938 resultados para chemically modified silica gel


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Good optical quality Eu3+-doped silica-polyethyleneglycol hybrids were prepared by the sol-gel process. Thermomechanical analysis showed an increase of the glass transition temperature, due to the stiffness of the polymeric network, as the amount of Eu3+ increased. Europium luminescent properties were used to study structural evolution during the sol-gel transition. For lower doping concentrations dried gels present statistical distributions of Eu3+, typical of an amorphous environment, while for higher concentrations a crystalline-like environment of Eu3+ was observed. A broad emission band was observed in the visible part of the electromagnetic spectrum and assigned to the intrinsic emission from the hybrid polymeric network.

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This work describes a modified sol-gel method for the preparation of V 2O 5/TiO 2 catalysts. The samples have been characterized by N 2 adsorption at 77K, x-ray diffractometry (XRD) and Fourier Transform Infrared (FT-IR). The surface area increases with the vanadia loading from 24 m 2 g -1, for pure TiO 2, to 87 m 2 g -1 for 9wt.% of V 2O 5. The rutile form is predominant for pure TiO 2 but became enriched with anatase phase when vanadia loading is increased. No crystalline V 2O 5 phase was observed in the catalysts diffractograms. Two species of surface vanadium observed by FT-IR spectroscopy a monomeric vanadyl and polymeric vanadates, the vanadyl/vanadate ratio remains practically constant.

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The structural characteristics of saturated silica sonogels were studied by means of small-angle x-ray scattering (SAXS) and thermogravimetric analysis (TG), after a long time of aging in saturated conditions. The sonogels were obtained by a sol-gel routine from ultrasound stimulated tetramethoxysilane (TMOS) hydrolysis carried out with the initial water/TMOS molar ratio (r) ranging from 2 to 10. The saturated sonogel structure can be described as composed by mass fractal-like aggregates (clusters) of primary silica particles, all imbibed in a liquid phase. The values of the mass fractal dimension (D) of the clusters was found all around 2.5, while the characteristic size of the clusters (ξ) was found generally increasing with r, going from approximately 2.3 nm (r = 2) to 4.5 nm (r = 10). The volume fraction of the clusters was estimated from the SAXS data. The results were compared to the values of weight loss fraction at the inflection point that has been found in the derivative of the TG curve, which should accounts for the instant in which the meniscus of the liquid phase penetrates into the clusters under a rapid evaporation process as in a TG test.

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The present paper describes the one-pot procedure for the formation of self-assembled thin films of two silanes on the model oxidized silicon wafer, SiO2/Si. SiO2/Si is a model system for other surfaces, such as glass, quartz, aerosol, and silica gel. MALDI-TOF MS with and without a matrix, XPS, and AFM have confirmed the formation of self-assembled thin films of both 3-imidazolylpropyltrimethoxysilane (3-IPTS) and 4-(N- propyltriethoxysilane-imino)pyridine (4-PTSIP) on the SiO2/Si surface after 30 min. Longer adsorption times lead to the deposition of nonreacted 3-IPTS precursors and the formation of agglomerates on the 3-IPTS monolayer. The formation of 4-PTSIP self-assembled layers on SiO2/Si is also demonstrated. The present results for the flat SiO2/Si surface can lead to a better understanding of the formation of a stationary phase for affinity chromatography as well as transition-metal-supported catalysts on silica and their relationship with surface roughness and ordering. The 3-IPTS and 4-PTSIP modified SiO2/Si wafers can also be envisaged as possible built-on-silicon thin-layer chromatography (TLC) extraction devices for metal determination or N-heterocycle analytes, such as histidine and histamine, with on-spot MALDI-TOF MS detection. © 2005 Elsevier Inc. All rights reserved.

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Organo-clay complex of ligand-hexadecyltrimethylammonium with montmorillonite was made for the purpose of application as a preconcentration agent in a chemically modified carbon paste electrode for determination of mercury (II) in aqueous solution. It was found out that the adsorption of Hg(II) by organo-clay complex is independent of the pH of the solution. It was also found out that the adsorption of the remaining metals Cd(II), Ps(II), Cu(II), Zn(II), and Ni(II) was dependent on the changes in pH solutions and increased when it varies from 1 to 8. The resultant material was characterized by cyclic and differential pulse anodic voltammetry using a modified graphite paste electrode in different supporting electrolytes. The mercury response was evaluated with respect to pH, electrode composition, preconcentration time, mercury concentration, possible interferences and other variables.

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A study on the electrochemical behavior of histamine species in aqueous medium is described. A glassy carbon electrode chemically modified with copper (II) hexacyanoferrate (CuHCFe) film and covered with Nafion® film was employed. The interaction between the analyte and the CuHCFe film can be demonstrated by a decrease in both the cathodic and anodic peak currents at 0.68V (vs. Ag/AgCl), attributed to the film and the appearance of new peak current at 0.47V. Cyclic voltammetric parameters obtained for histamine indicate the formation of stable complex between histamine adsorbed at the electrode surface. The dependence of peak currents on the concentration of the analyte is not linear in the employed work range, indicating the presence of a coupled chemical reaction in the electrodic process. © 2010 by ESG.

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The use of chemically modified starches is widely accepted in various industries, with several applications. In this research, natural cassava starch granules were treated with standard sodium hypochlorite solution at 0.8, 2.0, and 5.0 g Cl/100 g starch. The native and modified starch samples were investigated by means of the following techniques: simultaneous thermogravimetry-differential thermal analysis, which allowed us to verify the thermal decomposition associated with endothermic or exothermic phenomena; and differential scanning calorimetry that was used to determine gelatinization enthalpy as well as the rapid viscoamylographic analysis that provided the pasting temperature and viscosity. By means of non-contact-atomic force microscopy method and X-ray powder patterns diffractometry, it was possible to observe the surface morphology, topography of starch granules, and alterations in the granules' crystallinity. © 2012 Akadémiai Kiadó, Budapest, Hungary.

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Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

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