Photolumiscent Properties of Nanorods and Nanoplates Y2O3:Eu3+

Nanorods and nanoplates of Y2O3:Eu3+ powders were synthesized through the thermal decomposition of the Y(OH)(3) precursors using a microwave-hydrothermal method in a very short reaction time. These powders were analyzed by X-ray diffraction, field emission scanning electron microscopy, Fourrier transform Raman, as well as photoluminescence measurements. Based on these results, these materials presented nanoplates and nanorods morphologies. The broad emission band between 300 and 440 nm ascribed to the photoluminescence of Y2O3 matrix shifts as the procedure used in the microwave-hydrothermal assisted method changes in the Y2O3:Eu3+ samples. The presence of Eu3+ and the hydrothermal treatment time are responsible for the band shifts in Y2O3:Eu3+ powders, since in the pure Y2O3 matrix this behavior was not observed. Y2O3:Eu3+ powders also show the characteristic Eu3+ emission lines at 580, 591, 610, 651 and 695 nm, when excited at 393 nm. The most intense band at 610 nm is responsible for the Eu3+ red emission in these materials, and the Eu3+ lifetime for this transition presented a slight increase as the time used in the microwave-hydrothermal assisted method increases.

Synthesis, characterization and photophysical properties of Eu3+ doped in BaMoO4

In this work Ba0.99Eu0.01MoO4 (BEMO) powders were prepared by the first time by the Complex Polymerization Method. The structural and optical properties of the BEMO powders were characterized by Fourier Transform Infra-Red (FTIR), X-ray Diffraction (XRD), Raman Spectra, High-Resolution Scanning Electron Microscopy (HR-SEM) and Photoluminescent Measurements. XRD show a crystalline scheelite-type phase after the heat treatment at temperatures greater than 400 degrees C. The ionic radius of Eu3+ (0.109 nm) is lower than the Ba2+ (0.149 nm) one. This difference is responsible for the decrease in the lattice parameters of the BEMO compared to the pure BaMoO4 matrix. This little difference in the lattice parameters show that Eu3+ is expected to occupy the Ba2+ site at different temperatures, stayed the tetragonal (S-4) symmetry characteristic of scheelite-type crystalline structures of BaMoO4. The emission spectra of the samples, when excited at 394 nm, presented the D-5(1)-> F-7(0, 1 and 2) and D-5(0)-> F-7(0, 1, 2, 3 and 4) Eu3+ transitions at 523, 533, 554, 578, 589, 614, 652 and 699 nm, respectively. The emission spectra of the powders heat-treated at 800 and 900 degrees C showed a marked increase in its intensities compared to the materials heat-treated from 400 to 700 C. The decay times for the sample were evaluated and all of them presented the average value of 0.61 ms. Eu3+ luminescence decay time follows one exponential curve indicating the presence of only one type of Eu3+ symmetry site.

Relation between kinetic parameters for reactions of organic matter degradation in waste environmental matrix

The organic fraction of urban solid residues disposed of in sanitary landfills during the decomposition yields biogas and leachate, which are sources of pollution. Leachate is a resultant liquid from the decomposition of substances contained in solid residues and it contains in its composition organic and inorganic substances. Literature shows an increase in the use of thermoanalytical techniques to study the samples with environmental interest, this way thermogravimetry is used in this research. Thermogravimetric studies (TG curves) carried out on leachate and residues shows similarities in the thermal behavior, although presenting complex composition. Residue samples were collected from landfills, composting plants, sewage treatment stations, leachate, which after treatment, were submitted for thermal analysis. Kinetic parameters were determined using the Flynn-Wall-Ozawa method. In this case they show little divergence between the kinetic parameter that can be attributed to different decomposition reaction and presence of organic compounds in different phases of the decomposition with structures modified during degradation process and also due to experimental conditions of analysis.

Structural study of thin films prepared from tungstate glass matrix by Raman and X-ray absorption spectroscopy

Thin films were prepared using glass precursors obtained in the ternary system NaPO(3)-BaF(2)-WO(3) and the binary system NaPO(3)-WO(3) with high concentrations of WO(3) (above 40% molar). Vitreous samples have been used as a target to prepare thin films. Such films were deposited using the electron beam evaporation method onto soda-lime glass substrates. Several structural characterizations were performed by Raman spectroscopy and X-ray Absorption Near Edge Spectroscopy (XANES) at the tungsten L(I) and L(III) absorption edges. XANES investigations showed that tungsten atoms are only sixfold coordinated (octahedral WO(6)) and that these films are free of tungstate tetrahedral units (WO(4)). In addition, Raman spectroscopy allowed identifying a break in the linear phosphate chains as the amount of WO(3) increases and the formation of P-O-W bonds in the films network indicating the intermediary behavior of WO(6) octahedra in the film network. Based on XANES data, we suggested a new attribution of several Raman absorption bands which allowed identifying the presence of W-O and W=O terminal bonds and a progressive apparition of W-O-W bridging bonds for the most WO(3) concentrated samples (above 40% molar) attributed to the formation of WO(6) clusters. (C) 2008 Elsevier B.V. All rights reserved.

The role of matrix effects on the quantification of abscisic acid and its metabolites in the leaves of Bauhinia variegata L. using liquid chromatography combined with tandem mass spectrometry

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

Development of metal - SiO2 nanocomposites in a single-step process by the polymerizable complex method

This work presents the synthesis and characterization of SiO2:metal (Ni, Co, Ag, and Fe) nanocomposites processed by the polymerizable complex method. The polymeric precursor solutions obtained were characterized by means of FT-Raman and C-13 NMR spectroscopy. The results show the formation of a hybrid polymer with carbon and silicon in the macromolecule chain and the transition metal cation arrested within this polymeric chain. The nanocomposites are formed during the controlled polymeric precursor pyrolysis. The reduction of the metal cation is promoted by the CO/CO2 atmosphere resulting from the pyrolysis of the organic material. Microstructural characterization, performed by TEM and X-ray diffraction (XRD), showed that the nanocomposites are formed by metal nanoparticles embedded in a amorphous matrix formed by SiO2 and carbon. In the SiO2:Fe system, Fe3C was also detected by XRD.

Study of alternative schemes for the parameterization step of the continuation power flow method based on physical parameters, part I: Mathematical modeling

The conventional power flow method is considered to be inadequate to obtain the maximum loading point because of the singularity of Jacobian matrix. Continuation methods are efficient tools for solving this kind of problem since different parameterization schemes can be used to avoid such ill-conditioning problems. This paper presents the details of new schemes for the parameterization step of the continuation power flow method. The new parameterization options are based on physical parameters, namely, the total power losses (real and reactive), the power at the slack bus (real or reactive), the reactive power at generation buses, and transmission line power losses (real and reactive). The simulation results obtained with the new approach for the IEEE test systems (14, 30, 57, and 118 buses) are presented and discussed in the companion paper. The results show that the characteristics of the conventional method are not only preserved but also improved.

Study of alternative schemes for the parameterization step of the continuation power flow method based on physical parameters, part II: Performance evaluation

New parameterization schemes have been proposed by the authors in Part I of this paper. In this part these new options for the parameterization of power flow equations are tested, namely, the total power losses (real and reactive), the power at the slack bus (real or reactive), the reactive power at generation buses, and the transmission line power losses (real and reactive). These different parameterization schemes can be used to obtain the maximum loading point without ill-conditioning problems, once the singularity of Jacobian matrix is avoided. The results obtained with the new approach for the IEEE test systems (14, 30, 57, and 118 buses) show that the characteristics of the conventional method are not only preserved but also improved. In addition, it is shown that the proposed method and the conventional one can be switched during the tracing of PV curves to determine, with few iterations, all points of the PV curve. Several tests were also carried out to compare the performance of the proposed parameterization schemes for the continuation power flow method with the use of both the secant and tangent predictors.

A new potentiometric ibuprofenate ion sensor immobilized in a graphite matrix for determination of ibuprofen in tablets

The characteristics, performance, and application of an electrode, namely, Pt vertical bar Hg vertical bar Hg-2(IBP)(2)vertical bar Graphite, where IBP stands for ibuprofenate ion, are described. This electrode responds to IBP with sensitivity of (58.6 +/- 0.9) mV decade 1 over the range 5.0 x 10(-5)-1.0 x 10(-1) mol L-1 at pH 6.0-9.0 and a detection limit of 3.8 x 10(-5) mol L-1. The electrode is easily constructed at a relatively low cost with fast response time (within 1530 s) and can be used for a period of 5 months without any considerable divergence in potentials. The proposed sensor displayed good selectivity for ibuprofen in the presence of several substances, especially concerning carboxylate and inorganic anions. It was used for the direct assay of ibuprofen in commercial tablets by means of the standard additions method. The analytical results obtained by using this electrode are in good agreement with those given by the United States Pharmacopeia procedure. (c) 2006 Elsevier B.V. All rights reserved.

Benzoate ion determination in beverages by using a potentiometric sensor immobilized in a graphite matrix

The characteristics, performance, and application of an electrode, namely. Pt\Hg\Hg-2(Bzt)(2)\graphite, where Bzt stands for benzoate ion. are described. This electrode responds to Bzt with sensitivity of 57.7 +/- 1.0 mV/decade over the range 5 x 10(-4)-1 x 10(-1) mol l(-1) at pH 6.0-8.0 with a detection limit of 1.6 x 10(-4) mol l(-1). The electrode shows easy construction, fast response rime (between 10-30 s), low-cost, acid excellent response stability (lifetime > 6 months, in continuous use), the proposed sensor displayed good selectivity for benzoate in the presence of several carboxylate and inorganic anions. It was used to determine benzoate in various beverages by means of the standard additions method. The results obtained by using this electrode compared very favorably with those given by the official AOAC spectrophotometric method and by a HPLC procedure as well. (C) 2001 Elsevier B.V. B.V. All rights reserved.

p-Aminobenzoate ion determination in pharmaceutical formulations by using a potentiometric sensor immobilized in a graphite matrix

The characteristics, performance, and application of an electrode, namely, Pt\Hg\Hg-2(PABzt)(2)\ graphite, where PABzt stands for p-aminobenzoate ion, are described. This electrode responds to PABzt with sensivity of (58.1 +/- 1.0) mV per decade over the range 1.0 x 10(-4) to 1.0 x 10(-1) mol l(-1) at pH 6.5-8.0 and a detection limit of 3.2 x 10(-5) mol l(-1). The electrode shows easy construction, fast response time (within 10-30 s), low-cost, and excellent response stability (lifetime greater than 6 months, in continuous use). The proposed sensor displayed good selectivity for p-aminobenzoate in the presence of several substances, especially, concerning carboxylate and inorganic anions. It was used to determine p-aminobenzoate in pharmaceutical formulations by means of the standard additions method. The results obtained by using this electrode compared very favorably with those given by an HPLC procedure. (C) 2004 Elsevier B.V. All rights reserved.

Picrosirius-polarization staining method as an efficient histopathological tool for collagenolysis detectin in vesical prolapse lesions

The Picrosirius-polarization method has been indicated as a selective histochemical stain for collagen detection in tissue sections. This method can also be of value for studying collagen degradation given that, under polarized light, collagen displays birefringence due to its molecular order. The aim of this study is to highlight this staining method as an additional instrument for a rapid and excellent confirmatory diagnosis of the presence of collagenolysis in connective tissue in the vaginal wall with vesical prolapse lesion, in tissue sections. Dramatic changes in collagen morphology were found in vaginal mucosa in vesical prolapse disorder: they were weakly stained by Sirius red and under polarized light appeared as thin, pale (weakly birefringent), greenish, and with fibers more scattered, while the histoarchitecture of the organ showed a disrupted appearance. Thus, in the present study, we showed in vaginal mucosa in the vesicle prolapse that corroded collagenous framework appears as fragmentary and irregularly separated collagenous structures, that are weakly birefringent, corresponding to a molecular disorganization of these fibers caused by collagenolysis. (C) 2006 Elsevier Ltd. All rights reserved.

Effect of a pilot washing system on dicofol levels in orange matrix

An efficient analytical method is described for the analysis of dicofol residues in pulp and orange peel. Samples are mixed with Celite and transferred to chromatographic columns prepacked with silica gel. Dicofol is eluted with ethyl acetate, and the extracts are analyzed by gas chromatography with electron capture detection. Mean recoveries for dicofol at levels of 0.5, 2.0, 5.0, and 10 mg/kg ranged from 87 to 95% with relative standard deviation values between 2.6 and 9.0%. To investigate the effect of a pilot washing system on dicofol residues in oranges, the analytical procedure was applied to samples submitted to different treatments with commercial formulations under field and laboratory conditions. The orange samples with and without washing were analyzed in duplicate, and the results indicated that washing under the described conditions did not allow a complete removal of dicofol residues from orange peel.

Evaluation of Bi as internal standard to minimize matrix effects on the direct determination of Pb in vinegar by graphite furnace atomic absorption spectrometry using Ru permanent modifier with co-injection of Pd/Mg(NO3)(2)

Bismuth was evaluated as an internal standard for the direct determination of Pb in vinegar by graphite furnace atomic absorption spectrometry using Ru as a permanent modifier with co-injection of Pd/Mg(NO3)(2). The correlation coefficient of the graph plotted from the non-nalized absorbance signals of Bi versus Pb was r=0.989. Matrix effects were evaluated by analyzing the slope ratios between the analytical curve, and analytical curves obtained from Pb additions in red and white wine vinegar obtained from reference solutions prepared in 0.2% (v/v) HNO3, samples. The calculated ratios were around 1.04 and 1.02 for analytical curves established applying an internal standard and 1.3 and 1.5 for analvtical curves without. Analytical curves in the 2.5-15 pg L-1 Pb concentration interval were established using the ratio Pb absorbance to Bi absorbance versus analvte concentration, and typical linear correlations of r=0.999 were obtained. The proposed method was applied for direct determination of Pb in 18 commercial vinegar samples and the Pb concentration varied from 2.6 to 31 pg L-1. Results were in agreement at a 95% confidence level (paired t-test) with those obtained for digested samples. Recoveries of Pb added to vinegars varied from 96 to 108% with and from 72 to 86% without an internal standard. Two water standard reference materials diluted in vinegar sample were also analyzed and results were in agreement with certified values at a 95% confidence level. The characteristic mass was 40 pg Pb and the useful lifetime of the tube was around 1600 firings. The limit of detection was 0.3 mu g L-1 and the relative standard deviation was <= 3.8% and <= 8.3% (n = 12) for a sample containing, 10 mu L-1 Pb with and without internal standard, respectively. (C) 2007 Elsevier B.V. All rights reserved.

Simplified multiresidue method for the determination of organophosphorus insecticides in olive oil

A simple and rapid method for the determination of 13 organophosphorus insecticides and their metabolites in olive oil by GC is described. The pesticide was extracted from oil with acetonitrile and no cleanup was needed. GC-nitrogen-phosphorus detection response factors of pesticides were affected by solvents and coextractive substances. Pesticides in hexane showed on average higher response factors. Standards were prepared in the residue-free oil extract solubilized in hexane to handle effects of matrix and solvent. The low amount of coextractive substances does not decrease the column efficiency, even after a few hundred analyses. Recovery at three fortification levels (ca. 0.1, 1.0 and 3.0 mg/kg) ranged from 74 to 118%, With coefficients of variation ranging from 1 to 16.