Use of chemically modified silica with beta-diketoamine groups for separation of alpha-lactoalbumin from bovine milk whey by affinity chromatography

Silica gel surface was chemically modified with beta-diketoamine groups by reacting the silanol from the silica surface with 3-aminopropyl-triethoxysilane and 3-bromopentanedione, With this material, copper ions were adsorbed from aqueous solutions, the chemical analysis of the silica-gel-immobilized acetylacetone provided a quantity of 0.67 mmol g(-1) of organic groups attached to the support and 0.63 mmol g(-1) of copper, This material was used as a stationary phase in IMAC (immobilized metal affinity chromatography), to separate alpha-lactoalbumin from bovine milk whey, the results showed an efficient separation in the chromatographic column, the possibility of reutilization of the stationary phase was also investigated. (C) 1997 Academic Press

Small angle X-ray scattering and IR spectroscopy study of metal carbonyl complexes immobilized on a silica gel surface chemically modified with piperazine

The carbonyl complexes [WCl(CO)(3)(bipy) (HgCl)] (1), [Fe(CO)(4)(HgCl)(2)] (2) and W(CO)(6)] (3) were immobilized on a silica gel surface organofunctionalized with piperazine groups. The products obtained were studied by IR spectroscopy and small angle X-ray scattering (SAXS) techniques. The IR data show that the immobilization of heterobimetallic compounds 1 and 2, on the functionalized surface, occurred through the mercury atom, while for 3 the displacement of one CO group by the nitrogen of a piperazine molecule was observed. The data obtained from SAXS indicate that particles have a uniform size and reveal suitable modifications on the functionalized surface after immobilization of metal carbonyl complexes. The average intermolecular distance (l(ij)) for piperazine ligands on support is 8.7 Angstrom, for the metal carbonyl complex 1 it is 18.8 Angstrom, for complex 2 it is 16.2 Angstrom and for complex 3 it is 15.3 Angstrom. Copyright (C) 1996 Elsevier B.V. Ltd

Titania-based organic-inorganic hybrid planar waveguides

Eu3+ -doped titania-silica planar waveguides were prepared from tetraethylorthotitanate (TEOT) and modified silane 3-amino-propyltriethoxysilane (APTS). Films were deposited on borosilicate glass substrates by a dip-coating technique. The refractive index, the thickness and the total attenuation coefficient of the waveguides were measured at 632.8 and 1550 nm by prism coupling technique. Starting from pure titania films, the addition of modified silane leads to a decrease in the refractive index and an increase in thickness. Squared electric field simulation has shown that the light confinement in the waveguide increases with the silane content of the so]. Emission spectra present a broad emission band due to the modified silane and EU emission transitions arising mainly from the D-5(0) level to the F-7(J) (J = 0-4) manifolds. The dependence of transition intensities and excited state lifetimes on the initial composition and also on the heat treatment performed was interpreted in terms of structural changes occurring during the preparation process. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Preparation of new glass systems by the polymeric precursor method for dental applications

Glass ionomer cements (GICs) are largely employed in Dentistry for several applications, such as luting cements for the attachment of crowns, bridges, and orthodontic brackets as well as restorative materials. The development of new glass systems is very important in Dentistry to improve of the mechanical properties and chemical stability. The aim of this study is the preparation of two glass systems containing niobium in their compositions for use as GICs. Glass systems based on the composition SiO2,Al2O3-Nb2O5-CaO were prepared by chemical route at 700degreesC. The XRD and DTA results confirmed that the prepared materials are glasses. The structures of the obtained glasses were compared to commercial material using FTIR, Al-27 and Si-29 MAS-NMR. The analysis of FTIR and MAS-NMR spectra indicated that the systems developed and commercial material are formed by SiO4 and AlO4 linked tetrahedra. These structures are essential to get the set time control and to have cements. These results encourage further applications of the experimental glasses in the formation of GICs. (C) 2004 Elsevier B.V. All rights reserved.

Structural characteristics of silica sonogels prepared with additions of isopropyl alcohol

Wet silica gels with similar to 1.4 x 10(-3) mol SiO2/cm(3) and similar to 92 vol% liquid phase were obtained from sonohydrolysis of tetraethoxysilane (TEOS) with different additions of isopropyl alcohol ( IPA). The IPA/TEOS molar ratio R was changed from 0 to 4. Aerogels were obtained by supercritical CO2 extraction. The samples were analyzed by small-angle X-ray scattering (SAXS) and nitrogen adsorption. The wet gels exhibit mass fractal structure with fractal dimension increasing from D similar to 2.10 to D similar to 2.22, characteristic length xi decreasing from similar to 9.5 to similar to 6.9 nm, as R increases from 0 to 4, and an estimated characteristic length for the primary silica particles lower than similar to 0.3 nm. The supercritical process apparently eliminates a fraction of the porosity, increasing the mass fractal dimension and shortening the fractality domain in the mesopore region. The fundamental role of isopropyl alcohol on the structure of the resulting aerogels is to decrease the porosity and the pore mean size as R changes from pure TEOS to R = 4. A secondary structure appearing in the micropore region of the aerogels can be described as a mass/surface fractal structure, with correlated mass fractal dimension D-m similar to 2.7 and surface fractal dimension D-s similar to 2.3, as inferred from SAXS and nitrogen adsorption data.

Preparation and properties of colloidal particles. Silica on yttrium iron garnet

Various properties of particles can be altered by coating them with a layer of different chemical composition. Yttrium iron garnet (YIG) particles has been coated with silica for control of their sintering, corrosion resistance, and stabilization of magnetic properties. This silica cover was obtained by hydrolysis of tetraethylorthosilicate (TEOS) in 2-propanol. This material was characterized by transmission (TEM) electron microscopy, (XEDS) X-ray energy-dispersive spectrometry, (XPS) X-ray photoemission spectroscopy and (VSM) vibrating sample magnetometry. YIG was heterocoagulated by silica as indicated by TEM micrographies. XPS measurements indicated that only binding energy for silicon and oxygen was found on the silica shell, which confirms that the YIG was covered. The values of the saturation magnetization differ from the heterocoagulated system to well-crystallized YIG.

Structural study of composites of aerosil fumed silica and tetraethoxysilane-derived sonogels

Composites of aerosil fumed silica and tetraethoxysilane-derived sonogel were prepared by changing the aerosil content between 0 and 30wt% with respect to the silica content in the original tetraethoxysilane (TEOS). The structural characteristics were studied by density and Vickers microhardness measurements and analyzed by means of small-angle X-ray scattering (SAXS). The structure of the composite aerosil/TEOS-derived sonogel can be described as inclusions of the aerosil particles embedded in the matrix of the TEOS-derived sonogel, forming an aerosil/matrix interfacial surface inside the composite. The weakening of the bonding of aerosil/matrix interface, as suggested by the reported decrease in microhardness, increases the fracture toughness of the composite. The additive effect of the aerosil particles on the structure of the sonogel accounts for the increase of the bulk density and reduction of the specific surface of the composite. Some internal structure associated with the microclusters making up the sonogels is apparent from systematic deviations from Porod's law found in the system with small aerosil contents. (c) 2005 Elsevier B.V. All rights reserved.

On-line preconcentration and speciation analysis of Cr(III) and Cr(VI) using baker's yeast cells immobilised on controlled pore glass

A study was undertaken to evaluate Saccharonzyces cerevisiae as a substrate for the biosorption of Cr(III) and Cr(VI) aiming to the selective determination of these species in aqueous solutions. The yeast cells were covalently immobilised on controlled pore glass (CPG), packed in a minicolumn and incorporated in an on-line flow injection system. The effect of chemical and physical variables affecting the biosorption process was tested in order to select the optimal analytical conditions for the Cr retention by S. cerevisiae. Cr(III) was retained by the immobilised cells and Cr(VI) were retained by CPG. The speciation was possible by selective and sequential elution of Cr(III) with 0.05 mol L-1 HCl and 2.0 mol L-1 HNO3 for Cr(VI). The influence of some concomitant ions up to 20 mg L-1 was also tested. Quantitative determinations of Cr were carried out by means of inductively coupled plasma optical emission spectrometry (ICP OES). Preconcentration factors of 12 were achieved for Cr(III) and 5 for Cr(VI) when 1.7 mL of sample were processed reaching detection limits of 0.45 for Cr(III) and 1.5 mu g L-1 for Cr(VI). The speciation of inorganic Cr in different kinds of natural waters was performed following the proposed method. Spiked water samples were also analysed and the recoveries were in all cases between 81 and 103%. (c) 2005 Elsevier B.V. All rights reserved.

Effects of self-assembly process of latex spheres on the final topology of macroporous silica

This paper surveys the topology of macroporous silica prepared using latex templates covering the submicrometric range (0.1-0.7 mu m). The behavior of latex spheres in aqueous dispersion has been analyzed by dynamic light scattering (DLS) measurement indicating the most appropriate conditions to form well-defined cubic arrays. The optical behavior of latex spheres has been analyzed by transmittance and reflectance measurements in order to determine their diameter and filling factor when they were assembled in bidimensional arrays. Macroscopic templates have been obtained by a centrifugation process and their crystalline ordering has been confirmed by porosimetry and scanning electron microscopy. These self-assembled structures have been used to produce macroporous silica, whose final topology depends on the pore size distribution of the original template. It has been seen that latex spheres are ordered in a predominant fcc arrangement with slipping of tetragonal pores due to the action of attractive electrostatic interactions. The main effect is to change the spherical shape of voids in macroporous silica into a hexagonal configuration with possible applications to fabricate photonic devices with novel optical properties. (c) 2005 Elsevier B.V. All rights reserved.

Collapse and Color Changes in Grapefruit Juice Powder as Affected by Water Activity, Glass Transition, and Addition of Carbohydrate Polymers

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Upconversion luminescence and thermal effects in terbium-ytterbium codoped fluorogermanate glass-ceramic

Cooperative energy transfer upconversion luminescence is investigated in Tb(3+)/Yb(3+)-codoped PbGeO(3)-PbF(2)-CdF(2) glass-ceramic and its precursor glass under resonant and off resonance infrared excitation. Bright UV-visible emission signals around 384, 415, 438 nm, and 473-490, 545, 587, and 623 nm are identified as due to the (5)D(3)((5)G(6))->(7)F(1) (J=6,5,4) and (5)D(4)->(7)F(1) (J=6,5,4,3) transitions, respectively, and readily observed. The results indicate that cooperative energy transfer between ytterbium and terbium. ions followed by excited state absorption are the dominant upconversion excitation mechanisms involved. Comparison of the upconversion process in a glass-ceramic sample and its glassy precursor revealed that the former present much higher upconversion efficiency. The dependence of the upconversion emission upon pump power, temperature, and doping content is also examined.

Influence of Environmental Conditioning on the Shear Behavior of Poly(phenylene sulfide)/Glass Fiber Composites

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Gelation and drying of weakly bonded silica-PPO nanocomposites

Silica-poly(oxypropylene) (PPO) nanocomposites containing PPO with weak physical bonds between the organic (PPO) and inorganic (silica) phases were obtained by the sol-gel procedure. Three precursor sols containing silica and PPO with molecular weights of 1000, 2000 and 4000g/mol were prepared. The structure changes during the whole sol-gel process, i.e. sol formation, sol-gel transition and gel aging and drying were investigated in situ by small angle X-ray scattering (SAXS). The experimental SAXS curves corresponding to sols and wet gels containing PPO of molecular weight 1000g/mol indicate that the aggregates formed during the studied process are fractal objects. Close to the sol-gel transition and during gel aging the fractal dimension is D=2.5. A clearly different structure evolution occurs in samples prepared with PPO with molecular weights 2000 and 4000 g/mol. Our SAXS results indicate the presence of two coexisting and well-defined structure levels, one of them corresponding to small silica clusters and the other to large silica aggregates. These two levels remain along the whole transformation. The SAXS curves of all dry samples are similar to those of the corresponding wet gels suggesting that no significant changes at nanoscopic scale occur during the drying process.

SAXS study of monodispersed silica nanospheres obtained by an amino acid route

Spherical silica nanoparticles were prepared using a basic amino acid catalysis route and the kinetics of the particles growth was investigated by small angle X-ray scattering (SAXS). L-arginine was used in the polar aqueous phase as the basic catalyst whereas the tetraethylorthosilicate (TEOS) was dissolved in the cyclohexane oil phase as the silicate monomer source. The SAXS measurements were taken in the aqueous phase at different reaction times. A high degree of monodispersity was clearly evidenced for the spherical nanoparticles as a result of the pronounced high-order oscillations observed in the SAXS curves. The SAXS data show that the particles number density remains unchanged since both the particle size as well as the volume fraction gradually increase. This process was discussed based on a reaction-controlled addition of monomer species at the surface of the growing particles. Consequently, the monodispersed spherical nanoparticles radius can as such be finely tuned from 7 to 12 nm by varying the reaction time. (C) 2010 Elsevier B.V. All rights reserved.