Effect of precursor solution on the formation of perovskite phase of Pb(Mg-1/Nb-3(2/3))O-3 thin films

Precursor solutions for Pb(Mg1/3Nb2/3)O-3 (PMN) synthesis were obtained by Pechini's method. The influence of the concentration of organic materials on the phase formation has been studied. For this purpose, PMN solutions were prepared with different precursors and were characterized by thermogravimetric and differential thermal analysis. The obtained solutions were deposited onto a Si (100) substrate by dip coating and pre-treated in a hot plate at 300 degreesC for 1 h. The films were annealed at 600, 700, 800 and 900 degreesC for 1 h and characterized by X-ray diffraction. The perovskite phase was formed after annealing at 600 and 700 degreesC when the solution of PMN was prepared with a lower amount of organic material and starting with mobium oxide. By increasing the temperature to 800 or 900 degreesC, only the formation of pyrochlore phase was observed. With the solution prepared from mobium ethoxide, only the presence of pyrochlore phase was observed independently of the annealing temperature. (C) 2002 Elsevier B.V. B.V. All rights reserved.

Effects of organic and inorganic additives on flotation recovery of washed cells of Saccharomyces cerevisiae resuspended in water

Separation of microbial cells by flotation recovery is usually carried out in industrial reactors or wastewater treatment systems, which contain a complex mixture of microbial nutrients and excretion products. In the present study, the separation of yeast cells by flotation recovery was carried out using a simple flotation recovery systems containing washed yeast cells resuspended in water in order to elucidate the effects of additives (defined amounts of organic and inorganic acids, ethanol, surfactants and sodium chloride) on the cellular interactions at interfaces (cell/aqueous phase and cell/air bubble). When sodium chloride, organic acids (notably propionic, succinic and acetic acids) and organic surfactants (sodium dodecyl sulphate (SDS), cetyltrimethylammonium bromide (CTAB) and Nonidet P40) were added to the flotation recovery system, significant increases in the cell recovery of yeast hydrophobic cells (Saccharomyces cerevisiae, strain FLT-01) were observed. The association of ethanol to acetic acid solution (a minor by-product of alcoholic fermentation) in the flotation recovery system, containing washed cells of strain FLT-01 resuspended in water, leading to an increased flotation recovery at pH 5.5. Thus, the association among products of the cellular metabolism (e.g., ethanol and acetic acid) can improve yeast cell recovery by flotation recovery. (c) 2006 Elsevier B.V. All rights reserved.

Determination of sugar cane herbicides in soil and soil treated with sugar cane vinasse by solid-phase extraction and HPLC-UV

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Organic acid profile of commercial sour cassava starch

A presença de ácidos orgânicos no polvilho azedo, além de contribuir com aspectos como sabor e aroma, tem, conforme a literatura indica, correlação com a propriedade de expansão, que é um fator determinante no uso alimentício. Amostras de polvilho azedo foram coletadas nas Regiões Sul e Sudeste diretamente nas empresas ou no comércio. Foram preparadas para análise em cromatografia líquida de alta eficiência (CLAE), sendo que o cromatógrafo estava equipado com coluna Biorad Aminex HPX-87H para análise de ácidos orgânicos e detector refratométrico. As condições de análise envolveram o emprego da fase móvel ácido sulfúrico 0,005M, fluxo de 0,6 ml/min e temperatura da coluna de 60oC. Os ácidos quantificados foram lático (0,036 a 0,813 g/100g), acético (0 a 0,068 g/100g), propiônico (0 a 0,013 g/100g) e butírico (0 a 0,057 g/100g), presentes na fermentação natural. Os resultados revelaram grande variação entre as amostras, com diferenças mesmo dentro das Regiões. Algumas amostras apresentaram quantidades elevadas de ácidos, especialmente do ácido lático, mas nestas amostras os ácidos propiônico e butírico não foram detectados. A ausência do ácido butírico não era esperada, uma vez que esse ácido está diretamente relacionado com o aroma característico do polvilho azedo. O fato pode sugerir que a obtenção de algumas das amostras estudadas pode ter ocorrido sem o processo fermentativo natural.

Cassava wastewater (manipueira) treatment using a two-phase anaerobic biodigestor

Um biodigestor anaeróbio de duas fases foi utilizado para se analisar a produção de metano com diferentes cargas de entrada de manipueira. A fase acidogênica foi realizada em processo de batelada e a metanogênica em biodigestor anaeróbio de fluxo ascendente e leito fixo com alimentação contínua. As cargas orgânicas de entrada variaram de 0,33 a 8,48 gDQO (Demanda Química de Oxigênio)/L.dia. A maior porcentagem de metano encontrada foi de 80,9%, com carga orgânica de 0,33g e a menor, 56,8%, obtida com 8,49gDQO/L.d. A maior taxa de redução de DQO foi de 88,89%, obtida com carga orgânica de 2,25g e a menor, 54,95%, com 8,48gDQO/L.d. Analisando-se os dados apresentados verificou-se que a biodigestão anaeróbia pode ser conduzida, pelo menos, de duas maneiras, ou seja, para produção de energia (metano) ou para redução de carga orgânica. A carga orgânica de entrada deve ser calculada em função do objetivo a ser alcançado com a biodigestão anaeróbia.

Planar and UV written channel optical waveguides prepared with siloxane poly(oxyethylene)-zirconia organic-inorganic hybrids. Structure and optical properties

Organic-inorganic hybrids were prepared using ureapropyltriethoxysilane, methacryloxypropyltrimethoxysilane and acrylic acid modified zirconium(IV) n-propoxide precursors and were characterized by small angle X-ray scattering, X-ray diffraction and photoluminescence spectroscopy. The results indicate an effective interaction between the zirconium-based nanoparticles and the siliceous nanodomains that induces changes in the hybrids' emission features. Planar waveguides were obtained by spin-coating of the prepared sols on sodalime and silica substrates. Refractive index, thickness, number of propagating modes, and attenuation coefficient were measured at 543.5, 632.8 and 1550 nm by the prism coupling technique. The synergism between the two hybrid precursors resulted in monomode planar waveguides with low losses in the infrared ( from 0.6-1.1 dB cm(-1)) which also support a number of propagating modes in the visible ( losses from 0.4-1.5 dB cm(-1)). Channel waveguides were also obtained by UV photopatterning using amplitude or phase masks and propagating modes were observed at 1550 nm.

Polycyclic aromatic hydrocarbons and other selected organic compounds in ambient air of Campo Grande City, Brazil

Fourteen samples of particulate matter and semi-volatile organic compounds were collected during 6 months in the city of Campo Grande, South Mato Grosso State, Brazil. Particle-bound polycyclic aromatic hydrocarbons (PAHs) were collected on Fluoropore PTFE filters and gas-phase PAHs were collected into sorbent tubes with XAD-2 resin. Both types of samples were extracted with a dichloromethane/methanol mixture (4:1 v/v), then the extracts were subjected to gas chromatography-mass spectrometry (GC-MS) analysis. PAHs, oxidized PAH (oxy-PAHs), phenols and methoxyphenols were identified by use of GC retention indices and MS files. The average value obtained for the sum of 15 PAHs was 21.05 ng m(-3) (range: 8.94-62.5 ng m(-3)). The presence of specific tracers and calculations of characteristic ratios (e.g. [Phe]/[Phe] + [Ant]) were used to identify the sources of the emissions of PAHs in the atmospheric samples. Levoglucosan (the anhydride of beta-glucose), retene (1-methyl-7-isopropylphenanthrene) and methoxyphenols (derivatives of syringol and guaiacol) and tracers for wood burning were identified. This study demonstrates that biomass burning from the rural zone is the main source of PAHs and emissions of other substances in the investigated site of Campo Grande. (c) 2004 Elsevier Ltd. All rights reserved.

Solid-phase extraction of sugar cane soot extract for analysis by gas chromatography with flame ionisation and mass spectrometric detection

The incomplete combustion of biomass is one of the most important sources of emissions of organic compounds into the atmosphere, like polycyclic aromatic hydrocarbons (PAHs) which show genotoxic activity. Since environmental samples generally contain interferents and trace amounts of PAHs of interest, concentration and clean-up procedures are usually required prior to the final chromatographic analysis. This paper discusses the performance of Sep-Pak cartridges (silica gel and RP18) on clean-up of sugar cane soot extract. The best results were obtained with a silica Sep-Pak cartridge. The recoveries ranged from 79% (benzo[b]fluoranthene) to 113% (benzo[e]pyrene). (C) 2000 Elsevier B.V. B.V. All rights reserved.

NMR study of ion-conducting organic-inorganic nanocomposites poly(ethylene glycol) - Silica - LiClO4

Hybrid organic-inorganic ionic conductors, also called ormolytes, were obtained by dissolution of LiClO4 into silica/poly(ethylene glycol) matrices. Solid-state nuclear magnetic resonance (NMR) was used to probe the inorganic phase structure (Si-29) and the effects of the temperature and composition on the dynamic behavior of the ionic species (Li-7) and the polymer chains (H-1 and C-13). The NMR results between -100 and +90 degrees C show a strong correlation with ionic conductivity and differential scanning calorimetry experiments. The results also demonstrate that the cation mobility is assisted by segmental motion of the polymer, which is in agreement with the results previously reported for pure poly(ethylene oxide), PEG, electrolytes.

Use of diffusive gradients in thin films and tangential flow ultrafiltration for fractionation of Al(III) and Cu(II) in organic-rich river waters

Diffusive gradients in thin films (DGT) and tangential-flow ultrafiltration (TF-UF) were combined for fractionation of Al and Cu in river water containing high content of dissolved organic carbon. A procedure based on ultrafiltration data is proposed to determine diffusion coefficients of the analytes in water samples and model solutions containing both free metal (M) and complex (metal - humic substance). Aiming to evaluate the accuracy of the proposed approach, the DGT results were compared with those from a protocol for determination of labile Al and Cu based on solid phase extraction (SPE). Good agreement between data from DGT and SPE were attained for model solutions. For analysis of real organic-rich water samples, differences between DGT and SPE measurements were consistent with the time-scales of the techniques. The concentration of labile Al determined by DGT were lower than the total dissolved concentrations (determined by inductively coupled plasma mass spectrometry) and exceeded the ultrafiltered concentration, indicating that inorganic Al species (species small enough to pass through 1 kDa membrane) were minor species as compared with Al organic complexes. For both Al and Cu, there were species not measured by DGT as they are not sufficiently labile. (C) 2007 Elsevier B.V. All rights reserved.

Plasma enhanced chemical vapor deposition of titanium(IV) ethoxide-oxygen-helium mixtures

Thin films were deposited by plasma enhanced chemical vapor deposition from titanium (IV) ethoxide (TEOT)-oxygen-helium mixtures. Actinometric optical emission spectroscopy was used to obtain the relative plasma concentrations of the species H, CH, O and CO as a function of the percentage of oxygen in the feed, R(ox). The concentrations of these species rise with increasing R(ox) and tend to fall for R(ox) greater than about 45%. As revealed by a strong decline in the emission intensity of the actinometer Ar as R(ox) was increased, the electron mean energy or density (or both) decreased as greater proportions of oxygen were fed to the chamber. This must tend to reduce gas-phase fragmentation of the monomer by plasma electrons. As the TEOT flow rate was fixed, however, and since the species H and CH do not contain oxygen, the rise in their plasma concentrations with increasing R(ox) is explained only by intermediate reactions involving oxygen or oxygen-containing species. Transmission infrared (IRS) and X-ray photoelectron (XPS) spectroscopies were employed to investigate film structure and composition. The presence of CH(2), CH(3), C=C, C-O and C=O groups was revealed by IRS. In addition, the presence of C-O and C=O groups was confirmed by XPS, which also revealed titanium in the +4 valence state. The Ti content of the films, however, was found to be much less than that of the monomer material itself. (C) 2007 Elsevier B.V. All rights reserved.

Phase separation suppression in InGaN epitaxial layers due to biaxial strain

Phase separation suppression due to external biaxial strain is observed in InxGa1-xN alloy layers by Raman scattering spectroscopy. The effect is taking place in thin epitaxial layers pseudomorphically grown by molecular-beam epitaxy on unstrained GaN(001) buffers. Ab initio calculations carried out for the alloy free energy predict and Raman measurements confirm that biaxial strain suppress the formation of phase-separated In-rich quantum dots in the InxGa1-xN layers. Since quantum dots are effective radiative recombination centers in InGaN, we conclude that strain quenches an important channel of light emission in optoelectronic devices based on pseudobinary group-III nitride semiconductors. (C) 2002 American Institute of Physics.

Photopatternable di-ureasil-zirconium oxocluster organic-inorganic hybrids as cost effective integrated optical substrates

Organic-inorganic hybrids containing methacrylic acid (McOH, CH(2)= C(CH(3))COOH)) modified zirconium tetrapropoxide, Zr(OPr(n))(4), classed as di-ureasil-zirconium oxo-cluster hybrids, have been prepared and structurally characterized by X-ray diffraction (XRD), small-angle X-ray scattering (SAXS), Fourier transform infrared (FT-IR) and Raman (FT-Raman) spectroscopies, Si and C nuclear magnetic resonance (NMR), and atomic force microscopy (AFM). XRD and SAXS results have pointed out the presence of Si- and Zr-based nanobuilding blocks (NBBs) dispersed into the organic phase. Inter-NBBs correlation distances have been estimated for the pure di-ureasil and a model compound obtained. by hydrolysis/condensation of Zr(OPr(n))(4):McOH (molar ratio 1: 1): d(Si) approximate to 26 +/- 1 angstrom and d(Zr) approximate to 16 +/- 1 angstrom, respectively. In the case of the di-ureasil-zirconium oxo-cluster hybrids, these distances depend on the Zr relative molar percentage (rel. mol. Zr %) (d(Si) ranges from 18 to 25 angstrom and d(Zr) from 14 to 23 angstrom, as the rel. mol. Zr % increases from 5 to 75), suggesting that the Si- and Zr-based clusters are interconstrained. Complementary data from FT-IR, FT-Raman, (29)Si and (13)C NMR, and AFM support to a structural model where McOH-modified Zr-based NBBs (Zr-OMc) are present over the whole range of composition. At low Zr-OMc contents (rel. mol. Zr % <30) the clusters are well-dispersed within the di-ureasil host, whereas segregation occurs at the 0.1 mu m scale at high Zr-OMc concentration (rel. mol. Zr % = 50). No Zr-O-Si heterocondensation has been discerned. Monomode waveguides, diffractions gratings, and Fabry-Perot cavities have been written through the exposure of the hybrid monoliths to UV light. FT-Raman has shown that the chemical process that takes place under illumination is the polymerization of the methacrylate groups of the Zr-OMc NBBs. The guidance region in patterned channels is a Gaussian section located below the exposed surface with typical dimensions of 320 mu m wide and 88 mu m deep. The effective refractive index is 1.5162 (maximum index contrast on the order of 1 x 10(-4)) and the reflection coeficient of the Fabry-Perot cavity (formed by a grating patterned into a 0.278 cm channel) is 0.042 with a free spectral range value of 35.6 GHz.

Inorganic-Organic Nanocomposite Assembly Using Collagen as a Template and Sodium Tripolyphosphate as a Biomimetic Analog of Matrix Phosphoprotein

Nanocomposites created with polycarboxylic acid alone as a stabilization agent for prenucleation clusters-derived amorphous calcium phosphate exhibit nonperiodic apatite deposition. In the present study, we report the use of inorganic polyphosphate as a biomimetic analog of matrix phosphoprotein for directing poly(acrylic acid)-stabilized amorphous nano-precursor phases to assemble into periodic apatite-collagen nanocomposites. The sorption and desorption characteristics of sodium tripolyphosphate to type I collagen were examined. Periodic nanocomposite assembly with collagen as a template was demonstrated with TEM and SEM using a Portland cement-based resin composite and a phosphate-containing simulated body fluid. Apatite was detected within the collagen at 24 h and became more distinct at 48 h, with prenucleation clusters attaching to the collagen fibril surface during the initial infiltration stage. Apatite-collagen nanocomposites at 72 h were heavily mineralized with periodically arranged intrafibrillar apatite platelets. Defect-containing nanocomposites caused by desorption of TPP from collagen fibrils were observed in regions lacking the inorganic phase.

Optical chemical sensors using polythiophene derivatives as active layer for detection of volatile organic compounds

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