Synthesis of manganese porphyrinosilica imprinted with templates using the sol-gel process

The optimized conditions for the preparation of a new manganese porphyrinosilica-template material are reported. The manganese porphyrinosilica-template was prepared by the sol-gel process, by the reaction of -SO2Cl groups present in the phenyl rings of MnTDC(SO2Cl)PPCl with 3-aminopropyltriethoxysilane. The reaction produces a precursor porphyrinopropylsilyl species, which were then polymerized with tetraethoxysilane. The presence of manganese porphyrin on xerogel is confirmed by ultraviolet visible absorption spectroscopy and thermogravimetric analysis (TGA). The prepared materials have surface areas between 19 and 674 m2 g-1. Electron spectroscopy imaging of the materials show that manganese distribution in the xerogel is uniform. Both manganese(III) porphyrinosilica-template and a similar iron(III) porphyrinosilica-template can catalyze the epoxidation of cyclooctene using iodozylbenzene as oxygen donor. The metalloporphyrinosilica-template presents catalytic activity similar to that of metaloporphyrin in solution. © 2000 Elsevier Science B.V. All rights reserved.

A surface modification for hydrogen storage intermetallic particles by sol-gel method

A new process for the surface modification of hydrogen storage intermetallic particles used as anode material in secondary batteries is proposed in this article. The copper oxide particles coverage obtained by the sol-gel method is proposed to produce, under operational conditions of a Ni-MH battery, a metallic framework that tolerates the volume changes in charge/discharge cycles and does not inhibit the hydrogen absorption. Furthermore it was noticed an enhancement on the discharge capacity of the electrode material that can be related to a new hydrogen storage phase or to an inhibition of the surface oxidation promoted by the film coverage.

Caracterização textural e estrutural de V 2O 5/TiO 2 obtidos via sol-gel: Comparação entre secagem convencional e supercrítica

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.

Contribution of oxygen related defects to the electronic transport in SnO2 sol-gel films

SnO2 deposited by sol-gel is a polycrystalline film with small grain size. Oxygen present at a less grain boundary traps electrons and then the depletion layer around the potential barrier of the grain boundary becomes wider, comparable to the grain size. We have modeled the conductivity taking into account the trapped charge at the depletion layer of the grain boundary and other scattering mechanisms such as ionized impurity and polar optical. Experimental data of photoconductivity of SnO2 sol-gel films are simulated considering the dominant scattering at grain boundary and crystallite bulk. The fraction of trapped charge at the grain boundary depends on temperature and wavelength of irradiating light, being as high as 50% for illumination in the range 500-600 nm for SnO2-2%Nb as grown sample annealed in air to 550°C. This fraction can be quite reduced depending on exposure to light and annealing under different oxygen partial pressure conditions.

Effects of bleaching with carbamide peroxide gels on microhardness of restoration materials

The objective of this in vitro study was to quantitatively assess the effects of bleaching with 10 and 15% carbamide peroxide (CP) on restoration materials by performing superficial microhardness analysis. Acrylic cylindrical containers (4 x 2 mm) were filled with the following restoration products: Charisma (Heraues Kulzer, Vila Santa Catarina, São Paulo, Brazil), Durafill VS (Heraeus Kulzer), Vitremer (3M, Sumaré, São Paulo, Brazil), Dyract (Dentsply, Petrópolis, Rio de Janeiro, Brazil), and Permite C (SDI, São Pauio, São Paulo, Brazil). Sixty samples were prepared of each restoration material. Twenty samples received bleaching treatment with 10% CP, 20 samples received bleaching treatment with 15% CP, and 20 samples were kept submerged in artificial saliva, which was replaced daily. The treatment consisted of immersion of the specimens in 1 cm3 of CP at 10 and 15% for 6 hours per day during 3 weeks, whereupon the test specimens were washed, dried, and kept immersed in artificial saliva for 18 hours. Then the test and control specimens were analyzed using a microhardness gauge. The Knoop Hardness Number (KHN) was taken for each test and control specimen at five different locations by applying a 25 g force for 20 seconds. The values obtained were transformed into KHNs and the mean was calculated. The data were submitted to statistical analysis by analysis of variance and Tukey test, p < .05. The means/standard deviations were as follows: Charisma: CP 10% 38.52/4.08, CP 15% 34.31/6.13, saliva 37.36/4.48; Durafill VS: CP 10% 18.65/1.65, CP 15% 19.38/2.23, saliva 18.27/1.43; Dyract AP: CP 10% 30.26/2.81, CP 15% 28.64/5.44, saliva 33.88/3.46; Vitremer: CP 10% 28.15/3.04, CP 15% 17.40/3.11, saliva 40.93/4.18; and Permite C: CP 10% 183.50/27.09, CP 15% 159.45/5.78, saliva 215.80/26.15. A decrease in microhardness was observed for the materials Dyract AP, Vitremer, and Permite C after treatment with CP at 10 and 15%, whereas no effect on either of the two composites (Charisma and Durafill) was verified. CLINICAL SIGNIFICANCE: The application of the carbamide peroxide gels at 10 and 15% did not alter the microhardness of the composite resins Charisma and Durafill. In situ and clinical studies are necessary to enable one to conclude that the reduction in microhardness of the materials effectively results in clinical harm to the restorations.

Comparative study using small-angle x-ray scattering and nitrogen adsorption in the characterization of silica xerogels and aerogels

A comparative study using small-angle x-ray scattering (SAXS) and nitrogen adsorption has been carried out in the structural characterization of silica xerogels and aerogels, obtained from tetraethoxysilane sonohydrolysis. The specific surface and the mean pore size as measured by both the techniques were found to be in notable agreement in all cases for aerogels and xerogels. According to the SAXS data, aerogels at 500 °C exhibit a mass fractal structure with fractal dimension D∼2.4 in the range between the correlation length ξ∼5.3 nm and a∼0.75 nm. An experimental method to probe the mass fractal structure of aerogels from exclusively nitrogen adsorption isotherms has been presented. For aerogels at 500 °C, we have found D∼2.4 in the range between the pore width 2rξ∼33 nm and 2ra∼4.5 nm, which is in notable agreement with the SAXS results (D ∼2.4, ξ∼5.3 nm, a∼0.75 nm) if we assign the pore width 2r probed by the Kelvin equation in the adsorption method to the Bragg distance 2π/q associated to the correlation length 1/q probed by SAXS.

Small-angle x-ray scattering study of the structural evolution of the drying of sonogels with the liquid phase exchanged by acetone

The structural evolution on the drying of wet sonogels of silica with the liquid phase exchanged by acetone, obtained from tetraethoxisilane sonohydrolysis, was studied in situ by small-angle x-ray scattering (SAXS). The periods associated to the structural evolution as determined by SAXS are in agreement with those classical ones established on basis of the features of the evaporation rate of the liquid phase in the obtaining of xerogels. The wet gel can be described as formed by primary particles (microclusters), with characteristic length a ∼ 0.67 nm and surface which is fractal, linking together to form mass fractal structures with mass fractal dimension D=2.24 in a length scale ξ∼6.7 nm. As the network collapses while the liquid/vapor meniscus is kept out of the gel volume, the mass fractal structure becomes more compacted by increasing D and decreasing ξ, with smoothing of the fractal surface of the microclusters. The time evolution of the density of the wet gels was evaluated exclusively from the SAXS parameters ξ, D, and a. The final dried acetone-exchanged gel presents Porod's inhomogeneity length of about 2.8 nm and apparently exhibits an interesting singularity D →3, as determined by the mass fractal modeling used to fit the SAXS intensity data for the obtaining of the parameters ξ and D.

Effects of five carbamide peroxide bleaching gels on composite resin microhardness.

The purpose of this study was to evaluate the effects of five home bleaching products containing 15-16% carbamide peroxide on the microhardness of microhybrid composite resin Z-250 (3M/Espe). A total of 72 specimens were fabricated in cylindrical acrylic matrices (4 x 2 mm), filled with composite resin and photo-activated for 40 seconds. They were divided in 6 study groups (n = 12), according to the bleaching product: Review (SS White), Magic Bleaching (Vigodent), Opalescence (Ultradent), Whiteness Perfect (FGM), Claridex (Biodinâmica), and a control group (not bleached). Specimens were exposed to 1 cc of bleaching gel for 6 hours daily for 2 weeks. The control group specimens were kept in artificial saliva throughout this time. All the specimens were then analyzed in a microhardness tester. Knoop hardness measurements were performed, and the results were submitted to parametric statistical analysis (analysis of variance and Tukey's test). Mean Knoop values and standard deviation were: baseline, 68.52a (4.28); control, 63.42b (7.16); Whiteness Perfect, 57.57c (1.81); Magic Bleaching, 57.22c (3.84); Opalescence, 57.03cd (4.00); Claridex, 53.64de (3.33); Review 51.45e (2.82). Identical letters mean statistical equality according to Tukey's test at the 5% significance level. The products significantly decreased Z-250 (3M/Espe) microhardness.

Utilização de componentes principais para analisar o comportamento do cafeeiro a pleno sol e sombreado

The aim of this work is to describe the behavior of coffee (Coffea arabica L.) grown for nine years under organic management systems in full sun and shaded by banana trees (Musa sp.) and Erythrina verna Vell., in Valença, RJ. We performed a joint evaluation of vegetative characteristics, nutritional content and yield, with the aid of a principal component analysis. Twelve treatments were arranged in a randomized block design with four replications in a split plot. The plots evaluated farming systems in full sun and shade, and the subplots consisted of the following varieties of coffee: Tupi IAC 1669-33, MG 6851, IAC 3282 Icatu, Catucaí 2SL, Obatã IAC 1669-20; lineage IAC IAC 144. After five years we assessed the following variables, height, stem and canopy diameter, leaf area, number of branches, number of nodes per branch, number of leaves present, the distance between nodes, the percentage of green,ripe and dried fruit, number of dead plants, number of plants with death of the apical bud, coffee yield, and foliar concentrations of N, P, K, Ca and Mg. A multivariate analysis efficiently discriminates the variables in full sun and shaded cropping systems. Shading increases the percentage of green fruit, leaf area, height, diameter, distance between nodes, number of leaves on the branches, number of branches and leaf N content, but does not reduce the level of productivity when the shade is adequate.

Antibacterial activity of gels with pomegranate, apricot and green tea glycolic extracts

Pomegranate (PGE) and green tea (GTGE) glycolic extracts are being employed in formulations because of their antiseptic and astringent effects. Apricot (AGE) glycolic extract possesses function cooling and antibacterial. The aim was to verify the antibacterial activity of these extracts incorporated in gel base. The antibacterial activity was verified by diffusion in agar method, using cylinder in plate. Plates containing Staphylococcus aureus (ATCC 6538p), Pseudomonas aeruginosa (ATCC 27853), Escherichia coli (ATCC 10536) and Salmonella sp. (ATCC 19196) were incubated at 37°C for 24 hours. After incubation, the results were analysed with a pachymeter, observing the bacterial growth inhibition halo diameter and the statistical significance level was determined. PGE presented activity only against P. aeruginosa; GTGE presented activity against S. aureus, P. aeruginosa and E. coli; and AGE presented activity against P. aeruginosa and Salmonella sp. According to the experimental conditions, it is possible to conclude that GTGE presented the greater growth inhibition halo diameter when compared with other extracts, suggesting higher antibacterial action of this extract.

Bleaching gels containing calcium and fluoride: Effect on enamel erosion susceptibility

This in vitro study evaluated the effect of 35 hydrogen peroxide (HP) bleaching gel modified or not by the addition of calcium and fluoride on enamel susceptibility to erosion. Bovine enamel samples (3 mm in diameter) were divided into four groups (n = 15) according to the bleaching agent: control-without bleaching (C); 35 hydrogen peroxide (HP); 35 HP with the addition of 2 calcium gluconate (HP + Ca); 35 HP with the addition of 0.6 sodium fluoride (HP + F). The bleaching gels were applied on the enamel surface for 40 min, and the specimens were subjected to erosive challenge with Sprite Zero and remineralization with artificial saliva for 5 days. Enamel wear was assessed using profilometry. The data were analyzed by ANOVA/ Tukey's test (P 0.05). There were significant differences among the groups (P = 0.009). The most enamel wear was seen for C (3.37 ± 0.80 μm), followed by HP (2.89 ± 0.98 μm) and HP + F (2.72 ± 0.64 μm). HP + Ca (2.31 ± 0.92 μm) was the only group able to significantly reduce enamel erosion compared to C. The application of HP bleaching agent did not increase the enamel susceptibility to erosion. However, the addition of calcium gluconate to the HP gel resulted in reduced susceptibility of the enamel to erosion. © 2012 Alessandra B. Borges et al.

TiO2-Cu photocatalysts: A study on the long- and short-range chemical environment of the dopant

In this study, the short- and long-range chemical environments of Cu dopant in TiO2 photocatalyst have been investigated. The Cu-doped and undoped TiO2 specimens were prepared by the sol-gel approach employing CuSO4·5H2O and Ti(O-iPr)4 precursors and subjecting the dried gels to thermal treatment at 400 and 500 C. The photocatalytic activity, investigated by methylene blue degradation under sunlight irradiation, showed a significantly higher efficiency of Cu-doped samples than that of pure TiO2. The X-ray diffraction results showed the presence of anatase phase for samples prepared at 400 and 500 C. No crystalline CuSO4 phase was detected below 500 C. It was also found that doping decreases the crystallite size in the (004) and (101) directions. Infrared spectroscopy results indicated that the chemical environment of sulfate changes as a function of thermal treatment, and UV-vis spectra showed that the band gap decreases with thermal treatment and Cu doping, showing the lowest value for the 400 C sample. X-ray absorption fine structure measurements and analysis refinements revealed that even after thermal treatment and photocatalytic assays, the Cu2+ local order is similar to that of CuSO4, containing, however, oxygen vacancies. X-ray photoelectron spectroscopy data, limited to the near surface region of the catalyst, evidenced, besides CuSO4, the presence of Cu1+ and CuO phases, indicating the active role of Cu in the TiO2 lattice. © 2013 Springer Science+Business Media New York.

Liquid foam templates associated with the sol-gel process for production of zirconia ceramic foams

The unique properties of ceramic foams enable their use in a variety of applications. This work investigated the effects of different parameters on the production of zirconia ceramic foam using the sol-gel process associated with liquid foam templates. Evaluation was made of the influence of the thermal treatment temperature on the porous and crystalline characteristics of foams manufactured using different amounts of sodium dodecylsulfate (SDS) surfactant. A maximum pore volume, with high porosity (94%) and a bimodal pore size distribution, was observed for the ceramic foam produced with 10% SDS. Macropores, with an average size of around 30 μm, were obtained irrespective of the SDS amount, while the average size of the supermesopores increased systematically as the SDS amount was increased up to 10%, after which it decreased. X-ray diffraction analyses showed that the sample treated at 500 °C was amorphous, while crystallization into a tetragonal metastable phase occurred at 600 °C due to the presence of sulfate groups in the zirconia structure. At 800 and 1000 °C the monoclinic phase was observed, which is thermodynamically stable at these temperatures. © 2013 by the authors; licensee MDPI, Basel, Switzerland.

Atividade antioxidante dos extratos de shiitake (Lentinus edodes) e de cogumelo do sol (Agaricus blazei) aplicados em óelo de soja sob aquecimento

Pós-graduação em Engenharia e Ciência de Alimentos - IBILCE