Estudo da obtenção de cerâmica composta de alumina e beta alumina sódica utilizando-se resíduo cerâmico de velas de ignição e pó químico de extintores de incêndio

Ceramic materials the alumina base are large industrial applications. They are required for these products, specific characteristics obtained by following strict criteria during the manufacturing process. However, after life, not always these products are reused by a suitable waste management process. In ceramist context, advance research aimed at the reuse of waste aimed at obtaining ceramics and composite materials, with marked reduction of conventional raw materials. Aiming to generate scientific, technological and environmental contribution, this work studied to obtain a composite of alumina ceramic (Al2O3) and sodium beta alumina (NaAl11O17 ), and as starting materials the residue of the ceramic insulator of spark plugs, as a source alumina (Al2O3) powder and unusable sodium bicarbonate (NaHCO3) of fire extinguishers, as a source of sodium oxide (Na2O). The final ceramic product was obtained from a conventional mixture of sodium aluminum oxide in appropriate molar proportions. Sample spark plugs were obtained, discarded by lifetime, specific to a manufacturer, which, after passing through mechanical stress (grinding, magnetic purification, washing, drying and grinding the high energy), which resulted in residue powder with ceramic content of 84.34 % alumina (Al2O3), found by FRX chemical analysis, the phases present and identified by DRX. The dry chemical fire extinguisher, baking soda-based (NaHCO3) with expired, was obtained through direct collection of the waste generated during maintenance. Subjected to heat treatment at 120 °C , the NaHCO3 powder was decomposed in sodium oxide ( Na2O), which, subjected to chemical analysis (FRX) and mineralogical (DRX) revealed a content of 86.62 % sodium oxide (Na2O) . In the following steps the experimental procedure, chemical formulations were made on a molar basis of the starting material (1:9, 1:10 and 1:11 de Na2O/ Al2O3) inclusion of additives, milling parameters, sieve analysis, dilatometry, conformation of specimens, sintering in firing steps at 800 °C , 1000 °C and 1.200 °C with varying stays 30 , 60 and 120 minutes in each of the levels. The characterization of the final product was made by the following physical tests: water absorption, porosity, linear shrinkage, mineralogical analysis by DRX and microstructural analysis by MEV. A higher formation of sodium beta alumina (NaAl11O17), in sintered specimens in levels of 1.200 °C and 120 minutes, despite the prevailing coexistence of alpha phase alumina (Al2O3). From the results obtained opens up prospects for the reuse of waste studied in this work, the potter context and in other technological areas.

Estudo da obtenção de cerâmica composta de alumina e beta alumina sódica utilizando-se resíduo cerâmico de velas de ignição e pó químico de extintores de incêndio

Ceramic materials the alumina base are large industrial applications. They are required for these products, specific characteristics obtained by following strict criteria during the manufacturing process. However, after life, not always these products are reused by a suitable waste management process. In ceramist context, advance research aimed at the reuse of waste aimed at obtaining ceramics and composite materials, with marked reduction of conventional raw materials. Aiming to generate scientific, technological and environmental contribution, this work studied to obtain a composite of alumina ceramic (Al2O3) and sodium beta alumina (NaAl11O17 ), and as starting materials the residue of the ceramic insulator of spark plugs, as a source alumina (Al2O3) powder and unusable sodium bicarbonate (NaHCO3) of fire extinguishers, as a source of sodium oxide (Na2O). The final ceramic product was obtained from a conventional mixture of sodium aluminum oxide in appropriate molar proportions. Sample spark plugs were obtained, discarded by lifetime, specific to a manufacturer, which, after passing through mechanical stress (grinding, magnetic purification, washing, drying and grinding the high energy), which resulted in residue powder with ceramic content of 84.34 % alumina (Al2O3), found by FRX chemical analysis, the phases present and identified by DRX. The dry chemical fire extinguisher, baking soda-based (NaHCO3) with expired, was obtained through direct collection of the waste generated during maintenance. Subjected to heat treatment at 120 °C , the NaHCO3 powder was decomposed in sodium oxide ( Na2O), which, subjected to chemical analysis (FRX) and mineralogical (DRX) revealed a content of 86.62 % sodium oxide (Na2O) . In the following steps the experimental procedure, chemical formulations were made on a molar basis of the starting material (1:9, 1:10 and 1:11 de Na2O/ Al2O3) inclusion of additives, milling parameters, sieve analysis, dilatometry, conformation of specimens, sintering in firing steps at 800 °C , 1000 °C and 1.200 °C with varying stays 30 , 60 and 120 minutes in each of the levels. The characterization of the final product was made by the following physical tests: water absorption, porosity, linear shrinkage, mineralogical analysis by DRX and microstructural analysis by MEV. A higher formation of sodium beta alumina (NaAl11O17), in sintered specimens in levels of 1.200 °C and 120 minutes, despite the prevailing coexistence of alpha phase alumina (Al2O3). From the results obtained opens up prospects for the reuse of waste studied in this work, the potter context and in other technological areas.

Sinterização flash do condutor catiônico beta-alumina sintetizada pelo método dos precursores poliméricos.

A beta-alumina de sódio é uma cerâmica condutora de íons Na+ utilizada como eletrólito sólido em baterias de sódio para armazenamento de energias intermitentes como energia solar e eólica. Devido ao alto teor de sódio, esse material é instável a altas temperaturas, podendo sofrer variações de composição durante a etapa de sinterização convencional que utiliza altas temperaturas por longos períodos de tempo. A sinterização flash é uma técnica de sinterização ativada por corrente elétrica que proporciona a densificação de compactos cerâmicos em poucos segundos, a temperaturas notavelmente mais baixas que as convencionais. Uma vez obrigatória a passagem de corrente elétrica através da amostra, a sinterização flash de qualquer material condutor parece bastante razoável. Não obstante, até o presente momento a maioria dos trabalhos publicados sobre o assunto aborda apenas condutores de vacância de oxigênio ou semicondutores, materiais compatíveis com eletrodos de platina (Pt). Nesse trabalho a sinterização flash de um condutor catiônico foi estudada utilizando-se a beta-alumina como material modelo. A beta-alumina foi sintetizada pelo método dos precursores poliméricos, caracterizada e então submetida à sinterização flash. O material de eletrodo padrão (platina) provou ser um eletrodo bloqueador em contato com a beta-alumina. O sucesso da sinterização flash foi determinado pela troca do material de eletrodo por prata (Ag), o que possibilitou uma reação eletroquímica reversível nas interfaces eletrodo-cerâmica e possibilitou a obtenção de um material densificado com morfologia e composição química homogêneas. Devido à metaestabilidade da beta-alumina, a atmosfera dos experimentos precisou ser alterada para manter a integridade desse material rico em um metal alcalino (Na+). A sinterização flash de um condutor catiônico é apresentada pela primeira vez na literatura e ressalta a importância da reação de eletrodo, que é um fator limitante para o sucesso da sinterização flash e precisa ser estudada e adaptada para cada tipo de material.

Quantitative analysis of aluminum dross by the Rietveld method

Aluminum white dross is a valuable material principally due to its high metallic aluminum content. The aim of this work is to develop a method for quantitative analysis of aluminum white dross with high accuracy. Initially, the material was separated into four granulometric fractions by means of screening. Two samples of each fraction were obtained, which were analyzed by means of X-ray fluorescence and energy dispersive spectroscopy in order to determine the elements present in the samples. The crystalline phases aluminum, corundum, spinel, defect spinel, diaoyudaoite, aluminum nitride, silicon and quartz low were identified by X-ray diffraction. The quantitative phase analysis was performed by fitting the X-ray diffraction profile with the Rietveld method using the GSAS software. The following quantitative results were found: 77.8% aluminum, 7.3% corundum, 2.6% spinel, 7.6% defect spinel, 1.8% diaoyudaoite, 2.9% aluminum nitride, and values not significant of quartz and silicon.

Magnetic resonance study of a vanadium pentoxide gel

In this work we report results from continuous-wave (CW) and pulsed electron paramagnetic resonance (EPR) and proton nuclear magnetic resonance (NMR) studies of the vanadium pentoxide xerogel V2O5:nH(2)O (n approximate to 1.6). The low temperature CW-EPR spectrum shows hyperfine structure due to coupling of unpaired V4+ electron with the vanadium nucleus. The analysis of the spin Hamiltonian parameters suggests that the V4+ ions are located in tetragonally distorted octahedral sites. The transition temperature from the rigid-lattice low-temperature regime to the high temperature liquid-like regime was determined from the analysis of the temperature dependence of the hyperfine splitting and the V4+ motional correlation time. The Electron Spin Echo Envelope Modulation (ESEEM) data shows the signals resulting from the interaction of H-1 nuclei with V4+ ions. The modulation effect was observed only for field values in the center of the EPR absorption spectrum corresponding to the single crystals orientated perpendicular to the magnetic field direction. At least three protons are identified in the xerogel by our magnetic resonance experiments: (I) the OH groups in the equatorial plane, (ii) the bound water molecules in the axial V=O bond and (iii) the free mobile water molecules between the oxide layers. Proton NMR lineshapes and spin-lattice relaxation times were measured in the temperature range between 150 K and 323 K. Our analysis indicates that only a fraction of the xerogel protons contribute to the measured conductivity.

Total oxidation of naphthalene using palladium nanoparticles supported on BETA, ZSM-5, SAPO-5 and alumina powders

A range of catalysts based on Pd nanoparticles supported on inorganic supports such as BETA and ZSM-5 zeolites, a silicoaluminophosphate molecular sieve (SAPO-5) and γ-alumina as a standard support have been tested for the total oxidation of naphthalene (100 ppm, total flow 50 ml/min) showing a conversion to carbon dioxide of 100% between 165 and 180 °C for all the analysed catalysts. From the combined use of zeolites with PVP polymer protected Pd based nanoparticles, enhanced properties have been found for the total abatement of naphthalene in contrast with other kinds of catalysts. A Pd/BETA catalyst has been demonstrated to have excellent activity, with a high degree of stability, as shown by time on line experiments maintaining 100% conversion to CO2 during the 48 h tested.

Análise químico-farmacêutica de cefazolina sódica em pó liofilizado para solução injetável

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

Análise químico-farmacêutica de preparações injetáveis de ampicilina sódica

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

Desenvolvimento de método analítico para estudo de degradação forçada de cefalotina sódica na forma farmacêutica pó liofilizado para solução injetável

Pós-graduação em Ciências Farmacêuticas - FCFAR

Impaired Compensatory Beta-cell Function And Growth In Response To High-fat Diet In Ldl Receptor Knockout Mice.

In this study, we investigated the effect of low density lipoprotein receptor (LDLr) deficiency on gap junctional connexin 36 (Cx36) islet content and on the functional and growth response of pancreatic beta-cells in C57BL/6 mice fed a high-fat (HF) diet. After 60 days on regular or HF diet, the metabolic state and morphometric islet parameters of wild-type (WT) and LDLr-/- mice were assessed. HF diet-fed WT animals became obese and hypercholesterolaemic as well as hyperglycaemic, hyperinsulinaemic, glucose intolerant and insulin resistant, characterizing them as prediabetic. Also they showed a significant decrease in beta-cell secretory response to glucose. Overall, LDLr-/- mice displayed greater susceptibility to HF diet as judged by their marked cholesterolaemia, intolerance to glucose and pronounced decrease in glucose-stimulated insulin secretion. HF diet induced similarly in WT and LDLr-/- mice, a significant decrease in Cx36 beta-cell content as revealed by immunoblotting. Prediabetic WT mice displayed marked increase in beta-cell mass mainly due to beta-cell hypertrophy/replication. Nevertheless, HF diet-fed LDLr-/- mice showed no significant changes in beta-cell mass, but lower islet-duct association (neogenesis) and higher beta-cell apoptosis index were seen as compared to controls. The higher metabolic susceptibility to HF diet of LDLr-/- mice may be explained by a deficiency in insulin secretory response to glucose associated with lack of compensatory beta-cell expansion.

Macrophage Cell Activation With Acute Apical Abscess Contents Determined By Interleukin-1 Beta And Tumor Necrosis Factor Alpha Production.

This clinical study has investigated the antigenic activity of bacterial contents from exudates of acute apical abscesses (AAAs) and their paired root canal contents regarding the stimulation capacity by levels of interleukin (IL)-1 beta and tumor necrosis factor alpha (TNF-α) throughout the root canal treatment against macrophage cells. Paired samples of infected root canals and exudates of AAAs were collected from 10 subjects. Endodontic contents were sampled before (root canal sample [RCS] 1) and after chemomechanical preparation (RCS2) and after 30 days of intracanal medication with calcium hydroxide + chlorhexidine gel (Ca[OH]2 + CHX gel) (RCS3). Polymerase chain reaction (16S rDNA) was used for detection of the target bacteria, whereas limulus amebocyte lysate was used to measure endotoxin levels. Raw 264.7 macrophages were stimulated with AAA exudates from endodontic contents sampled in different moments of root canal treatment. Enzyme-linked immunosorbent assays were used to measure the levels of TNF-α and IL-1 beta. Parvimonas micra, Porphyromonas endodontalis, Dialister pneumosintes, and Prevotella nigrescens were the most frequently detected species. Higher levels of endotoxins were found in samples from periapical exudates at RCS1 (P < .005). In fact, samples collected from periapical exudates showed a higher stimulation capacity at RCS1 (P < .05). A positive correlation was found between endotoxins from exudates with IL-1 beta (r = 0.97) and TNF-α (r = 0.88) production (P < .01). The significant reduction of endotoxins and bacterial species achieved by chemomechanical procedures (RCS2) resulted in a lower capacity of root canal contents to stimulate the cells compared with that at RCS1 (P < .05). The use of Ca(OH)2 + CHX gel as an intracanal medication (RCS3) improved the removal of endotoxins and bacteria from infected root canals (P < .05) whose contents induced a lower stimulation capacity against macrophages cells at RCS1, RCS2, and RCS3 (P < .05). AAA exudates showed higher levels of endotoxins and showed a greater capacity of macrophage stimulation than the paired root canal samples. Moreover, the use of intracanal medication improved the removal of bacteria and endotoxins from infected root canals, which may have resulted in the reduction of the inflammatory potential of the root canal content.

Enhanced Glucose-induced Intracellular Signaling Promotes Insulin Hypersecretion: Pancreatic Beta-cell Functional Adaptations In A Model Of Genetic Obesity And Prediabetes.

Obesity is associated with insulin resistance and is known to be a risk factor for type-2 diabetes. In obese individuals, pancreatic beta-cells try to compensate for the increased insulin demand in order to maintain euglycemia. Most studies have reported that this adaptation is due to morphological changes. However, the involvement of beta-cell functional adaptations in this process needs to be clarified. For this purpose, we evaluated different key steps in the glucose-stimulated insulin secretion (GSIS) in intact islets from female ob/ob obese mice and lean controls. Obese mice showed increased body weight, insulin resistance, hyperinsulinemia, glucose intolerance and fed hyperglycemia. Islets from ob/ob mice exhibited increased glucose-induced mitochondrial activity, reflected by enhanced NAD(P)H production and mitochondrial membrane potential hyperpolarization. Perforated patch-clamp examination of beta-cells within intact islets revealed several alterations in the electrical activity such as increased firing frequency and higher sensitivity to low glucose concentrations. A higher intracellular Ca(2+) mobilization in response to glucose was also found in ob/ob islets. Additionally, they displayed a change in the oscillatory pattern and Ca(2+) signals at low glucose levels. Capacitance experiments in intact islets revealed increased exocytosis in individual ob/ob beta-cells. All these up-regulated processes led to increased GSIS. In contrast, we found a lack of beta-cell Ca(2+) signal coupling, which could be a manifestation of early defects that lead to beta-cell malfunction in the progression to diabetes. These findings indicate that beta-cell functional adaptations are an important process in the compensatory response to obesity.

Partial-hepatectomized (70%) Model Shows A Correlation Between Hepatocyte Growth Factor Levels And Beta-cell Mass.

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Caracterização do complexo de inclusão ropivacaína: beta-ciclodextrina

Characteriza of the inclusion complex ropivacaine: beta-cyclodextrin. Ropivacaine (RVC) is a widely used local anesthetic. The complexation of RVC with beta-cyclodextrin (beta-CD) is of great interest for the development of more efficient local anesthetic formulations. The present work focuses on the characterization of the RVC:beta-CD complex by nuclear magnetic resonance (NMR). The stoichiometry of the complex is 1:2 RVC:beta-CD. DOSY-NMR shows that the association constant is 55.5 M-1. Longitudinal relaxation time results show that RVC changes its mobility in the presence of beta-CD. This study is focused on the physicochemical characterization of inclusion complexes that are potentials options for pain treatment.

Indução assimétrica 1,5-Anti na adição de enolatos de boro de metilcetonas beta-oxigenadas a aldeídos

High levels of substrate-based 1,5-stereoinduction are obtained in the boron-mediated aldol reactions of beta-oxygenated methyl ketones with achiral and chiral aldehydes. Remote induction from the boron enolates gives the 1,5-anti adducts, with the enolate pi-facial selectivity critically dependent upon the nature of the beta-alkoxy protecting group. This 1,5-anti aldol methodology has been strategically employed in the total synthesis of several natural products. At present, the origin of the high level of 1,5-anti induction obtained with the boron enolates is unclear, although a model based on a hydrogen bonding between the alkoxy oxygen and the formyl hydrogen has been recently proposed.