Compatibility studies between captopril and pharmaceutical excipients used in tablets formulations

Captopril (CAP) was the first commercially available angiotensine-converting enzyme (ACE) inhibitor. In the anti-hypertensive therapy is considered the selected drug has to be therapeutically effective together with reduced toxicity. CAP is an antihypertensive drug currently being administered in tablet form. In order to investigate the possible interactions between CAP and excipients in tablets formulations, differential scanning calorimetry (DSC) and thermogravimetric (TG) analysis completed by X-ray powder diffraction (XRPD) and Fourier transform infrared spectroscopy (FTIR) were used for compatibility studies. A possible drug-excipient interaction was observed with magnesium stearate by DSC technique.

PtSnCe/C electrocatalysts for ethanol oxidation: DEFC and FTIR ""in-situ"" studies

The ethanol oxidation reaction (EOR) was investigated using PtSnCe/C electrocatalysts in different mass ratios (72:23:5, 68:22:10 and 64:21:15) that were prepared by the polymeric precursor method. Transmission electron microscopy (TEM) showed that the particles ranged in size from approximately 2 to 5 nm. Changes in the net parameters observed for Pt suggest the incorporation of Sn and Ce into the Pt crystalline network with the formation of an alloy between Pt, Sn and/or Ce. Among the PtSnCe catalysts investigated, the 68:22:10 composition showed the highest activity toward ethanol oxidation, and the current time curves obtained in the presence of ethanol in acidic media showed a current density 50% higher than that observed for commercial PtSn/C (E-Tek). During the experiments performed on single direct ethanol fuel cells, the power density for the PtSnCe/C 68:22:10 anode was nearly 40% higher than the one obtained using the commercial catalyst. Data from Fourier transform infrared (FTIR) spectroscopy showed that the observed behavior for ethanol oxidation may be explained in terms of a double mechanism. The presence of Sn and Ce seems to favor CO oxidation, since they produce an oxygen-containing species to oxidize acetaldehyde to acetic acid. Copyright (C) 2011, Hydrogen Energy Publications, LLC. Published by Elsevier Ltd. All rights reserved.

Evaluation of Postpolymerization as a Function of the Storage Time of Triethylene Glycol Dimethacrylate/2,2-Bis[4-(2-Hydroxy-3-Methacryloxy-Prop-1-Oxy)-Phenyl]-propane Bisphenyl-alpha-Glycidyl Ether Dimethacrylate Copolymers Used in Dental Resins by Differential Scanning Calorimetry and Dynamic Mechanical Analysis

The aim of this work was to evaluate the effect of the storage time on the thermal properties of triethylene glycol dimethacrylate/2,2-bis[4-(2-hydroxy-3-methacryloxy-prop-1-oxy)-phenyl]propane bisphenyl-alpha-glycidyl ether dimethacrylate (TB) copolymers used in formulations of dental resins after photopolymerization. The TB copolymers were prepared by photopolymerization with an Ultrablue IS light-emitting diode, stored in the dark for 160 days at 37 degrees C, and characterized with differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA), and Fourier transform infrared spectroscopy with attenuated total reflection. DSC curves indicated the presence of an exothermic peak, confirming that the reaction was not completed during the photopolymerization process. This exothermic peak became smaller as a function of the storage time and was shifted at higher temperatures. In DMA studies, a plot of the loss tangent versus the temperature initially showed the presence of two well-defined peaks. The presence of both peaks confirmed the presence of residual monomers that were not converted during the photopolymerization process. (C) 2009 Wiley Periodicals, Inc. J Appl Polym Sci 112: 679-684, 2009

A comparative study of the electrogeneration of hydrogen peroxide using Vulcan and Printex carbon supports

A comparative study of two different conductive carbon-black pigments, Vulcan XC-72 R and Printex L6, for the electrogeneration of hydrogen peroxide (H(2)O(2)) by reducing dissolved oxygen in an alkaline solution was performed. The materials were physically characterized by X-ray diffraction (XRD), Fourier transform infrared attenuated total reflection (ATR-FTIR) and X-ray photoelectron spectroscopy (XPS). XRD shows the presence of SO(2) and ATR-FTIR technique indicates a difference in NO and SO(2) functional groups between the two carbon pigments. XPS indicated presence of SO and NO and more oxygenated acid species on Printex L6. A rotating ring-disk electrode was used for electrochemical analysis of the oxygen reduction reaction (ORR). The results showed that the Printex L6 was better than Vulcan XC-72 R for H(2)O(2) production. Results also indicate that the number of electrons transferred in the ORR for Printex L6 and Vulcan XC-72 R were 2.2 and 2.9, respectively, while the percentages of H(2)O(2) formed were 88% and 51%. Scanning electrochemistry microscopy images confirmed the higher amount of H(2)O(2) formed in the Printex L6 pigment. Printex L6 was shown to be a more promising for H(2)O(2) production than Vulcan XC-72 R, while the latter was shown to have more potential for fuel cells. (C) 2011 Elsevier Ltd. All rights reserved.

A novel nanostructured composite formed by interaction of copper octa(3-aminopropyl)octasilsesquioxane with azide ligands: Preparation, characterization and a voltammetric application

This study presents the preparation, characterization and application of copper octa(3-aminopropyl)octasilsesquioxane following its subsequent reaction with azide ions (ASCA). The precursor (AC) and the novel compound (ASCA) were characterized by Fourier transform infrared spectra (FTIR), nuclear magnetic resonance (NMR), electron paramagnetic resonance (EPR), scanning electronic microscopy (SEM), X-ray diffraction (XRD), Thermogravimetric analyses and voltammetric technique. The cyclic voltammogram of the modified graphite paste electrode with ASCA (GPE-ASCA), showed one redox couple with formal potential (E(1/2)(ox)) = 0.30 V and an irreversible process at 1.1 V (vs. Ag/AgCl; NaCl 1.0 M; v = 20 mV s(-1)). The material is very sensitive to nitrite concentrations. The modified graphite paste electrode (GPE-ASCA) gives a linear range from 1.0 x 10(-4) to 4.0 x 10(-3) mol L(-1) for the determination of nitrite, with a detection limit of 2.1 x 10(-4) mol L(-1) and the amperometric sensitivity of 8.04 mA/mol L(-1). (C) 2010 Elsevier Ltd. All rights reserved.

Characterization by Fluorescence of Organic Matter from Oxisols under Sewage Sludge Applications

Sewage sludge from wastewater treatment contains organic matter and plant nutrients that can play an important role in agricultural production and the maintenance of soil fertility, The present study has aimed to evaluate the degree of humification following sewage sludge application of soil organic matter by laser-induced fluorescence and humic acids using ultraviolet-visible fluorescence, and including comparison with Fourier-transform infrared spectroscopy and elemental analysis. Sewage sludge applications to the soil caused a decrease in the degree of humification of the soil organic matter and humic acids for both a Typic Eutrorthox (clayey) soil and a Typic Haplorthox (sandy) soil of around 14 and 27%, respectively. This effect is probably clue to incorporation of newly formed humic substances from the sewage sludge into the characteristics of less humified material, and to the indigenous soil humic substances. The minor alterations observed in the clay soil probably occurred due to both the greater mineral association, which better stabilized the indigenous soil organic matter, and the higher microbial activity in this soil, which accelerated sewage sludge mineralization. Sewage sludge applications increased the C content for the clay and sandy soils by 7.4 and 15.4 g kg(-1), respectively, suggesting a positive effect on these two soils.

Desenvolvimento de redes de polímeros interpenetrantes (IPN) para a aplicação como eletrólito polimérico

Uma nova rede de polímeros interpenetrantes (IPN) baseada em poliuretana de óleo de mamona e poli(etileno glicol) e poli(metacrilato de metila) foi preparada para ser utilizada como eletrólito polimérico. Os seguintes parâmetros de polimerização foram avaliados: massa molecular do poli(etileno glicol) (PEG), concentração de PEG e concentração de metacrilato de metila. As membranas de IPN foram caracterizadas por calorimetria diferencial de varredura (DSC) e espectroscopia de infravermelho por transformada de Fourier (FT-IR). Os eletrólitos de redes de polímeros interpenetrantes (IPNE) foram preparados a partir da dopagem com sal de lítio através do inchamento numa solução de 10% em massa de LiClO4 na mistura de carbonato de etileno e carbonato de propileno na razão mássica de 50:50. As IPNEs foram caracterizadas por espectroscopia de impedância eletroquímica e Raman. As IPNEs foram testadas como eletrólito polimérico em supercapacitores. As células capacitivas foram preparadas utilizando eletrodos de polipirrol (PPy). Os valores de capacitância e eficiência foram calculados por impedância eletroquímica, voltametria cíclica e ciclos galvonostáticos de carga e descarga. Os valores de capacitância obtidos foram em torno de 90 F.g-1 e eficiência variou no intervalo de 88 a 99%. Os valores de densidade de potência foram superiores a 250 W.kg-1 enquanto que a densidade de energia variou de 10 a 33 W.h.kg-1, dependendo da composição da IPNE. As características eletroquímicas do eletrólito formado pela IPN-LiClO4 (IPNE) foram comparadas aos eletrólitos poliméricos convencionais, tais como poli(difluoreto de vinilideno)-(hexafluorpropileno) ((PVDF-HFP/LiClO4) e poliuretana comercial (Bayer desmopan 385) (PU385/LiClO4). As condutividades na temperatura ambiente foram da ordem de 10-3 S.cm-1. A capacitância da célula utilizando eletrodos de PPy com eletrólito de PVDFHFP foi de 115 F.g-1 (30 mF.cm-2) e 110 F.g-1 (25 mF.cm-2) para a célula com PU385 comparadas a 90 F.g-1 (20 mF.cm-2) para a IPNE. Os capacitores preparados com eletrólito de IPNE apresentaram valores de capacitância inferior aos demais, entretanto provaram ser mais estáveis e mais resistentes aos ciclos de carga/descarga. A interpenetração de duas redes poliméricas, PU e PMMA produziu um eletrólito com boa estabilidade mecânica e elétrica. Um protótipo de supercapacitor de estado sólido foi produzindo utilizando eletrodos impressos de carbono ativado (PCE) e o eletrólito polimérico de IPNE. A técnica de impressão de carbono possui várias vantagens em relação aos outros métodos de manufatura de eletrodos de carbono, pois a área do eletrodo, espessura e composição são variáveis que podem ser controladas experimentalmente. As células apresentaram uma larga janela eletroquímica (4V) e valores da capacitância da ordem de 113 mF.cm-2 (16 F.g-1). Métodos alternativos de preparação do PCE investigados incluem o uso de IPNE como polímero de ligação ao carbono ativado, estes eletrodos apresentaram valores de capacitância similares aos produzidos com PVDF. A influência do número de camadas de carbono usadas na produção do PCE também foi alvo de estudo. Em relação ao eletrólito polimérico, o plastificante e o sal de lítio foram adicionados durante a síntese, formando a IPNGel. As células apresentaram alta capacitância e boa estabilidade após 4000 ciclos de carga e descarga. As membranas de IPN foram testadas também como reservatório de medicamento em sistemas de transporte transdérmico por iontoforese. Os filmes, mecanicamente estáveis, formaram géis quando inchado em soluções saturadas de lidocaina.HCl, anestésico local, em propileno glicol (PG), poli(etileno glicol) (PEG400) e suas misturas. O grau de inchamento em PG foi de 15% e 35% em PEG400. Agentes químicos de penetração foram utilizados para diminuir a resistência da barreira causada pela pele, dentre eles o próprio PG, a 2-pirrolidinona (E1) e a 1-dodecil-2-pirrolidinona (E2). Os géis foram caracterizados por espectroscopia de impedância eletroquímica e transporte passivo e por iontoforese através de uma membrana artificial (celofane). O sistema IPN/ lidocaina.HCl apresentou uma correlação linear entre medicamento liberado e a corrente aplicada. Os melhores resultados de transporte de medicamento foram obtidos utilizando o PG como solvente.

Obtenção de nanopartículas de hexaferrita de bário pelo método pechini

In this study barium hexaferrite was (general formulae BaFe12O19) was synthesized by the Pechini method under different conditions of heat treatment. Precursors like barium carbonate and iron nitrate were used. These magnetic ceramic, with magnetoplumbite type structure, are widely used as permanent magnet because of its excellent magnetic properties, such as: high Curie temperature, good magnetic anisotropy, high coercivity and corrosion resistance. The samples were characterized by thermal analysis (DTA and TG), X- ray Diffraction (XRD), Fourier transform infrared spectroscopy (FTIR), Scanning Electron Microscopy (SEM) end Vibrating sample Magnetometer (VSM). The results confirm the expected phase, which was reinforced according to our analysis. A single phase powder at relatively high temperatures with particle sizes around 100 nm was obtained. The characteristic magnetic behavior one of the phases has been noted (probably superparamagnetic material), while another phase was identified as a ferrimagnetic material. The ferrimagnetic phase showed vortex configuration with two central and slightly inclined plateaus. In general, increase of heat treatment temperature and time, directly influenced the technological properties of the samples

Influência do uso de combustíveis alternativos na síntese por combustão via microondas para a produção de materiais cerâmicos com estrutura espinélio

The development and study of detectors sensitive to flammable combustible and toxic gases at low cost is a crucial technology challenge to enable marketable versions to the market in general. Solid state sensors are attractive for commercial purposes by the strength and lifetime, because it isn t consumed in the reaction with the gas. In parallel, the use of synthesis techniques more viable for the applicability on an industrial scale are more attractive to produce commercial products. In this context ceramics with spinel structure were obtained by microwave-assisted combustion for application to flammable fuel gas detectors. Additionally, alternatives organic-reducers were employed to study the influence of those in the synthesis process and the differences in performance and properties of the powders obtained. The organic- reducers were characterized by Thermogravimetry (TG) and Derivative Thermogravimetry (DTG). After synthesis, the samples were heat treated and characterized by Fourier Transform Infrared Spectroscopy (FTIR), X-ray Diffraction (XRD), analysis by specific area by BET Method and Scanning Electron Microscopy (SEM). Quantification of phases and structural parameters were carried through Rietveld method. The methodology was effective to obtain Ni-Mn mixed oxides. The fuels influenced in obtaining spinel phase and morphology of the samples, however samples calcined at 950 °C there is just the spinel phase in the material regardless of the organic-reducer. Therefore, differences in performance are expected in technological applications when sample equal in phase but with different morphologies are tested

Síntese e impregnação de peneiras moleculares Fe MCM-41 derivada de sílica da casca do arroz

The mesoporous molecular sieves of the MCM-41 and FeMCM-41 type are considered promissory as support for metals used as catalysts in oil-based materials refine processes and as adsorbents for environmental protection proposes. In this work MCM-41 and FeMCM41 were synthesized using rice husk ash - RHA as alternative to the conventional silica source. Hydrothermal synthesis was the method chosen to prepare the materials. Pre-defined synthesis parameters were 100°C for 168 hours, later the precursor was calcinated at 550°C for 2 hours under nitrogen and air flow. The sieves containing different proportions of iron were produced by two routes: introduction of iron salt direct synthesis; and a modification post synthesis consisting in iron salt 1 % and 5% impregnation in the material followed by thermal decomposition. The molecular sieves were characterized by X ray diffraction XRD, Fourier transform infrared spectroscopy FT-IR, X ray fluorescence spectroscopy XFR, scanning electronic microscopy SEM, specific surface area using the BET method, Termogravimetry TG. The kinetic model of Flynn Wall was used with the aim of determining the apparent activation energy of the surfactant remove (CTMABr) in the MCM- 41 porous. The analysis made possible the morphology characterization, identifying the presence of hexagonal structure typical for mesoporous materials, as well as observation of the MCM41 and iron of characteristic bands.

Síntese, aplicação e avaliação do efeito do teor de fósforo da celulose fosfatada em argamassa de alvenaria com aditivo comercial a base de hidroxi-etil-metil celulose (HEMC)

Generally, cellulose ethers improves mortar properties such as water retention, workability and setting time, along with adherence to the substrate. However, a major disadvantage of the addition of cellulose ethers in mortars is the delay in hydration of the cement. In this paper a cellulose phosphate (Cp) was synthesized water soluble and has been evaluated the effect of their incorporation into mortar based on Portland cement. Cellulose phosphate obtained was characterized by spectrophotometry Fourier transform infrared (FTIR), X-ray diffraction (XRD), elemental analysis and scanning electron microscopy (SEM). Mortar compositions were formulated with varying phosphorus content in cellulose and cellulose phosphate concentrations, when used in partial or total replacement of the commercial additive based hydroxyethyl methyl cellulose (HEMC). The mortars formulated with additives were prepared and characterized by: testing in the fresh state (consistency index, water retention, bulk density and air content incorporated) and in the hardened state (absorption by capillarity, density, flexural and compression strength). In mixtures the proportion of sand:cement of 1:5 (v / v) and factor a / c = 1.31 and water were held constant. Overall, the results showed that the celluloses phosphates employed in mortars added acted significantly when partially substituting the commercial additive. With regard to consistency index, water retention and bulk density in the fresh state and absorption by capillarity and bulk density apparent in the hardened state, showed no appreciable differences as compared to the commercial additive. The incorporated air content in the fresh state reduced markedly, but did not affect other properties. The mortars with cellulose phosphate, partially replacing the commercial additive showed an improvement of the properties of flexural strength and compressive strength

Caracterização microestrutural e elétrica de La(FexNi1-x)O3 sintetizado pelo método da gelatina

The present work deals with the synthesis of materials with perovskite structure with the intention of using them as cathodes in fuel cells SOFC type. The perovskite type materials were obtained by chemical synthesis method, using gelatin as the substituent of citric acid and ethylene glycol, and polymerizing acting as chelating agent. The materials were characterized by X-ray diffraction, thermal analysis, spectroscopy Fourier transform infrared, scanning electron microscopy with EDS, surface area determination by the BET method and Term Reduction Program, TPR. The compounds were also characterized by electrical conductivity for the purpose of observing the possible application of this material as a cathode for fuel cells, solid oxide SOFC. The method using gelatin and polymerizing chelating agent for the preparation of materials with the perovskite structure allows the synthesis of crystalline materials and homogeneous. The results demonstrate that the route adopted to obtain materials were effective. The distorted perovskite structure have obtained the type orthorhombic and rhombohedral; important for fuel cell cathodes. The presentation material properties required of a candidate cathode materials for fuel cells. XRD analysis contacted by the distortion of the structures of the synthesized materials. The analyzes show that the electrical conductivity obtained materials have the potential to act as a cell to the cathode of solid oxide fuel, allowing to infer an order of values for the electrical conductivities of perovskites where LaFeO3 < LaNiO3 < LaNi0,5Fe0,5O3. It can be concluded that the activity of these perovskites is due to the presence of structural defects generated that depend on the method of synthesis and the subsequent heat treatment

Síntese hidrotérmica assistida por micro-ondas de tiO2, e aplicação em nanocompósito

In recent decades have seen a sharp growth in the study area of nanoscience and nanotechnology and is included in this area, the study of nanocomposites with self-cleaning properties. Since titanium dioxide (TiO2) has high photocatalytic activity and also antimicrobial, self-cleaning surfaces in your application has been explored. In this study a comparison was made between two synthesis routes to obtain TiO2 nanoparticles by hydrothermal method assisted by microwave. And after analysis of XRD and SEM was considered the best material for use in nanocomposites. It was deposited nanocomposite film of poly (dimethyl siloxane) (PDMS) with 0.5, 1, 1.5 and 2% by weight of nanoparticles of titanium dioxide (TiO2) by the spraying method. The nanocomposite was diluted with hexane and the suspension was deposited onto glass substrate, followed by curing in an oven with forced air circulation. The photocatalytic activity of the nanocomposite impregnated with methylene blue was evaluated by UV- vis spectroscopy from the intensity variation of absorption main peak at 660nm with time of exposure to the UV chamber. Changes in the contact angle and microhardness were analyzed before and after UV aging test. The effect of ultraviolet radiation on the chemical structure of the PDMS matrix was evaluated by spectrophotometry Fourier transform infrared (FTIR).The results indicated that the addition of TiO2 nanoparticles in the coating PDMS gave high photocatalytic activity in the decomposition of methylene blue, an important characteristic for the development of self-cleaning coatings

Síntese e caracterização do poli(ácido láctico) para potencial uso em sistemas de liberação controlada de fármacos

With the advances in medicine, life expectancy of the world population has grown considerably in recent decades. Studies have been performed in order to maintain the quality of life through the development of new drugs and new surgical procedures. Biomaterials is an example of the researches to improve quality of life, and its use goes from the reconstruction of tissues and organs affected by diseases or other types of failure, to use in drug delivery system able to prolong the drug in the body and increase its bioavailability. Biopolymers are a class of biomaterials widely targeted by researchers since they have ideal properties for biomedical applications, such as high biocompatibility and biodegradability. Poly (lactic acid) (PLA) is a biopolymer used as a biomaterial and its monomer, lactic acid, is eliminated by the Krebs Cycle (citric acid cycle). It is possible to synthesize PLA through various synthesis routes, however, the direct polycondensation is cheaper due the use of few steps of polymerization. In this work we used experimental design (DOE) to produce PLAs with different molecular weight from the direct polycondensation of lactic acid, with characteristics suitable for use in drug delivery system (DDS). Through the experimental design it was noted that the time of esterification, in the direct polycondensation, is the most important stage to obtain a higher molecular weight. The Fourier Transform Infrared (FTIR) spectrograms obtained were equivalent to the PLAs available in the literature. Results of Differential Scanning Calorimetry (DSC) showed that all PLAs produced are semicrystalline with glass transition temperatures (Tgs) ranging between 36 - 48 °C, and melting temperatures (Tm) ranging from 117 to 130 °C. The PLAs molecular weight characterized from Size Exclusion Chromatography (SEC), varied from 1000 to 11,000 g/mol. PLAs obtained showed a fibrous morphology characterized by Scanning Electron Microscopy (SEM)

Síntese do Poli (ácido láctico) por policondensação direta utilizando um planejamento fatorial

The environmental impact caused by the disposal of non-biodegradable polymer packaging on the environment, as well as the high price and scarcity of oil, caused increase of searches in the area of biodegradable polymers from renewable resources were developed. The poly (lactic acid) (PLA) is a promising polymer in the market, with a large availability of raw material for the production of its monomer, as well as good processability. The aimed of this study was synthesis PLA by direct polycondesation of lactic acid, using the tool of experimental design (DOE) (central composite rotatable design (CCRD)) to optimize the conditions of synthesis. The polymer obtained was characterized by scanning electron microscopy (SEM), Fourier transform infrared spectroscopy (FTIR), viscosimetric analysis, differential scanning calorimeter (DSC) and size exclusion chromatography (SEC). The results confirmed the formation of a poly (lactic acid) semicrystalline in the syntheses performed. Through the central composite rotatable design was possible to optimize the crystallization temperature (Tc) and crystallinity degree (Xc). The crystallization temperature maximum was found for percentage of catalyst around the central point (0,3 (%W)) and values of time ranging from the central point (6h) to the upper level (+1) (8h). The crystallization temperature maximum was found for the total synthesis time of 4h (-1) and percentage of catalyst 0,1(W%) (-1). The results of size exclusion chromatography (SEC) showed higher molecular weights to 0,3 (W%) percent of catalyst and total time synthesis of 3,2h