Compósitos magnéticos baseados em hidrotalcitas para a remoção de contaminantes aniônicos em água

In this work the adsorption features of hydrotalcites (Al, Mg- CO3) and the magnetic properties of iron oxides have been combined in a composite to produce a magnetic adsorbent. These magnetic composites can be used as adsorbents for anionic contaminants in water and subsequently removed from the medium by a simple magnetic process. The magnetic hydrotalcites were characterized by XRD, magnetization measurements, N2 adsorption isotherms and Mössbauer spectroscopy. These magnetic adsorbents show remarkable adsorption capacity for anionic contaminants in water.

Efecto de la naturaleza del precursor sobre las caracteristicas de las nanoparticulas de SnO2 sintetizadas

Tin oxide (SnO2) is widely used in industry as raw material for electronic devices, plating of different types of materials, for dyes and pigments, for electroplating, heterogeneous catalysis, etc. In this work SnO2 was obtained by a controlled precipitation method with special attention to the effects the tin precursor has on the microstructure of the final product. The most appropriate pH for obtaining SnO2 with the rutile structure as the main phase is 6.25 for SnCl2 and 6.40 for SnSO4. After heat treatment at 600 °C, particles of nanometric order (~10 - 30 nm approx) were obtained. The characterization of the solid phase was made by X-ray diffraction (XRD), thermal analysis (DTA/TG), transmission electron microscopy (TEM) and Fourier transformed infrared spectroscopy (FTIR).

Nióbia magnética como adsorvente de contaminantes orgânicos em meio aquoso: efeito da temperatura e do pH

This work describes novel materials based on pure iron oxide and iron oxide/niobia composite to produce a magnetic adsorbent. These materials were prepared with synthetic iron oxide and characterized by powder XRD, SEM, FTIR, TPR and Mössbauer spectroscopy. Results showed that the main iron oxides formed were goethite (aFeOOH) and maghemite (gFe2O3) with small particle size. The iron oxide and iron oxide/niobia composite showed high adsorption ability for organic compounds. The positive enthalpy indicated an endothermic adsorption process suggesting physical adsorption.

Análise química de pigmento vermelho em osso humano

This work presents a chemical study of human bones painted red located at the Morro dos Ossos site, Piauí State, Brazil. The pigment was studied using X-ray diffraction (XRD), energy dispersive spectroscopy (EDS), scanning electron microscopy (SEM), complexation reactions with thiocyanate and UV-Vis absorption spectroscopy. The results confirmed the presence of ochre and that the pigment layer is essentially composed of a mixture of clay and hematite, α-Fe2O3.

Preparação e caracterização de blendas de quitosana/poli(álcool vinílico) reticuladas quimicamente com glutaraldeído para aplicação em engenharia de tecido

In this study, novel Chitosan/PVA based films were chemically crosslinked by glutaraldehyde, under pH=(4,00 ±0,05), in order to achieve structures tailored for wound tissue engineering applications. Both precursors and developed films were characterized by FTIR, SEM and XRD in order to determine the presence of chemicals groups and nanostructural order, respectively. The results have shown that the glutaraldehyde crosslinking have altered the crystallinity of pure chitosan and the increase on the C=N bands and simultaneous decrease on NH2 bands suggested that Chitosan/GA crosslinking has preference to occur in carbon-2 of the saccharide ring by the Schiff's base reaction. Also, FTIR spectroscopy clearly showed that crosslinking has also taken place with blends of PVA and chitosan. The mechanical properties presented high degree dependence with on the increase of the content of chitosan and glutaraldehyde. The results have indicated that, by controlling the ratio [PVA]/[chitosan] in the blends and the extent of chemical crosslinking, it was possible to tailor the hybrid network produced aiming to obtain properties of interest for the specific application.

Obtenção de filmes finos de TiO2 nanoestruturado pelo método dos precursores poliméricos

This work focuses in optimizing setup for obtaining TiO2 thin films by polymeric precursor route due to its advantages on stoichiometric and morphological control. Precursor stoichiometry, synthesis pH, solids concentration and rotation speed at deposition were optimized evaluating thin films morphology and thickness. Thermogravimetry and RMN were applied for precursor's characterization and AFM, XRD and ellipsometry for thin films evaluation. Results showed successful attainment of homogeneous nanocrystalline anatase TiO2 thin films with outstanding control over morphological characteristics, mean grain size of 17 nm, packing densities between 57 and 75%, estimated surface areas of 90 m²/g and monolayers thickness within 20 and 128 nm.

Um novo procedimento de síntese da zeólita A empregando argilas naturais

This work proposes the synthesis of zeolite A by IZA standard proceedures starting from a natural clay. The clay was used in its natural form and after calcination at 900ºC. The resulting materials were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and porosity analysis by nitrogen adsorption. Results showed low surface area for Na-A zeolite in sodium form, but a higher one in CaA based on the nitrogen accessibility. The presence of cubic crystals for the A phase was observed in the SEM micrographies. The new procedure starting from natural clay favors the formation of sodalite while that using the calcinated clay gives A.

Remoção de azul de metileno de solução aquosa usando zeólitas sintetizadas com amostras de cinzas de carvão diferentes

Batch sorption experiments were carried out to remove methylene blue from its aqueous solutions using zeolites synthesized from fly ashes as an adsorbent. The adsorbents were characterized by XFR, XRD and SEM. Nearly 90 min of contact time are found to be sufficient for the adsorption of dye to reach equilibrium. Equilibrium data have been analyzed using Langmuir and Freundlich isotherms and the results were found to be well represented by the Freundlich isotherm equation. Adsorption data were fitted to both Lagergren first-order and pseudo-second-order kinetic models and the data were found to follow pseudo-second-order kinetics.

Caracterização de cinza obtida por combustão de casca de arroz em reator de leito fluidizado

The rice husk combustion in a bubbling and atmospheric fluidized bed reactor was investigated. This paper presents the rice husk ash characterization employing the techniques of X-ray diffraction (XRD), X-ray fluorescence (XRF), and scanning electron microscopy (SEM) among others. After combustion, a rice husk ash containing 93% amorphous silica and <3% unburned char was produced. Methods usually applied to fixed bed considering external sources of energy and high reaction times were employed. Thus, the potential of this type of reactors with respect to speed, continuity and self-sufficiency energy of the process was shown.

Nióbia sintética modificada como catalisador na oxidação de corante orgânico: utilização de H2O2 e O2 atmosférico como oxidantes

In this work synthetic niobia was used to promote the oxidation of methylene blue dye in aqueous medium. The niobia was characterized by N2 adsorption/desorption, XRD and TG measurements. The presence of reactive species on the niobia surface strongly increased the oxidation rate of the methylene blue dye. The reaction mechanism was studied by ESI-MS suggesting that the oxidation of the organic dye involve oxidizing species generated mainly after previous treatment with H2O2. It can be observed that the catalyst is a good material in the activation of gas (atmospheric oxygen) or liquid (hydrogen peroxide) oxidant agent with a total discoloration of the dye solution after only 1 h of reaction.

Remoção de compostos orgânicos em água empregando carvão ativado impregnado com óxido de ferro: ação combinada de adsorção e oxidação em presença de H2O2

In this work, composites based on activated carbon/iron oxide (AC/Fe) were prepared in two different proportions (AC/Fe 5/1 and 1/1) and evaluated in the removal of the organic dye methylene blue (MB). Physical-chemical properties of the composites were determined by X-ray diffraction (XRD), adsorption/dessorption of N2 isotherm, temperature programmed reduction (TPR) and scanning electron microscopy (SEM). Results showed that goethite (α- FeOOH), with nanometer particle size, was formed over carbon surface for both composites. These materials showed high efficiency to remove MB from solution by combined adsorption and oxidation process. The AC/Fe 1/1 showed to be more active in (MB) oxidation then AC/Fe 5/1.

Síntese e caracterização de nanopartículas de óxido de ferro suportadas em matriz carbonácea: remoção do corante orgânico azul de metileno em água

In this work were prepared composites of iron oxide and carbonaceous materials in two different weight proportions (Carbon/Fe 1/1 and 1/2). The physico-chemical properties of the composites were determined by temperature programmed reduction (TPR), adsorption/dessorption of N2, X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS) and pulse titration H2. The XRD and XPS analysis showed a cubic iron oxide phase, identified as maghemite, formed over the carbon surface. The particle size of maghemite showed to be within 10-30 nm. Carbon/Fe 1/2 was the most active in MB removal kinetics and ESI-MS studies showed that MB removal by both composites leads to oxidized intermediates.

Estudo e caracterização da zeólita OFF Tipo T empregando diferentes fontes de silício

Offretite T zeolite was synthesized using different source of Si (Ludox AS-30, Ludox LS-30 and Aerosil 200 Degussa). The obtained materials were characterized by different complementary techniques: XRD, textural analysis by N2 adsorption, IV, SEM and chemistry analysis. This zeolite has an intermediary structure between offretite and erionite zeolites. In all experiments offretite T phase was obtained. Offretite phase presenting better crystalility are obtained in synthesis with stirring and employing aerosil as silicon source. This zeolite presents a potencial application as catalyst for hydroisodewaxing process.

Caracterização e propriedades do material coloidal nanoestruturado β-FeOOH/bentonita

A new mixed material was obtained through the combination of the suspensions of iron oxy-hydroxide and bentonite clay, denoted BFe. Analysis of its structure (XRD, Mossbauer and TGA) and composition (AAS) suggests the maintenance of the layer structure of the clay and an increase in the thermal stability of the BFe. Electrochemical studies performed in different electrolytes show that only in an alkaline medium it is possible to observe the redox peaks relative to the processes involving Fe+2/Fe+3 pair. Tests that evaluated the potential use of the photo-Fenton process showed an efficient degradation process of the dyes in significantly reduced reaction times.

Caracterização de argilas bentonitas e diatomitas e sua aplicação como adsorventes

Five samples of natural clays denominated: diatomite, CN-20, CN-29, CN-40 and CN-45 from Aliança Latina LTDA were characterized by differents supplementary techniques such as: XRD, chemical analysis, adsorption N2 measurements, infrared spectroscopy analysis, thermogravimetric analysis. Clays were tested in adsorption of blue methylene. All of isotherms adjust in a model of physics adsorption with formation of multilayers, however in the case of diatomite was a favorable adsorption (type II) and the CNs were a not favorable adsorption (type III). In the case of CNs had flocculation of clay in high concentration of coloring.