Determinação de misturas de sulfametoxazol e trimetoprima por espectroscopia eletrônica multivariada

In this work a multivariate spectroscopic methodology is proposed for quantitative determination of sulfamethoxazole and trimethoprim in pharmaceutical associations. The multivariate model was developed by partial least-squares regression, using twenty synthetic mixtures and the spectral region between 190 and 350 nm. In the validation stage, which involved the analysis of five synthetic mixtures, prediction errors lower that 3% were observed. The predictive capacity of the multivariate models is seriously affected by spectral changes induced by pH variations, a fact that acquires a great significance in the analysis of real samples (pharmaceuticals) that contain chemical additives.

Estudo da decomposição térmica de propelente sólido compósito de baixa emissão de fumaça

The thermal decomposition of hydroxyl-terminated polybutadiene (HTPB)/ammonium nitrate (AN) based propellants, so called smokeless formulations, and raw materials were investigated by differential scanning calorimetry (DSC) and thermogravimetry (TG). The thermoanalytical profile of different components and of propellant were evaluated and the Arrhenius parameters for the thermal decomposition of the propellant sample were determined by the Ozawa method. The kinetic parameters of the thermal decomposition of propellant samples were determined by DSC measurements. The values obtained for activation energy (Ea) and pre-exponential factor were 163 kJ mol-1 and 1.94x10(6) min-1.

Metodologia analítica para quantificar o teor de biodiesel na mistura biodiesel: diesel utilizando espectroscopia na região do infravermelho

Considered the best substitute for diesel, biodiesel can be blended with diesel in any ratio, bringing lots of environmental, economic and social advantages. Brazilian law Nº 11097/2005, proposes the introduction of biodiesel in to the Brazilian energy matrix, mixed with diesel at a minimum percentage of 2%. For consumers and sellers to be sure that the commercialized mixture of biodiesel:diesel contains the correct percentage, it is necessary to develop analytical methodologies to quantify the amount of biodiesel added. This work presents a fast, low-cost and simple methodology to determine the biodiesel proportion in mixtures of biodiesel:diesel, based on infrared spectroscopy.

Determinação não destrutiva do nitrogênio total em plantas por espectroscopia de reflectância difusa no infravermelho próximo

Diffuse reflectance near-infrared (DR-NIR) spectroscopy associated with partial least squares (PLS) multivariate calibration is proposed for a direct, non-destructive, determination of total nitrogen in wheat leaves. The procedure was developed for an Analytical Instrumental Analysis course, carried out at the Institute of Chemistry of the State University of Campinas. The DR-NIR results are in good agreement with those obtained by the Kjeldhal standard procedure, with a relative error of less than ± 3% and the method may be used for teaching purposes as well as for routine analysis.

Aplicacions de la fibra òptica a la monitorització d'estructures

Davant la gran necessitat que es té per reduir al mínim els costs relacionats amb el manteniment, prevenció i seguretat, la monitorització en el camp de les estructures civils és una activitat que ha anat adquirint un paper cada cop més important. Dins el camp de l’enginyeria civil, la instrumentació d’estructures d’edificació i obra civil ha experimentat una profunda expansió. Les aplicacions més habituals en aquest tipus d’ activitat, solen estar associades a l’avaluació d’esforços en estructures existents, i/o el seguiment de l’estat tenso-deformacional durant el procés de construcció. Hi ha una gran diversitat de dispositius de mesura que permeten realitzar aquest seguiment. Els sistemes basats en la tecnologia de fibra òptica ja ho permeten. La resistència a la corrosió i a la fatiga, la immunitat a les interferències electromagnètiques o la possibilitat de prendre mesures discretes al llarg del temps, podent referir-les en tot moment a l’origen, són alguns dels seus avantatges. Tot i els múltiples avantatges, aquest sistema també té els seus inconvenients. En tota seguretat el més important és l’influencia de la temperatura en els valors mesurats. El projecte es centre en aquest últim punt , concretament en les mesures de deformació. Els objectius que s’han dut a terme al llarg de la durada del treball han estat els següents: - Aprendre les bases teòriques d’aquesta tecnologia. - Determinar en quin grau, la temperatura afecta a les mesures adquirides mitjançant sensors de fibra òptica. - Establir els mecanismes adients per quantificar, corregir o minimitzar aquests efectes. - Comparar la fiabilitat d’aquest tipus de mesura respecte a la dels sensors basats en extensometria

Efeito do 1-metilciclopropeno sobre a emissão dos ésteres voláteis de bananas ao longo do amadurecimento

Fresh green bananas (Musa sp., subgroup Prata) were treated with a dose of only 90 ηg g-1 of 1-MCP for 13 hours and the evolution of the volatile compounds along the ripeness was studied. A method to quantify the emission of esters was developed by cryogenic headspace and gas chromatography. Esters of acetate, butyrate, isobutyrate and isovalerate were found as major compounds. The application of the 1-MCP for 13 hours delayed the appearance of the coloration 8 of the peel for 3 days and decreased quantitatively in about 46% the total production of esters in the banana until the 15° day of harvested.

Espectroscopia Mössbauer na caracterização de compostos ferrosos em solos e sua relação com retenção de fósforo

The chemical role of iron-bearing compounds on the dynamics of phosphorus in selected Brazilian latosols was investigated. The iron oxides were characterized in an attempt to assess their main chemical-mineralogical properties influencing the ion sorption mechanisms in those pedosystems. It was found that increasing total iron contents tend to increase the phosphorus adsorption capacity in the selected soils. 110 K-Mössbauer data reveal that the dominant iron oxides are hematite and goethite. Particularly for the yellower soil samples some prominent doublets, more certainly due to superparamagnetic relaxation, may be assigned to corresponding fractions of relatively small-sized particles.

Caracterização físico-química de queijo prato por espectroscopia no infravermelho e regressão de mínimos quadrados parciais

In this work an analytical methodology for the determination of relevant physicochemical parameters of prato cheese is reported, using infrared spectroscopy (DRIFT) and partial least squares regression (PLS). Several multivariate models were developed, using different spectral regions and preprocessing routines. In general, good precision and accuracy was observed for all studied parameters (fat, protein, moisture, total solids, ashes and pH) with standard deviations comparable with those provided by the conventional methodologies. The implantation of this multivariate routine involves significant analytical advantages, including reduction of cost and time of analysis, minimization of human errors, and elimination of chemical residues.

Aplicação e avanços da espectroscopia de luminescência em análises farmacêuticas

This paper provides a review on the latest advances and applications of the luminescence spectroscopy for the development of pharmaceuticals analyses methods, basically based on the photo- and chemiluminescence. The different forms of the drugs determination on pharmaceuticals through the fluorescence and chemiluminescence are discussed. The analyses include the drugs native fluorescence (liquid and solid-phases); the fluorescence from the oxidizing or reducing forms of the drug; the fluorescence from the chemical derivatization and their photochemistry and hydrolysis reactions. The quenching of luminescence and chemiluminescence generation for the pharmaceutical quantification are also shown. Finally, the trends and future perspectives of the luminescence spectroscopy in the field of the pharmaceutical research are discussed.

Efeito do intemperismo artificial em quatro madeiras tropicais monitorado por espectroscopia de infravermelho (DRIFT)

Four tropical woods, were investigated to compare their performance and natural resistances to artificial weathering using the diffuse reflectance infrared Fourier transform spectroscopy (DRIFT). The species were garapeira (Apuleia leiocarpa), itaúba (Mezilaurus itauba) and tauari (Couratari sp.), woods traditionally indicated for exterior uses, and marupá (Simarouba amara), that served as reference. The samples were submitted to cycles of UV radiation (350 nm) and water until 2,000 h. The photodegradation processes of woods surfaces were accomplished monitoring the changes in the intensities associated to lignin (1508 cm-1) and carbonyl group (1736 cm-1) absorptions. The results have shown that lignin was the first component to be photodegradated, resulting in surfaces mainly composed by cellulose, after 2,000 h of UV irradiation. The processes of formation and lixiviation of carbonyl compounds were different for each species. The experimental conditions used in this work were too severe to evaluate the wood density and extractives content influences during the treatment.

Técnica de bombeio e prova para medidas de absorção de estado excitado e de emissão estimulada, em materiais sólidos dopados com íons terras raras

Rare earth ion doped solid state materials are the most important active media of near-infrared and visible lasers and other photonic devices. In these ions, the occurrence of Excited State Absorptions (ESA), from long lived electronic levels, is commonplace. Since ESA can deeply affect the efficiencies of the rare earth emissions, evaluation of these transitions cross sections is of greatest importance in predicting the potential applications of a given material. In this paper a detailed description of the pump-probe technique for ESA measurements is presented, with a review of several examples of applications in Nd3+, Tm3+ and Er3+ doped materials.

Espectrofotometria de longo caminho óptico em espectrofotômetro de duplo-feixe convencional: uma alternativa simples para investigações de amostras com densidade óptica muito baixa

We describe the design and tests of a set-up mounted in a conventional double beam spectrophotometer, which allows the determination of optical density of samples confined in a long liquid core waveguide (LCW) capillary. Very long optical path length can be achieved with capillary cell, allowing measurements of samples with very low optical densities. The device uses a custom optical concentrator optically coupled to LCW (TEFLON® AF). Optical density measurements, carried out using a LCW of ~ 45 cm, were in accordance with the Beer-Lambert Law. Thus, it was possible to analyze quantitatively samples at concentrations 45 fold lower than that regularly used in spectrophotometric measurements.

Previsão das propriedades físicas do papel kraft por espectroscopia no infravermelho próximo (NIR) e regressão por mínimos quadrados parciais (PLS)

The main objective of the present work is represented by the characterization of the physical properties of industrial kraft paper (i.e. transversal and longitudinal tear resistance, transversal traction resistance, bursting or crack resistance, longitudinal and transversal compression resistance (SCT (Compressive Strength Tester) and compression resistance (RCT-Ring Crush Test)) by near infrared spectroscopy associated to partial least squares regression. Several multivariate models were developed, many of them with high prevision capacity. In general, low prevision errors were observed and regression coefficients that are comparable with those provided by conventional standard methodologies.

Estudo por espectroscopia micro-Raman dos mecanismos de separação de fase em vidros fosfatos de metais de transição

Glass-ceramics are prepared by controlled separation of crystal phases in glasses, leading to uniform and dense grain structures. On the other hand, chemical leaching of soluble crystal phases yields porous glass-ceramics with important applications. Here, glass/ceramic interfaces of niobo-, vanado- and titano-phosphate glasses were studied by micro-Raman spectroscopy, whose spatial resolution revealed the multiphase structures. Phase-separation mechanisms were also determined by this technique, revealing that interface composition remained unchanged as the crystallization front advanced for niobo- and vanadophosphate glasses (interface-controlled crystallization). For titanophosphate glasses, phase composition changed continuously with time up to the equilibrium composition, indicating a spinodal-type phase separation.

Concentrações de amônio na água da chuva e estimativa de emissão de amônia de rebanhos domésticos de Pinheiro e Viana, Baixada Maranhense

Rainwater samples (bulk deposition samples) were collected in Pinheiro and Viana. Rainwater pHs were higher than the range usually expected for unpolluted rain (5.0-5.6). The highest values were found in the beginning of the rainy season. High concentrations of ammonium found in the rainwater samples could probably explain the high pHs. Grazing animals and other human activities, combined with soil characteristics and climatic conditions can be the potential factors controlling the rainwater concentrations of ammonium in Baixada Maranhense.