Direct electron paramagnetic resonance monitoring of the peptide synthesis coupling reaction in polymeric support

This work demonstrates, for the first time. a time-resolved electron paramagnetic resonance (EPR) monitoring of a chemical reaction occurring in a polymeric structure. The progress of the coupling of a N-alpha-tert-butyloxycarbonyl-2.2.6.6-tetramethylpiperidine-1-oxyl-4-amino-4-carboxylic acid (Boc-TOAC) spin probe to a model peptide-resin was followed through EPR spectra. Progressive line broadening of EPR peaks was observed, indicative of an increased population of immobilized spin probe molecules attached to the solid support. The time for spectral stabilization of this process coincided with that determined in a previous Coupling study. thereby validating this in situ quantitative monitoring of the reaction. In addition, the influence of polymer swelling degree and solvent viscosity, as well as of the steric hindrance within beads. on the rate of coupling reaction was also addressed. A deeper evaluation of the latter effect was possible by determining unusual polymer parameters such as the average site-site distance and site-concentration within resin beads in each solvent system. (c) 2006 Elsevier Ltd. 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.

Synthesis, structural refinement and optical behavior of CaTiO3 powders: A comparative study of processing in different furnaces

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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)

Development of metal oxide nanoparticles by soft chemical method

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

Synthesis, ferroelectric and optical properties of (Pb,Ca)TiO3 thin films by soft solution processing

Calcium modified lead titanate sol was synthesized using a soft solution processing, the so-called polymeric precursor method. In soft chemistry method, soluble precursors such as lead acetate trihydrate, calcium carbonate and titanium isopropoxide, as starting materials, were mixed in aqueous solution. Pb0.7Ca0.3TiO3 thin films were deposited on platinum-coated silicon and quartz substrates by means of the spinning technique. The surface morphology and crystal structure, dielectric and optical properties of the thin films were investigated. The electrical measurements were conducted on metal-ferroelectric-metal (MFM) capacitors. The typical measured small signal dielectric constant and dissipation factor at a frequency of 100 kHz were 299 and 0.065, respectively, for a thin film with 230 nm thickness annealed at 600degreesC for 2 h. The remanent polarization (2P(r)) and coercive field (E-c) were 32 muC/cm(2) and 100 kV/cm, respectively. Transmission spectra were recorded and from them, refractive index, extinction coefficient, and band gap energy were calculated. Thin films exhibited good optical transmissivity, and had optical direct transitions. The present study confirms the validity of the DiDomenico model for the interband transition, with a single electronic oscillator at 6.858 eV. The optical dispersion behavior of PCT thin film was found to fit well the Sellmeir dispersion equation. The band gap energy of the thin film, annealed at 600degreesC, was 3.56 eV. The results confirmed that soft solution processing provides an inexpensive and environmentally friendly route for the preparation of PCT thin films.

Enhanced Eu3+ Emission in Aqueous Phosphotungstate Colloidal Systems: Stabilization of Polyoxometalate Nanostructures

Luminescent Eu3+-containing polyphosphate tungstate aqueous colloidal systems were prgared and studied as a function of the relative polyphosphate tungstate content. In polyphosphate-rich solutions, Eu-H- ions occupy cagelike sites composed of phosphate groups from the metaphosphate chains. In these sites, an average number of 0.5 water molecule coordinates to an Eu3+ ion and the 500 emission quantum efficiency is 0.22. Tungstatc addition leads to important modifications in neighboring Eu3+ leading to coordination sites in the aqueous medium where metal ions are completely hidden from interactions with solvent molecules. Transmission electron microscopy results clearly show \V-rich nanoparticles with sizes between 5 and 10 nm for all tungstate relative concentrations. For high tungstatc relative contents (above 30 mol %), spectroscopic results suggest the presence of Eu34- in polyoxometalate (P0M)-like sites by comparison with the well-known decatungstoeuropate [EuW10O36](9-) structure. These new aqueous colloids display surprisingly high 5llo emission quantum efficiencies of ca 80% because of the strong ligand field provided by tungstate POM ligands and the complete absence of water molecules from the Eu3+ first coordination shell.

Synthesis, X-ray Crystal Structure and Theoretical Calculations of Antileishmanial Neolignan Analogues

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

High-efficient microwave synthesis and characterisation of SrSnO3

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Stable colloidal suspensions of nanostructured zirconium oxide synthesized by hydrothermal process

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

SiO2-GeO2 soot preform as a core for Eu2O3 nanocoating: Synthesis and photophysical study

Nowadays solid state chemists have the possibility of work with low temperature strategies to obtain solid state materials with appropriate physical and chemical properties for useful technological applications. Photonic core shell materials having a core and shell domains composed by a variety of compounds have been synthesized by different methods. In this work we used silica-germania soot prepared by vapor-phase axial deposition as a core where a nanoshell of Eu2O3 was deposited. A new sol-gel like method was used to obtain the Eu2O3 nanoshell coating the SiO2-GeO2 particles, which was prepared by the polymeric precursor method. The photophysical properties of Eu3+ were used to obtain information about the rare earth surrounding in the SiO2-GeO2@Eu2O3 material during the sintering process. The sintering process was followed by the luminescence spectra of Eu3+ and all the samples present the characteristic emission related to the D-5(0) -> F-7(J) (J=0, 1, 2, 3 and 4). The ratios of the D-5(0) -> F-7(2)/D-5(0) -> F-7(1) emission intensity for the SiO2-GeO2@Eu2O3 systems were calculated and it was observed an increase in its values, indicating a low symmetry around the Eu3+ as the temperature increases.

(Sr,Tm)ZrO3 powders prepared by the polymeric precursor method: Synthesis, optical properties and morphological characteristics

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Synthesis and functionalization of magnetite nanoparticles with different amino-functional alkoxysilanes

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Synthesis, Characterization, Anisotropic Growth and Photoluminescence of BaWO4

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Synthesis and electrochemical behavior of single-crystal magnetite nanoparticles

Water-dispersed magnetite nanoparticle synthesis from iron(II) chloride in dimethyl sulfoxide (DMSO)-water solution at different DMSO-water ratios in alkaline medium was reported. TEM and XRD results suggest a single-crystal formation with mean particle size in the range 4-27 nm. Magnetic nanoparticles are formed by the oxidative hydrolysis reaction from green rust species that leads to FeOOH formation, followed by autocatalysis of the adsorbed available Fe(II) on the FeOOH surfaces. The available hydroxyl groups seem to be dependent on the DMSO-water ratio due to strong molecular interactions presented by the solvent mixture. Goethite phase on the magnetite surface was observed by XRD data only for sample synthesized in the absence of DMSO. In addition, cyclic voltammetry with carbon paste electroactive electrode (CV-CPEE) results reveal two reduction peaks near 0 and +400 mV associated with the presence of iron(III) in different chemical environments related to the surface composition of magnetite nanoparticles. The peak near +400 mV is related to a passivate thin layer surface such as goethite on the magnetite nanoparticle, assigned to the intensive hydrolysis reaction due to strong interactions between DMSO-water molecules in the initial solvent mixture that result in a hydroxyl group excess in the medium. Pure magnetite phase was only observed in the samples prepared at 30% (30W) and 80% (80W) water in DMSO in agreement with the structured molecular solvent cluster formation. The goethite phase present on the, magnetite nanoparticle surface like a thin passivate layer only was detectable using CV-CPEE, which is a very efficient, cheap, and powerful tool for surface characterization, and it is able to determine the passivate oxyhydroxide or oxide thin layer presence on the nanoparticle surface.