Structural and Luminescence Properties of Silica-Based Hybrids Containing New Silylated-Diketonato Europium(III) Complex

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

Design of novel iron compounds as potential therapeutic agents against tuberculosis

In the search for new therapeutic tools against tuberculosis two novel iron complexes, [Fe(L-H)3], with 3-aminoquinoxaline-2-carbonitrile N(1),N(4)-dioxide derivatives (L) as ligands, were synthesized, characterized by a combination of techniques, and in vitro evaluated. Results were compared with those previously reported for two analogous iron complexes of other ligands of the same family of quinoxaline derivatives. In addition, the complexes were studied by cyclic voltammetry and EPR spectroscopy. Cyclic voltammograms of the iron compounds showed several cathodic processes which were attributed to the reduction of the metal center (Fe(III)/Fe(II)) and the coordinated ligand. EPR signals were characteristic of magnetically isolated high-spin Fe(III) in a rhombic environment and arise from transitions between m(s) = +/- 1/2 (geff-9) or m(s) = +/- 3/2 (g(eff)similar to 4.3) states. Mossbauer experiments showed hyperfine parameters that are typical of high-spin Fe(III) ions in a not too distorted environment. The novel complexes showed in vitro growth inhibitory activity on Mycobacterium tuberculosis H(37)Rv (ATCC 27294), together with very low unspecific cytotoxicity on eukaryotic cells (cultured murine cell line J774). Both complexes showed higher inhibitory effects on M. tuberculosis than the "second-line" therapeutic drugs. (C) 2010 Elsevier B.V. All rights reserved.

Characterization of the colloidal products of pentacarbonyliron oxidation

Pentacarbonyliron was oxidized with H2O2, in organic solvents, to give colloidal sols. The aqueous-ethanolic sol is highly stable and undergoes thermally-reversible coagulation. Its solid phase was found to be a non-crystalline Fe (III) hydroxoacetate which is transformed to α-Fe2O3 when heated to 300°C. Iron-bound acetate groups are assumed to have a major role in the sol stability, by preserving the amorphous solid phase. Dry hydroxoacetate particles were heated under vacuum; scanning electron microscopy revealed that these particles coalesce and grow, as in a sintering process but at low temperatures (100-250°). © 1987.

Gold-bearing iron duricrust in Central Brazil

In the Cuiabá region-State of Mato Grosso, Central Brazil-primary gold mineralization is hosted by two generations of quartz veins in Precambrian metamorphic terrains of the Cuiabá Group. Gold is mined from the veins and mainly from the eluvial horizons that cover the deeply altered basement. In the lodes gold occurs as small particles (less than 1 mm) associated with pyrite and contains up to 5% Ag. Larger particles and nuggets of almost pure gold are found in the iron duricrust which caps the upper levels of the weathering profile. It is difficult to determine the average grade of this kind of deposit but some prospects in the Cuiabá region produce up to 2 g gold per ton of ore. Lateritization is responsible for both the formation of the iron crust and the concentration of gold within the regolith. Under a tropical climate, the supergene alteration of phyllites of the Cuiabá Group has led to the formation of a weathering profile consisting typically of saprolite, mottled clay zone and duricrust, from bottom to top. The duricrust is directly derived form the in situ weathering of phyllites. Geochemical balance calculations indicate that in the transition from the saprolite to the duricrust lateritization has promoted a progressive loss of Si, Al and K, and more than 500% of absolute Fe enrichment. Gold underwent a supergene evolution related to the development of the weathering profile. In the saprolite and mottled clay zone, associated with quartz and oxidized sulfides, gold dissolves as demonstrated by corrosion features at the surface of the particles. The formation of secondary gold in the duricrust is indicated by the larger size of the nuggets, their higher fineness and the close relationship between gold and the neoformed iron oxy-hydroxides. © 1991.

Morphological evolution of zinc oxide originating from zinc hydroxide carbonate

Zinc oxide can be obtained by thermal decomposition of hydrozincite, a topochemical reaction. This work reports the relation between zinc oxide morphology and the precursor zinc hydroxide carbonate precipitation time. The morphological evolution was monitored by SEM, IR and XRD. Zinc oxide obtained from initially precipitated hydrozincite consists of porous spherical aggregates and shows a single Zn-O IR vibrational band. At longer periods of precipitation time the aggregates were transformed into spherulitic-shaped zinc oxide particles showing the Zn-O split vibrational band. X-ray patterns show that the hexagonal zinc oxide phase is substantially increased as a function of hydrozincite precipitation time. © 1997 Elsevier Science S.A.

Preparation and characterization of spherical yttrium iron garnet via coprecipitation

The purpose of this work is to obtain spherical particles yttrium iron garnet (YIG) by coprecipitation technique. The spherical particles were obtained from either nitrate or chloride salt solutions by controlling the precipitation medium. Different agents of dispersion such as PVP and ammonium iron sulfate were used to optimize the shape and size of YIG. Samples were characterized by X-ray diffraction, scanning electron microscopy and vibrating sample magnetometry. The results show that the samples phase transition takes place at 850°C (orthorhombic phase) and at 1200°C (cubic phase). Spherical shape particles, with diameter of around 0.5 μm, present magnetization values close to the bulk value (26 emu g -1). © 2001 Elsevier Science B.V. All rights reserved.

Yttrium iron garnet heterocoagulated by silica

Coated purpose of homogeneous distribution as a second phase is introduced in magnetic systems. Yttrium iron garnet (YIG) shows special interest as magnetic dye, microwave absorber, and magnetic fluids when heterocoagulated by other material. Surface and interface magnetic properties are intimately connected with the new properties of the silica on YIG system. Néel first introduced the concept of surface anisotropy, and Chen et al. developed a model that describes the anisotropy effects at the boundary surface particle, which was applied in this work. Spherical YIG particles were prepared by coprecipitation method and coated with silica using the tetraethylorthosilicate (TEOS) hydrolysis process. The silica-YIG boundary was investigated by transmission electron microscopy. Hysteresis loops comparatively show the profile of the naked and silica-covered YIG particles. The surface anisotropies were calculated using the Chen et al. approach. Indeed, in heterocoagulation systems, the surface anisotropy is a result of the interface symmetry breaking, as observed.

Electrocatalytic and voltammetric determination of sulfhydryl compounds through iron nitroprusside modified graphite paste electrode

Iron nitroprusside Fe(II)NP was incorporated into a carbon paste electrode and the electrochemical studies were performed with cyclic voltammetry. The cyclic voltammogram of Fe(II)NP exhibits two redox couple with formal potential (E0')1 = 0.24 e (E0')2 = 0.85 V vs SCE attributed to Fe(II)/Fe(II) and Fe (II)(CN)5NO/Fe(III)(CN)5NO, respectively. The redox couple with (E0')2 = 0.85 V presents an electrocatalytic response for sulfhydryl compounds. The electrocatalytic oxidation of sulfhydryl compounds by the mediator has been used for the determination of L-cysteine and N-acetylcysteine. The modified graphite paste electrode gives a linear range from 9.2 x 10-4-2.0 x 10-2;; 9.6 x 10-4-1.4 x 10-2mol L-1 for the determination of L-cysteine and N-acetylcysteine, respectively, with detection limit of 1.9 x 10-4 mol L-1;; 1.5 x 10 -4 mol L-1 and relative standard desviations ± 5% and 1.5 x 10-3 mol L-1 ± 4% (n=3). The amperometric sensitivities are 0.024 and 0.027 μA/μmol L-1 for L-cysteine and N-acetylcysteine, respectively. The application of this electrode was tested and a commercial pharmaceutical product (Fluimucil) has been determined.

Evaluation of the diffusion capacity of calcium hydroxide pastes through the dentinal tubules

This study aimed to evaluate the diffusion capacity of calcium hydroxide pastes with different vehicles through dentinal tubules. The study was conducted on 60 extracted single-rooted human teeth whose crowns had been removed. The root canals were instrumented and divided into 4 groups according to the vehicle of the calcium hydroxide paste: Group I - distilled water; Group II - propylene glycol; Group III - 0.2% chlorhexidine; Group IV - 2% chlorhexidine. After placement of the root canal dressings, the teeth were sealed and placed in flasks containing deionized water. After 1, 2, 7, 15, 30, 45 and 60 days, the pH of the water was measured to determine the diffusion of calcium hydroxide through the dentinal tubules. The data were recorded and statistically compared by the Tukey test. The results showed that all pastes presented a similar diffusion capacity through dentin. Group IV did not present difference compared to group I. Group II presented difference compared to the other groups, as did Group III. In conclusion, groups I and IV presented a better diffusion capacity through dentin than groups II and III; 2% chlorhexidine can be used as a vehicle in calcium hydroxide pastes. © 2009 Sociedade Brasileira de Pesquisa Odontológica.

Response of human dental pulp to calcium hydroxide paste preceded by a corticosteroid/antibiotic dressing agent

Aim: To evaluate the treatment with corticosteroid/antibiotic dressing in pulpotomy with calcium hydroxide. Methods: Forty-six premolars were pulpotomized and randomly assigned into 3 groups. In Group I pulpal wound was directly capped with calcium hydroxide, and Group II and Group III received corticosteroid/antibiotic dressing for 10 min or 48 h, respectively, before pulp capping. Teeth were processed for histological analysis after 7, 30 or 60 days to determine inflammatory cell response, tissue disorganization, dentin bridge formation and presence of bacteria. Attributed scores were analyzed by Kruskal-Wallis and Mann-Whitney tests (α=0.05). Results: On the 7th day, all groups exhibited dilated and congested blood vessels in the tissue adjacent to pulpal wound. The inflammatory cell response was significantly greater in Group III (p<0.05). On the 30th day, in all groups, a thin dentin matrix layer was deposited adjacent to the pulpal wound and a continuous odontoblast-like cell layer underlying the dentin matrix was observed. On the 60th day, all groups presented a thick hard barrier characterized by an outer zone of dystrophic calcification and an inner zone of tubular dentin matrix underlined by a defined odontoblast-like cell layer. Conclusions: Within the limitations of present study, considering that the treatment was performed in healthy teeth, it may be concluded that the use of a corticosteroid/antibiotic dressing before remaining tissue protection with calcium hydroxide had no influence on pulp tissue healing.

Computer techniques towards the automatic characterization of graphite particles in metallographic images of industrial materials

The automatic characterization of particles in metallographic images has been paramount, mainly because of the importance of quantifying such microstructures in order to assess the mechanical properties of materials common used in industry. This automated characterization may avoid problems related with fatigue and possible measurement errors. In this paper, computer techniques are used and assessed towards the accomplishment of this crucial industrial goal in an efficient and robust manner. Hence, the use of the most actively pursued machine learning classification techniques. In particularity, Support Vector Machine, Bayesian and Optimum-Path Forest based classifiers, and also the Otsu's method, which is commonly used in computer imaging to binarize automatically simply images and used here to demonstrated the need for more complex methods, are evaluated in the characterization of graphite particles in metallographic images. The statistical based analysis performed confirmed that these computer techniques are efficient solutions to accomplish the aimed characterization. Additionally, the Optimum-Path Forest based classifier demonstrated an overall superior performance, both in terms of accuracy and speed. © 2012 Elsevier Ltd. All rights reserved.

Estudos da preparação de superfície da liga AA6063T5 e do desenvolvimento de revestimentos híbridos orgânico-inorgânicos a base de siloxano-PMMA para aplicação anticorrosiva

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Desenvolvimento de metodologias eletroanalíticas para determinação de potássio e fósforo em biodiesel

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Nanopartículas magnéticas de 'FE''CO'@'AU': preparação, caracterização e funcionalização com complexo de 'RU'(II) luminescente

Pós-graduação em Química - IQ

Structural, electronic and optical properties of Fe(III) complex with pyridine-2,6-dicarboxylic acid: A combined experimental and theoretical study

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