Immobilization of pectinmethylesterase from acerola (Malpighia glabra L.) in porous silica

The total and partially purified enzyme pectinmethylesterase from acerola fruit was covalently immobilized on porous silica particles. These efficiency values were 114% for the total PME and 351% for the partially purified PME. In both forms the immobilization resulted in compounds with high thermal stability.

DEVELOPMENT OF A CHEMICALLY MODIFIED ELECTRODE BASED ON CARBON PASTE AND FUNCTIONALIZED SILICA-GEL FOR PRECONCENTRATION AND VOLTAMMETRIC DETERMINATION OF MERCURY(II)

A mercury-sensitive chemically modified electrode (CME) based on modified silica gel-containing carbon paste was developed. The functional group attached to the silica gel surface was 3-(2-thiobenzimidazolyl)propyl, which is able to complex mercury ions. This electrode was applied to the determination of mercury(II) ions in aqueous solution. The mercury was chemically preconcentrated on the CME prior to voltammetric determination by anodic stripping in the differential-pulse mode. A calibration graph covering the concentration range from 0.08 to 2 mg l-1 was constructed. The precision for six determinations of 0.122 and 0.312 mg l-1 Hg(II) was 3.2 and 2.9% (relative standard deviation), respectively. The detection limit for a 5-min preconcentration period was 0.013 mg l-1. A study for foreign ions was also made.

Thermogravimetric investigations during the synthesis of silica-based MCM-41

MCM-41 material was synthesized starting from hydrogel containing colloidal fumed silica, sodium silicate, cetyltetramethylammonium bromide (CTMABr) as surfactant, and distilled water as solvent. These reactants were mixed to obtain a gel with the following composition: 4SiO(2):1Na(2)O:1CTMABr:200H(2)O. The hydrogel with pH=14 was hydrothermally treated at 100 degreesC, for 4 days. Each day, the pH was measured, and then adjusted to 9.5-10 by using 30% acetic acid solution. Thermogravimetry was the main technique, which was used to monitor the participation of the surfactant on the MCM-41 nanophase, being possible to determine the temperature ranges relative to water desorption as well as the surfactant decomposition and silanol condensation.

Luminescence of Eu(III) beta-diketone complex supported on functionalized macroporous silica matrix

This work reports on the photoluminescent properties of the complex diequatris(thenoyltrifluoroacetonate) europium(III), which was adsorbed or supported on tubes of modified surface silica matrix. The luminescence data and the experimental intensity parameter results evidence the existence of high interactions between the complex [Eu(tta)(3)(H2O)(2)] and the modified surface matrix. The anchored complex on macroporous silica shows higher intensity parameter values suggesting that the Eu-0 bond becomes more covalent than the adsorbed one. Therefore, the hypersensitive character of the D-5(0) --> F-7(2) transition increases evidencing a high contribution of the dynamic coupling mechanism possibly due to highly polarizable chemical environments occupied by europium(III) ion. The lifetimes of the complex on silica matrices were measured. (C) 2001 Elsevier B.V. Ltd. All rights reserved.

Er3+/Yb3+ co-activated silica-alumina monolithic xerogels

Monolithic silica xerogels doped with different concentrations of Er3+, Yb3+ and Al3+ were prepared by sol-gel route. Densification was achieved by thermal treatment in air at 950degreesC for 120 h with a heating rate of 0.1degreesC/min. We studied the luminescence properties of the I-4(13/2)-->I-4(15/2) emission band of Er3+ as a function of the Al/Er/Yb concentration and we paid particular attention to the alumina effects. Raman spectroscopy and Vis-NIR absorption were used to monitor the degree of densification of the glasses and the residual OH content.

UV-visible absorption characteristics of TEOS-derived and Cr-doped silica sonogels aged in different pH solutions and heat treated up to 600 degrees C

Cr-doped xerogels were obtained by sol-gel process from the acid-catalyzed and ultrasound-stimulated hydrolysis of tetraethoxysilane (TEOS) with addition of CrCl3.6H(2)O in water solution during the liquid step of the process. The gels were aged immersed in different pH solutions for about 30 days, after that they were allowed to dry. The samples were annealed at temperatures ranging from 40 to 600degreesC and analyzed by UV-visible absorption spectroscopy. Cr3+ is the preferable oxidation state of the chromium ion in the gels annealed up to 250-300degreesC, in the case of aging in solutions of pH=5 and 11. A high UV absorption below similar to320 nm, due to the host gel, and different absorption bands, depending on the temperature, due to the chromium ion were observed in the xerogels at temperatures below similar to250degreesC, in the case of aging in solutions of pH=1 and 2. These absorption bands have not been assigned. Above 300degreesC up to 600degreesC, Cr5+, and possibly Cr6+, are the preferable oxidation states of the chromium ion independent of the pH of the aging solution, so the xerogels turn to a yellowish appearance in all cases.

Functionalized silica synthesized by sol-gel process

This work considers some aspects of the chemistry involved in the preparation and description of silicon oxide functionalized by sol-gel process. In this work we studied the synthesis and measured the properties of silicon oxide functionalized with 3-chloropropyl, through a sol-gel process. Thermogravimetic analysis, infrared spectra, and elemental analyses were measured. The samples were prepared in the following proportions of tetraethylorthosilicate (TEOS): 3-chloropropyl trimethoxisilane molar ratio: 1:0, 1:1, 2:1, 3:1 and 4:1. The thermogravimetric data for the resulting materials established the 'minimum formulae' 2:0, 3:1, 4.1, 7:1 and 11:1, respectively. As expected, the relative amount of water is inversely proportional to the presence of propyl groups. Infrared data show Si-C and -CH2-vibration modes at 1250 to 1280 and 2920 to 2940 cm(-1), respectively. Thermogravimetric data and infrared spectra showed that inorganic polymers contained organic polymers. (C) 1999 Elsevier B.V. B.V. All rights reserved.

Investigation of the systems silica and silica containing chromium in alcohol medium

The purpose of this work is to obtain micrometer sized spherical particles of silica and silica-chromium from sodium silicate. Spherical particles were prepared by sol-gel method from hydrolysis to polycondensation of aqueous sodium silicate in alcohol medium. Chromium was added to the system for some samples. Compositions and morphologies were achieved by changing the precipitation agent. X-ray diffractometry, electrophoretic mobility, infrared spectroscopy and scanning electron microscopies were carried out on these particles to identify phases, determine particle mobility, morphology, particle sizes, shapes and order at short distance. Non-crystalline silica particles with spherical shapes and micrometric size were obtained. The surface potentials of the silica particles differed from that of the silica-chromium particles. (C) 1999 Elsevier B.V. B.V. All rights reserved.

Preparation and characterization of spherical silica-porphyrin catalysts obtained by the sol-gel methodology

This work describes the synthesis of a first-generation iron porphyrin catalyst entrapped in a silica matrix by the sol-gel route, leading to spherical particles. The catalyst was synthesized by the method of Stober, through hydrolysis and condensation of the alkoxysilane TEOS in a mixture of alcohol, water and ammonia, in the presence of the iron porphyrin Fe(TPP)Cl. The relation between particle morphology and catalytic activity of the different Fe(TPP)-SiO2, obtained using different H2O/silane molar ratios and ammonia concentrations in the xerogel syntheses, was studied.The obtained catalysts were characterized by UV-vis spectroscopy, NMR Si-29. thermogravimetric analysis and transmission electron microscopy. Their ability to catalyze (Z)-cyclooctene epoxidation and cyclohexane oxidation was tested using iodosylbenzene as oxygen donor; the oxidation products were analyzed by gas chromatography and the catalysts obtained in a form of particles spherical and monodispersed showed to be a promising catalytic system for selective oxidation. (c) 2005 Elsevier B.V. All rights reserved.

Montmorillonite (MMT) effect on the structure of poly(oxyethylene) (PEO)-MMT nanocomposites and silica-PEO-MMT hybrid materials

In this work we report the effects of incorporation of variable amounts (0.5-25%w/w) of montmorillonite in poly(oxyethylene) based materials in order to decrease the polymer crystallinity. Two different classes of materials were studied: silica-poly(oxyethylene)-montmorillonite hybrids prepared by the sol-gel route and poly(oxyethylene)-montmorillonite nanocomposites prepared by mixing the dry clay or the clay aqueous suspension into the melt poly(oxyethylene). The effects of monternorillonite loading on the poly(oxyethylene) crystallization control and on the nanostructural features were investigated by X-ray powder diffraction, small-angle X-ray scattering and differential scanning calorimetry. Experimental results show that free montmorillonite layers coexist with open aggregates and tactoids in the poly(oxyethylene)-montmorillonite nanocomposites, with different features depending on the filler proportion and preparation route. The intercalation of polymer chains in montmorillonite galleries markedly hinders the crystallization of the poly(oxyethylene) matrix. For hybrids materials the silica phase favors the exfoliation of montmorillonite tactoids, so that samples are predominantly constituted by dispersed platelets. (c) 2006 Elsevier B.V. All rights reserved.

A nonisothermal study of the kinetics of the nanoporosity elimination in sonogels-derived silica xerogels

A nonisothermal study of the kinetics of the nanoporosity elimination in monolithic silica xerogels, prepared from acid and ultrasound catalyzed hydrolysis of tetraethylortosilicate (TEOS), has been carried out by means of in situ linear shrinkage measurements performed with different heating rates. The study could be applied up to almost alpha similar to 0.6 of the volume fraction alpha of eliminated pores. The activation energy was found increasing from about 3.2 x 10(2) kJ/mol for alpha similar to 0.06 up to about 4.4 x 10(2) kJ/mol for alpha. similar to 0.44. The sintering process accompanying the nanopore elimination in this set of xerogels is in agreement with a viscous flux sintering process with the hydroxyl content diminishing with the volume fraction of eliminated pores. All the volume fraction of eliminated pores versus temperature (T) curves can be matched onto a unique curve with an appropriate rescaling of the T axis, independent of the heating rate. This scaling property suggests that the path of sintering seems the same, regardless of the heating rate; the difference is that the rate is faster at higher temperature.

Er-doped silica-based waveguides prepared by different techniques: RF-sputtering, sol-gel and ion-exchange

Erbium-activated silica-based planar waveguides were prepared by three different technological routes: RF-sputtering, sol-gel and ion exchange. Various parameters of preparation were varied in order to optimize the waveguides for operation in the NIR region. Particular attention was devoted to the minimization of the losses and the increase of the luminescence efficiency of the metastable I-4(13/2) state of the Er3+ ion. Waveguide properties were determined by m-line spectroscopy and loss measurements. Waveguide Raman and luminescence spectroscopy were used to obtain information about the structure of the prepared films and about the dynamical processes related to the luminescence of the Er3+ ions.

SAXS study of gelation, aging and drying of silica-polypropyleneglycol hybrid materials

New silica-polypropyleneglycol ormosils (organically modified silicates) with covalent bends between the organic (polymer) and inorganic (silica) phases have been prepared by the sol-gel process. Their structural evolution during sol formation, sol-gel transition, gel aging and drying has been studied in situ by small-angle X-ray scattering (SAXS). The experimental SAXS curves corresponding to sols and gels exhibit features expected from fractal objects. Clusters of size around 55 Angstrom with an initial fractal dimension D = 2.4 are formed in the sol. They are constituted of small primary silica particles chemically crosslinked at the end of the polymer chains. A strong liquid-like spatial correlation between the silica particles develops during drying due to the shrinkage of the polymeric network induced by water and ethanol evaporation. The continuous increase in SAXS intensity during drying, while the interparticle distance remains constant, is a consequence of the progressive growth of the dry fraction of the total volume. After drying, the gel structure consists of a rather compact arrangement of silica particles embedded in the polypropyleneglycol matrix.

Effects of different treatments on purity of silica from soluble sodium silicate

Noncrystalline silica was obtained with low iron, sodium, and nitrate ions concentrations from soluble sodium silicate (water glass) and nitric acid solution. Extractions with nitric acid solution and/or deionized water and/or dialysis were carried out to eliminate soluble metal ions. Products were dried in a microwave oven and characterized by chemical analysis, XRD, and IR. Dialysis seems to be the best treatment for the elimination of sodium and nitrate ions. Silica purified by nitric acid and water extractions followed by dialysis yields the purest silica sample.