Characterization of methylcellulose produced from sugar cane bagasse cellulose: Crystallinity and thermal properties

In the present work, methylcellulose produced from sugar cane bagasse was characterized by FTIR, WAXD, DTA and TGA techniques. Two samples were synthesized: methylcellulose A and rnethylcellulose B. The only difference in the process was the addition of fresh reactants during the preparation of methylcellulose B. The ratio between the absorption intensities of the C-H stretching band at around 2900 cm(-1) and C-H stretching at around 3400 cm(-1) for methylcellulose B is higher than for methylcellulose A, indicating that methylcellulose B showed an increase in the degree of substitution (DS). Methylcellulose A presents a more heterogeneous structure, which is similar to the original cellulose as seen through FTIR and DTA. Methylcellulose B showed thermal properties similar to commercial methylcellulose. The modification of rnethylcellulose preparation method allows the production of a material with higher DS, crystallinity and thermal stability in relation to the original cellulose and to methylcellulose A. (c) 2006 Elsevier Ltd. All rights reserved.

Spectroscopic characterization of BPSCCO thin films grown by dip-coating technique

This work describes the growth of Bi2-xPbxSr2Can-1CunO2n+4 thin films by the dip-coating technique for 0.4 less than or equal to x less than or equal to 1. X-ray and Raman spectroscopic techniques were carried out in order to characterize the films at room temperature. From X-ray data it is observed that the films are multi-phased presenting phases 2201, 2212 and 2223 along with the undesirable Ca2PbO4 phase. It is also observed that phase 2212 becomes dominant when Pb content increases. The Raman modes observed agree with the overall features expected for these compounds. (C) 2003 Elsevier B.V. B.V. All rights reserved.

Characterization of BaTi1-xZrxO3 thin films obtained by a soft chemical spin-coating technique

Single-phase perovskite structure BaZrxTi1-xO3 (BZT) (0.05less than or equal toxless than or equal to0.25) thin films were deposited on Pt-Ti-SiO2-Si substrates by the spin-coating technique. The structural modifications in the thin films were studied using x-ray diffraction and micro-Raman scattering techniques. Lattice parameters calculated from x-ray data indicate an increase in lattice (a axis) with the increasing content of zirconium in these films. Such Zr substitution also result in variations of the phonon mode wave numbers, especially those of lower wave numbers, for BaZrxTi1-xO3 thin films, corroborate to the structural change caused by the zirconium doping. on the other hand, Raman modes persist above structural phase transition, although all optical modes should be Raman inactive in the cubic phase. The origin of these modes must be interpreted as a function of a local breakdown of the cubic symmetry, which could be a result of some kind of disorder. The BZT thin films exhibited a satisfactory dielectric constant close to 181-138, and low dielectric loss tan delta<0.03 at the frequency of 1 kHz. The leakage current density of the BZT thin films was studied at elevated temperatures and the data obey the Schottky emission model. Through this analysis the Schottky barrier height values 0.68, 1.39, and 1.24 eV were estimated to the BZT5, BZT15, and BZT25 thin films, respectively. (C) 2004 American Institute of Physics.

Synthesis, characterization and initial biological studies of a new platinum(II) complex with deoxyalliin

A new platinum(II) complex with deoxyalliin was synthesized and characterized by chemical and spectroscopic techniques. Elemental and mass spectrometry analyses of the solid complex fit to the composition [Pt(C6H11NO2S)Cl-2] center dot H2O. C-13 NMR, N-15 NMR and infrared spectra of the complex are consistent with coordination of deoxyalliin to Pt( II) through the nitrogen and sulfur atoms forming a square-planar geometry. The complex is soluble in dimethylsulfoxide. Biological analysis for evaluation of a potential cytotoxic effect of the complex was performed using HeLa cells, a human cervix adenocarcinoma-derived cell line. The results were compared with those of a palladium( II) complex previously described.

Structural and phenomenological characterization of the thermoreversible sol-gel transition of a zirconyl aqueous precursor modified by sulfuric acid

The thermoreversible sol-gel transition is well-known in biological and organic polymeric systems but has not been reported for inorganic systems. In this paper we put in evidence a thermoreversible sol-gel transition for zirconyl chloride aqueous solutions modified by sulfuric acid in the ratio 3:1 Zr:SO4. The synthesis conditions are detailed and a variety of experimental techniques (turbidimetry, dynamic rheology, and EXAFS) have been employed for investigating the thermal reversibility and the chemical structure of this new material. Turbidimetric measurements performed for solutions containing different concentrations of precursor have evidenced that the sol-gel transformation temperature increases from 50 to 80 degrees C as the concentration of zirconyl chloride decreases from 0.22 to 0.018 mol L-1. A more detailed study has been done for the sample with [Zr] = 0.156 mol L-1, in which the sol-gel-sol transformation has been repeated several times by a cyclic variation of the temperature. The mechanical properties of this sample, evaluated by measuring the storage and the loss moduli, show a change from liquid like to viscoelastic to elastic behavior during the sol-gel transition and vice versa during the gel-sol one. In situ EXAFS measurements performed at the Zr K-edge show that no change of the local order around Zr occurs during the sol-gel-sol transition, in agreement with the concept of physical gel formation. We have proposed for the structure of the precursor an inner core made of hydroxyl and oxo groups bridging together zirconium atoms surrounded in surface by complexing sulfate ligands, the sulfate groups act as a protective layer, playing a key role in the linking propagation among primary particles during sol-gel-sol transition.

Structural characterization of blends containing both PVDF and natural rubber latex

Films containing different volumes of latex of natural rubber (NR) in a fixed mass of poly (vinylidene fluoride) (PVDF) powder were fabricated by compressing under annealing a mixture of both materials without using any solvent. This is an important issue keeping in mind that these films have to be used in the future as biomaterials in different applications once the solvents that are used to dissolve the PVDF become toxic to human. The films with different percentage of latex in PVDF were characterized using microRaman scattering and Fourier transform infrared absorption (FTIR) spectroscopies, thermomechanical techniques using thermogravimetry (TG), differential scanning calorimetry (DSC), dynamical-mechanical analysis (DMA) and scanning electron microscopy (SEM). The results showed that the latex of NR and PVDF do not interact chemically, leading to the formation of a polymeric blend with high thermal stability and mechanical properties suitable for applications involving bone (prostheses, for instance). Besides, the results recorded using the micro-Raman technique revealed that for a fixed amount of PVDF the higher the amount of latex in the blend, the better the miscibility between both materials. Copyright (c) 2005 John Wiley & Sons, Ltd.

Isolation and chemical characterization of PwTx-II: A novel alkaloid toxin from the venom of the spider Parawixia bistriata (Araneidae, Araneae)

Brazil has many species of spiders belonging to Araneidae family however, very little is known about the composition, chemical structure and mechanisms of action of the main venom components of these spiders. The main objective of this work was to isolate and to perform the chemical characterization of a novel beta-carboline toxin from the venom of the spider Parawixia bistriata, a typical species of the Brazilian 'cerrado'. The toxin was purified by RP-HPLC and structurally elucidated by using a combination of different spectroscopic techniques (UV, ESI-MS/MS and H-1 NMR), which permitted the assignment of the molecular structure of a novel spider venom toxin, identified as 1-4-guanidinobutoxy-6-hydroxy-1,2,3,4-tetrahydro-beta-carboline, and referred to here as PwTx-II. This compound is toxic to insects (LD50 = 12 +/- 3 eta g/mg honeybee), neurotoxic, convulsive and lethal to rats (LD50 = 9.75 mg/kg of male Wistar rat). (c) 2005 Elsevier Ltd. All rights reserved.

Formation and characterization of soy bean oil/surfactant/water microemulsions

Pseudoternary phase diagrams, at 25 degrees C, were constructed for the systems soy bean oil (SBO)/surfactant/water, with single anionic sodium bis(2-ethylhexyl)sulfosuccinate (AOT), nonionic monoolein (MO) and mixtures of these surfactants, showing the isotropic phase of W/O microemulsions (MEs). The area of ME formation in the phase diagrams was shown to be dependent of the relative amount of surfactants, being larger for MO:AOT equals to 2:1. Rheological and dynamic light scattering (DLS) studies indicated that the viscosity of the isotropic ME phase exhibited two different behaviors depending on composition. The viscosity of dry MEs initially decreased with increasing amount of water following a dilution line in the phase diagram, i.e., a constant surfactant:SBO percentage ratio. As the water content increased the relative viscosity attained a minimum and then increased. This minimum could be related to the transition between two ME regions, L-2 and L'(2), having different characteristics. DLS measurements confirm the existence of ordinary W/O ME droplets in the L-2 region and suggest the existence of another structure in the L'(2) region. The size of the MEs droplets in L-2 phase ranges from 3.6 to 16.5 nm, depending on composition of SBO, surfactant and water. Small angle X-ray scattering (SAXS) also indicates the existence of structures with different characteristics, for the SAXS curves exhibit a typical micelle asymmetrical peak at low scattering vector q for MEs in L-2 but a symmetrical correlation peak at higher q vector in L'(2). (c) 2006 Elsevier B.V. All rights reserved.

Characterization of an all sol-gel electrochromic device WO3/Ormolyte/CeO2-TiO2

Electrochemical lithium intercalation in thin films of CeO2-TiO2 and WO3, prepared by the sol-gel technique was investigated with cyclic voltammetry and spectroelectrochemical techniques in propylene carbonate solutions. A solid state system having the configuration WO3/Ormolyte/CeO2-TiO2 has been assembled. The solid electrolyte, an organically modified electrolyte (ormolyte), was prepared with different [O]/[Li] ratios. The transmittance variation of this system during a potentiostatic step from -0.7 V to 0.8 V was about 35% at 550 nm.

Multifractal characterization of saprolite particle-size distributions after topsoil removal

Multifractal analysis is now increasingly used to characterize soil properties as it may provide more information than a single fractal model. During the building of a large reservoir on the Parana River (Brazil), a highly weathered soil profile was excavated to a depth between 5 and 8 m. Excavation resulted in an abandoned area with saprolite materials and, in this area, an experimental field was established to assess the effectiveness of different soil rehabilitation treatments. The experimental design consisted of randomized blocks. The aim of this work was to characterize particle-size distributions of the saprolite material and use the information obtained to assess between-block variability. Particle-size distributions of the experimental plots were characterized by multifractal techniques. Ninety-six soil samples were analyzed routinely for particle-size distribution by laser diffractometry in a range of scales, varying from 0.390 to 2000 mu m. Six different textural classes (USDA) were identified with a clay content ranging from 16.9% to 58.4%. Multifractal models described reasonably well the scaling properties of particle-size distributions of the saprolite material. This material exhibits a high entropy dimension, D-1. Parameters derived from the left side (q > 0) of the f(alpha) spectra, D-1, the correlation dimension (D-2) and the range (alpha(0)-alpha(q+)), as well as the total width of the spectra (alpha(max) - alpha(min)) all showed dependence on the clay content. Sand, silt and clay contents were significantly different among treatments as a consequence of soil intrinsic variability. The D, and the Holder exponent of order zero, alpha(0), were not significantly different between treatments; in contrast, D-2 and several fractal attributes describing the width of the f(alpha) spectra were significantly different between treatments. The only parameter showing significant differences between sampling depths was (alpha(0) - alpha(q+)). Scale independent fractal attributes may be useful for characterizing intrinsic particle-size distribution variability. (c) 2006 Elsevier B.V. All rights reserved.

Synthesis and characterization of cellulose acetate produced from recycled newspaper

In this work, the viability of recycling newspaper for producing cellulose acetate was tested. Newspaper recycling is extremely important not only for the environment preservation, but also from the economical point of view of aggregating value to this residue. Cellulose acetate was produced from a homogeneous acetylation, and then characterized by FTIR, DSC and TGA. Acetylation times were 48 h for as received newspaper (CA48) and 24 h for delignified newspaper (CA24), resulting in cellulose diacetate (DS = 1.98 +/- 0.22) for CA48 and cellulose triacetate (DS = 2.79 +/- 0.02) for CA24, respectively. Membranes of these materials were produced and characterized according to the previously mentioned techniques and by measurements of water vapor flux, which were compared to membranes of nanofiltration SG from Osmonix (R). Results showed that independently of a purification step, it is possible to produce cellulose acetate membranes through the chemical recycling of newspaper and that membrane CA24 presents thermal stability comparable to membranes produced of commercial cellulose acetate. (C) 2007 Elsevier Ltd. All rights reserved.

Lithium thiazolidine-4-carboxylate: Synthesis, spectroscopic characterization and preliminary in vitro cytotoxic studies in human HeLa cells

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Cytochemical characterization of the endomembranous system during oocyte secondary growth in Serrasalmus spilopleura (Teleostei, Characiformes, Characidae)

The endomembranous system of Serrasalmus spilopleura oocyte secondary growth was analysed using structural and ultrastructural cytochemical techniques. In vitellogenic oocytes, the endoplasmic reticulum components, the nuclear envelope intermembranous space, some Golgi dictiossomes, lysosomes, yolk granules, regions of the egg envelope and sites of the follicle cells react to acid phosphatase detection (AcPase). The cortical alveoli, some heterogeneous cytoplasmic structures, regions of the egg envelope, and sites of the follicle cells are strongly contrasted by osmium tetroxide and zinc iodide impregnation (ZIO). The endoplasmic reticulum components, some vesicles, and sites of the follicle cells also react to osmium tetroxide and potassium iodide impregnation (KI). The biosynthetic pathway of lysosomal proteins, such as acid phosphatase, required for vitellogenesis, involves the endoplasmic reticulum, Golgi complex, vesicles with inactive hydrolytic enzymes, and, finally, lysosomes. In S. spilopleura oocytes at secondary growth, the endomembranous system takes part in the production of the enzymes needed for vitellogenesis, and in the metabolism of yolk exogenous components (AcPase detection). The endomembranous system compartments also show reduction capacity (KI reaction) and are involved in the metabolism of proteins rich in SH-groups (ZIO reaction).

Chemical, spectroscopic characterization, and in vitro antibacterial studies of a new gold(I) complex with N-acetyl-L-cysteine

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)

Electrical and Magnetic Characterization of BSCCO and YBCO HTS Tapes for Fault Current Limiter Application

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)