerization process. This validity refers to normative values groups, reproducibility in computerized applications process and data processing. Not every psychological test can be computerized. Therefore, our need to find a good test, with quality and plausible properties to transform in computerized application, leaded us to use The Millon Personality Inventory, created by Theodore Millon. This Inventory assesses personality according to 12 bipolarities distributed in 24 factors, distributed in categories motivational styles, cognitive targets and interpersonal relations. This instrument doesn t diagnose pathological features, but test normal and non adaptive aspects in human personality, comparing with Theodore Millon theory of personality. In oder to support this research in a Brazilian context in psychological testing, we discuss the theme, evaluating the advantages and disadvantages of such practices. Also we discuss the current forms in computerization of psychological testing and the main specific criteria in this psychometric specialized area of knowledge. The test was on-line, hosted in the site http://www.planetapsi.com, during the years of 2007 and 2008, which was available a questionnaire to describe social characteristics before test. A report was generated from the data entry of each user. An application of this test was conducted in a linear way through a national coverage in all Brazil regions, getting 1508 applications. Were organized nine groups, reaching 180 applications in test and retest subject, where three periods of time and three forms of retests for studies of on-line tests were separated. Parallel to this, we organized multi-application session offline group, 20 subjects who received tests by email. The subjects of this study were generally distributed by the five Brazilian regions, and were noticed about the test via the Internet. The performance application in traditional and on-line tested groups subsidies us to conclude that on-line application provides significantly consistency in all criteria for validity studied and justifies its use. The on-line test results were related not only among themselves but were similar to those data of tests done on pencil and paper (0,82). The retests results demonstrated correlation, between 0,92 and, 1 while multisessions had a good correlation in these comparisons. Moreover, were assessed the adequacy of operational criteria used, such as security, the performance of users, the environmental characteristics, the organization of the database, operational costs and limitations in this on-line inventory. In all these five items, there were excellent performances, concluding, also, that it s possible a self-applied psychometric test. The results of this work are a guide to question and establish of methodologies studies for computerization psychological testing software in the country

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This study aimed to apply, thermogravimetriy /derivative Thermogravimetriy (TG/DTG), differential scanning calorimetry (DSC), Differential Thermal Analysis (DTA), to conduct a comparative study on drug reference, generic and whose active principles are similar captopril hydrochlorothiazide, ampicillin, paracetamol, aspirin and mebendazole sold in local pharmacies. Samples of the active ingredients and dosage forms were also characterized by absorption infrared spectroscopy (IR), X-ray diffraction (XRD) and microscopy scanning electron (SEM). The TG / DTG curves showed a general similarity in the thermal behavior of the samples, but also showed the influence of excipients on the thermal stability. The DSC curve of the generic base hydrochlorothiazide showed no peak on the fusion of the drug due to interference of lactose as a diluent, which causes interaction with the active principle causing their degradation before the merger. The DSC curves of the drugs consisting of paracetamol showed reproducibility at the melting point of the active and the other thermal events. The DSC result of binary mixtures involving captopril / magnesium stearate and mebendazole/magnesium stearate showed possible interactions or incompatibilities evidenced by the displacement of the melting point of both drugs. The other mixtures showed no change. The infrared spectra presented were very similar, indicating the presence of functional groups characteristic of the constituents of the samples. The X-ray diffraction showed peaks indicative of crystalline structure of the active ingredients as well as some of the ingredients in the formulation of the drug and the micrographs indicate a general heterogeneity in the size distribution of particles in the samples

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In this work a biodegradable composite using the carnauba straw s powder as reinforcement on chitosan matrix polymeric were manufactured. Firstly, were carried out the chemistry characterization of the carnauba straw s powder before and after treatments with NaOH and hexane. Goering and Van Soest method (1970), flotation test, moisture absorption, FTIR, TG/DTG, DSC and SEM have also being carried out. Composites were developed with variations in granulometry and in powder concentrations. They were characterized by TG/DTG, SEM and mechanicals properties. The results of chemical composition showed that the carnauba straw s powder is composed of 41% of cellulose; 28,9% of hemicellulose and 14% of lignin.The flotation test have indicated that the chemical treatment with NaOH decreased the powder s hidrophilicity.The thermal analysis showed increased of thermal stability of material after treatments. The results of FTIR and SEM revealed the removal of soluble materials from the powder (hemicelluloses and lignin), the material became rougher and clean. The composites obtained showed that the mechanicals properties of the composites were decreased in respect at chitosan films, and the composites with the powder at 150 Mesh showed less variation in the modulus values. The speed test of 10 mm/min showed the better reproducibility of the results and is in agreement to the standard ASTM D638. The SEM analysis of fracture showed the low adhesion between the fiber/matrix. The increase of volume of powder in the composite caused a decrease in values of stress and strain for the samples with untreated powder and treated with hexane. The composite with 50% of the powder s treated in NaOH didn t have significant variation in the values of stress and strain as compared with the composites with 10% of the powder, showing that the increase in the volume of fiber didn t affect the stress and strain of the composite. Thereby, it is concluded that the manufacture of polymeric composites of chitosan using carnauba straw s powder can be done, without need for pre-treatment of reinforcement, become the couple of carnauba straw s powder-chitosan a good alternative for biodegradable composites

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Two pillaring methods were tested to synthesize pillared clays containing mixed Al/Co pillars. Using the first method, based on the traditional procedure, were obtained materials containing different Co concentrations: 10, 25, 50, 75 and 100 % of Co in the pillaring solution. Just the experiments with low concentrations (10 and 25 % of Co) has formed pillared clays, whereas the sample with 25 % of cobalt showed best results compared with the one obtained just using Al as pillaring agent (basal spacing higher than 18 Å and surface area bigger than 300 m²/g). The 27Al NMR results pointed out the formation of mixed Al/Co pillars due to decreased between the intensities of AlVI/AlIV signals, indicating that the AlIV content decreased while Co content increased, suggesting the isomorphic substitution of Al atoms for Co in the Keggin ion structure (pillaring agent). For the samples containing 75 and 100 % of cobalt, it was verified the formation of others materials, which could be identified as hydrotalcite like compounds. The second pillarization method was named mixed layers, because the objective was to intercalate clay layers with hydrotalcite layers. Thus, after calcination, the hydrotalcite layers would dehydroxylate, resulting just in the metals oxides, intercalated between the clay sheets, thus generating, a pillared clay. For this purpose, were tested 4 synthesis procedures: physical mixture, mixture in water, ionic exchange under reflux and in situ synthesis. Of these, the method which showed the best results was the in situ synthesis, in which basal spacings of 14 Å (after calcination) were obtained, indicating that the samples are intercalated with metal oxides (Mg and Al). This procedure was reproduced with a Co-Al LDH (layered double hydroxide) and similar results were obtained, testifying the method reproducibility

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The processing of heavy oil produced in Brazil is an emergency action and a strategic plan to obtain self-sufficiency and economic surpluses. Seen in these terms, it is indispensable to invest in research to obtain new catalysts for obtaining light fraction of hydrocarbons from heavy fractions of petroleum. This dissertation for the degree of Doctor of Philosophy reports the materials preparation that combine the high catalytic activity of zeolites with the greater accessibility of the mesoporosity, more particularly the HZSM-5/MCM-41 hybrid, done by synthesis processes with less environmental impact than conventional ones. Innovative methodologies were developed for the synthesis of micro-mesoporous hybrid material by dual templating mechanism and from crystalline zeolitic aluminosilicate in the absence of organic template. The synthesis of hybrid with pore bimodal distribution took place from one-single organic directing agent aimed to eliminate the use of organic templates, acids of any kind or organic solvents like templating agent of crystalline zeolitic aluminosilicate together with temperature-programmed microwave-assisted, making the experimental procedures of preparation most practical and easy, with good reproducibility and low cost. The study about crystalline zeolitic aluminosilicate in the absence of organic template, especially MFI type, is based on use of H2O and Na+ cation playing a structural directing role in place of an organic template. Advanced characterization techniques such as X-Ray Diffraction (XRD), Fourier Transform Infrared Spectroscopy (FTIR), Scanning Electron Microscopy (SEM), Highresolution Transmission Electron Microscopy (HRTEM), Adsorption of N2 and CO2, kinetic studies by Thermogravimetric Analysis (TGA) and Pyrolysis coupled to Gas Chromatography/Mass Spectrometry (Pyrolysis-GC/MS) were employed in order to evaluate the synthesized materials. Achieve the proposed objectives, has made available a set of new methodologies for the synthesis of zeolite and hybrid micro-mesoporous material, these suitable for catalytic pyrolysis of heavy oils aimed at producing light fraction