Ledjane Silva Barreto

Sulfadiazine/hydroxypropyl-β-cyclodextrin host–guest system: Characterization, phase-solubility and molecular modeling

In this work we prepared and characterized an inclusion complex of the dihydropteroate synthase inhibitor sulfadiazine (SDZ) in 2-hydroxypropyl-beta-cyclodextrin (HPBCD). From the phase-solubility diagram we observed an increase in the water solubility of the drug, calculating a binding constant of 1879M(-1). The inclusion mode involves a NH(2)-in orientation of the drug in the HPBCD cavity, according to the 2D NMR (ROESY) data and confirmed by molecular modeling using the semiempirical PM6 and RM1 methods.

Morphology and thermal properties of poly(3-hydroxybutyrate-co-3-hydroxyvalerate)/attapulgite nanocomposites

Poly(3-hydroxybutyrate-co-3-hydroxyvalerate) - PHBV is a biodegradable polyester which has been studied as an option for the production of disposable goods. Attapulgite is a fibrous clay mineral. The aim of this work was to produce and characterize renewable resource derived-nanocomposites based on PHBV and organophilic attapulgite (MAT). The nanocomposites were characterized by XRD, SEM and thermal analysis. It was observed reduction in degree of crystallinity, in melting and glass transition temperatures and in thermal stability of polymer due to the addition of clay to PHBV matrix. The best results were obtained for PHBV films containing 3 and 5% MAT. These films presented a slight increase in processing window and decrease in crystalline temperature and in degree of crystallinity as compared to pure PHBV.

One-step preparation of CdS nanocrystals supported on thiolated silica-gel matrix and evaluation of photocatalytic performance

Here we report the use of a thiol-functionalized silica-gel to prepare supported CdS nanocrystals by a facile one-step procedure. Upon changing the relative proportion of the matrix we obtained nanocrystals with different average sizes and size distributions, as evidenced by spectroscopic measurements as well as TEM images. Photoluminescence spectra also indicated that the main effect of the matrix is related to the size control since the spectral profiles were found to be strongly dependent on the excitation wavelength. The performance of the material in the photocatalytic degradation of two commercial dyes (methylene blue and rhodamine 6G) has been tested under sunlight radiation, showing promising results. Almost complete decolorization has been observed after 80 min of exposure, with no adsorption on the silica surface.

Characterization, phase solubility and molecular modeling of α-cyclodextrin/pyrimethamine inclusion complex

An inclusion complex between the dihydrofolate reductase inhibitor pyrimethamine (PYR) and alpha-cyclodextrin (alpha-CD) was prepared and characterized. From the phase-solubility diagram, a linear increase of PYR solubility was verified as a function of alpha-CD concentration, suggesting the formation of a soluble complex. A 1:1 host-guest stoichiometry can be proposed according to the Jobs plot, obtained from the difference of PYR fluorescence intensity in the presence and absence of alpha-CD. Differential scanning calorimetry (DSC) measurements provided additional evidences of complexation such as the absence of the endothermic peak assigned to the melting of the drug. The inclusion mode characterized by two-dimensional (1)H NMR spectroscopy (ROESY) involves penetration of the p-chlorophenyl ring into the alpha-CD cavity, in agreement to the orientation optimized by molecular modeling methods.

Ecomateriais: desenvolvimento e aplicação de materiais porosos funcionais para proteção ambiental

Fundamental aspects of the conception and applications of ecomaterials, in particular porous materials in the perspective of green chemistry are discussed in this paper. General recommendations for description and classification of porous materials are reviewed briefly. By way of illustration, some case studies of materials design and applications in pollution detection and remediation are described. It is shown here how different materials developed by our groups, such as porous glasses, ecomaterials from biomass and anionic clays were programmed to perform specific functions. A discussion of the present and future of ecomaterials in green chemistry is presented along with important key goals.

Physicochemical study and characterization of the trimethoprim/2-hydroxypropyl-γ-cyclodextrin inclusion complex.

Here we report the preparation of a trimethoprim/2-hydroxypropyl-γ-cyclodextrin inclusion complex along with a physicochemical study, structural characterization, and molecular modeling of the complex. As main results, we observed from phase-solubility studies at two temperatures (20 °C and 35 °C) that the association constants decrease with increasing temperature. Values for K(1:1) constant were of the same magnitude order of those found for the parent γ-CD. The inclusion orientation as evidenced by ROESY measurements involves the inclusion of the 3,4,5-trimethoxybenzyl ring in the CD cavity from the larger rim. This is in agreement with semiempirical molecular modeling calculation.

Conductive carbon―clay nanocomposites from petroleum oily sludge

Oily sludge samples formed in water-oil separation tanks from a petroleum industry were collected, characterized and heat-treated at different temperatures, in order to yield carbon-clay composites. EDX microanalysis, XRD and FTIR data revealed that before carbonization the oily sludge was formed mainly by a mixture of quartz, montmorillonite, calcite, barite and oil residues. After carbonization, mineral phases present were mainly quartz, anorthite and gehlenite, in addition to graphitic and disordered carbon domains, according to XRD, Raman and TEM measurements. A preliminary evaluation of the electrical conductivity performed by Impedance Spectroscopy revealed that the composites formed are conductive, exhibiting conductivity values typical of semiconductors, in contrast to the precursor material.

The increase of surface area of a Brazilian palygorskite clay activated with sulfuric acid solutions using a factorial design

Palygorskite is fibrous clay in which the structural tetrahedral and octahedral layers are organized in a way that structural channels are formed, leading to high surface area. However, impurities inside the channels and aggregated ones considerably reduce the available area. In order to increase the surface area, an activation treatment can be considered useful. The goal of this work is the activation of palygorskite from Guadalupe, Piaui, via sulfuric acid treatment using a two-level factorial design. The influence of three parameters (solution molarity, temperature and time) on BET surface area was determined. Moreover, samples were characterized via X-ray diffraction (XRD) and fluorescence (XRF), Fourier-transform infrared spectroscopy (FTIR) and transmission electron microscopy (TEM). The largest surface area (282 m2/g) without considerable changes in clay structure and morphology was found in a sample treated with 5M H2SO4 at 70°C for 1h. The main parameters that favored the improvement of the surface area were the solutions molarity, temperature and their interaction.

Use of coir pith particles in composites with Portland cement

Brazil is the fourth largest worlds producer of coconut (Cocos nucifera L.). Coconut crops generate several wastes, including, coir pith. Coir pith and short fibers are the byproducts of extracting the long fibers and account for approximately 70% of the mature coconut husk. The main use of coir pith is as an agricultural substrate. Due to its shape and small size (0.075-1.2 mm), this material can be considered as a particulate material. The aim of this study was to evaluate the use of coir pith as an aggregate in cementitious composites and to evaluate the effect of the presence of sand in the performance of these composites. Some composites were produced exclusively with coir pith particles and other composites with coir pith partially substituting the natural sand. The cementitious composites developed were tested for their physical and mechanical properties and characterized by X-ray diffraction, scanning electron microscopy, energy dispersive X-ray spectroscopy and Fourier transform infrared spectroscopy to evaluate the effect of coir pith particles addition in cement paste and sand-cement-mortar. The statistical significance of the results was evaluated by one-way analysis of variance (ANOVA) test followed by multiple comparisons of the means by Tukeys test that showed that the composites with coir pith particles, with or without natural sand, had similar mechanical results, i.e., means were not statistically different at 5% significance level. There was a reduction in bulk density and an improved post-cracking behavior in the composites with coir pith particles compared to conventional mortar and to cement paste. These composites can be used for the production of lightweight, nonstructural building materials, according to the values of compressive strength (3.97-4.35 MPa) and low bulk density (0.99-1.26 g/cm(3)).

Caracterização de escamas do peixe piau (Leporinus elongatus) e sua aplicação na remoção de Cu(II) de meio aquoso

Characterization of fish scales of Leporinus elongatus and their application in the removal of Cu(II) from aqueous solutions are described. It was observed that the scales are mainly formed by hydroxyapatite and type I collagen. Adsorption of Cu(II) was performed using batch experiments at 25 0C. The ANOVA statistical results have shown that the Langmuir model was successful applied to determine the maximum adsorption capacity of 2.686 x10-4 mol g-1 and the Langmuir equilibrium parameter (b) of 168.8 L mol-1. The Langmuir separation parameter, RL, has shown favorable adsorption of Cu(II) on the scales.