Efeito da temperatura no desempenho catalítico de óxidos de ferro contendo cobre e alumínio

Aluminum and copper doped hematite was evaluated in the high temperature shift (HTS) reaction at several temperatures in order to find catalysts that can work in different operational conditions. It was found that the catalysts work in kinetic regime in the range of 300-400 ºC. Both copper and aluminum increases the activity and selectivity. Aluminum acts as textural promoter whereas copper acts as structural one. The most promising catalyst is that with both copper and aluminum which showed higher activity and selectivity than a commercial sample. This catalyst has the advantages of being non toxic and can work at low temperatures.

Recuperação de sílica-gel utilizando processos oxidativos avançados: uma alternativa simples e de baixo custo

Silica gel is widely used as adsorbent for isolating and purifying natural compounds. Intensive use and high cost make this process expensive and generate solid residues contaminated with many different organic compounds. In the present work a simple method for recycling silica was investigated, by using Advanced Oxidative Processes. Silica gel was treated with H2O2/solar light and compared with a sample treated by conventional methods (high temperature and oxidation with KMnO4). High temperature treatment changes the structure of the silica and, consequently, the separation efficiency. Oxidation by using KMnO4 requires multiple steps and produces residues, including manganese and oxalic acid. The method using H2O2/solar light to recuperate silica gel does not modify its separation efficiency and is less expensive than the traditional methods. Additionally, HPLC and GC-MS analysis indicate that H2O2/solar light eliminates all residues of the silica gel.

Cromatografia unificada

The scope of this study encompasses an overview of the principles of unified chromatography as well as the principles of chromatographic techniques as applied to unified systems, which include gas chromatography, liquid chromatography, supercritical fluid chromatography, high temperature and high pressure liquid chromatography, micro-liquid chromatography, enhanced fluidity chromatography, and solvating gas chromatography. Theoretical considerations and individual instrumental parameters such as mobile phase, sample introduction system, columns, and detection system are also discussed. Future applications of this separation approach are discussed.

Synthesis and NMR characterization of aliphatic-aromatic copolyesters by reaction of poly(ethylene terephthalate) post-consumer and poly(ethylene adipate)

An aliphatic-aromatic copolyester of poly(ethylene terephthalate), PET, and poly(ethylene adipate), PEA, PET-co-PEA, was synthesized by the high temperature melt reaction of post-consumer PET and PEA. As observed by NMR spectroscopy, the reaction yielded random copolyesters in a few minutes through ester-interchange reactions, even without added catalyst. The copolyesters obtained in the presence of a catalyst presented higher intrinsic viscosity than that obtained without the addition of catalyst, due to simultaneous polycondensation and ester-interchange reactions. The structure of the aliphatic-aromatic copolyesters obtained in different PET/PEA ratio is random as observed by NMR analysis.

Filmes de diamante CVD dopado com boro. Parte I . Histórico, produção e caracterização

This review presents a brief account concerning the production, characterization and evolution of the knowledge in the area of diamond and boron-doped diamond films. The most important methods used for the growth of these films, such as chemical vapor deposition and high pressure/high temperature systems, as well as the several kinds of reactors which can be employed are reviewed. However, larger emphasis is given to the CVD method. Morphological, structural and electric properties of these films, as well as their role in the performance of voltammetric electrodes for electrochemistry and electroanalytical chemistry are also discussed.

Remoção de chumbo(II) em sistemas descontínuos por carvões ativados com ácido fosfórico e com vapor

Adsorption of heavy metal cations by activated carbon is dependent on the capacity of the material in promoting adsorption and the time needed to reach equilibrium. Carbon samples were previously activated either by phosphoric acid treatment at 400 ºC or by steam at 800 ºC. The results of Pb(II) adsorption by these activated carbons have shown that equilibrium was typically reached within the first 5 min of contact between carbon and metal solution, with a maximum adsorption capacity higher than 69 mg g-1 for the vapor-activated sample. Temperature influences the sorption capacity, which corresponds to an endothermic process. Lead(II) retention is more pronounced at high temperature and low pH.

Micro- and nanostructuring of poly(ethylene-2,6-naphthalate) surfaces, for biomedical applications, using polymer replication techniques

Here we investigate the formation of superficial micro- and nanostructures in poly(ethylene-2,6-naphthalate) (PEN), with a view to their use in biomedical device applications, and compare its performance with a polymer commonly used for the fabrication of these devices, poly(methyl methacrylate) (PMMA). The PEN is found to replicate both micro- and nanostructures in its surface, albeit requiring more forceful replication conditions than PMMA, producing a slight increase in surface hydrophilicity. This ability to form micro/nanostructures, allied to biocompatibility and good optical transparency, suggests that PEN could be a useful material for production of, or for incorporation into, transparent devices for biomedical applications. Such devices will be able to be autoclaved, due to the polymer's high temperature stability, and will be useful for applications where forceful experimental conditions are required, due to a superior chemical resistance over PMMA.

The role of bound chlorine in the brightness reversion of bleached hardwood kraft pulp

Our previous paper showed fragmentary evidence that pulp brightness reversion may be negatively affected by its organically bound chlorine (OX) content. A thorough investigation on eucalyptus kraft pulp led to the conclusion that OX increases reversion of certain pulps but this trend is not universal. Alkaline bleaching stages decrease reversion regardless of pulp OX content. Pulps bleached with high temperature chlorine dioxide revert less than those bleached with conventional chlorine dioxide in sequences ending with a chlorine dioxide stage but similarly in sequences ending with a final peroxide stage. The use of secondary condensate for pulp washing decreases reversion.

Termocromismo em soluções de alcóxidos de Vanádio(IV): uma abordagem pela modelagem molecular

The thermochromic behavior exhibited by vanadium(IV) alkoxides, [V2(μ-OPr i)2(OPr i) 6] and [V2(μ-ONep)2(ONep)6 ], OPr i = isopropoxide and ONep = neopentoxide, was studied by molecular modeling using DFT, TDDFT and INDO/S methods. The vibrational and electronic spectra calculated for [V2(μ-OPr i)2(OPr i) 6] were very similar to the experimental data registered for crystalline samples of the complex and for its solutions at low temperature (< 210 K), while spectra recorded at high temperature (> 315 K) were compatible with those calculated for the monomeric form, [V(OPr i)4]. These results consistently point to a monomer/dimer equilibrium as an explanation for the solution thermochromism of {V(OPr i)4}n. In spite of the structural similarity between [V2(μ-ONep)2(ONep)6 ] and [V2(μ-OPr i)2(OPr i) 6] in the solid state, the thermochromic behavior of the former could not be explained by the same model, and the possibility of tetranuclear aggregation at low temperatures was also investigated.

Hidrólise do óleo de Azadirachta indica em água subcrítica e determinação da composição dos triacilglicerídeos e ácidos graxos por cromatografia gasosa de alta resolução a alta temperatura e cromatografia gasosa de alta resolução acoplada à espectrometria de massas

The development of modern analytical tools plays an important role in quality control. The main purpose of this study was to explore the use of subcritical water as a versatile analytical tool, employed simultaneously as a reagent and solvent, as well as the application of high temperature-high resolution gas chromatography (HT-HRGC) to develop a procedure for the analysis of triacylglycerides and fatty acids in Azadirachta indica A. Juss. (Neem) oil without the need for solvents, chemical reagents, or catalytic agents. The developed method presented satisfactory results and is in agreement with the concepts of Green Analytical Chemistry (GAC).

Possibilidades e limitações no uso da temperatura em cromatografia líquida de fase reversa

High-temperature liquid chromatography (HTLC) is a technique that presents a series of advantages in liquid phase separations, such as: reduced analysis time, reduced pressure drop, reduced asymmetry factors, modified retentions, controlled selectivities, better efficiencies and improved detectivities, as well as permitting green chromatography. The practical limitations that relate to instrumentation and to stationary phase instability are being resolved and this technique is now ready to be applied for routine determinations.

Desenvolvimento e avaliação de um porta-amostra de baixo custo para caracterização elétrica de materiais cerâmicos

Conventional sample holder cells used to the electric characterization of ceramics at high temperature consists of an alumina tube and platinum wires and plates using a complex design. The high cost materials used in the conventional sampler holder cell were replaced by stainless steel and conventional ceramics. The sample holder was validated by characterizing yttria-stabilized-zirconia in a temperature range of 25 to 700 ºC. The results do not present variations, discontinuity or unusual noise in the electric signals. Several samples were characterized without maintenance, which demonstrates that the sample holder is electric and mechanic adequate to be used to electrical characterization of ceramics up to 700 ºC.

Construção de uma célula-autoclave para medidas eletroquímicas a altas temperaturas

Measurements at high temperature using liquid solutions require special cells and materials which are able to support the temperature and pressure developed inside. The constructed cell was designed to support pressures up to 20 bar, temperatures relatively high up to around 200 ºC, depending on the pressure developed inside the system. It also supports aggressive solutions since its inner wall is made of Teflon. The electrolyte has no contact with the metallic body of the cell. Then, it is supposed that this work represents a great contribution to the electrochemical studies of materials in solutions at high pressure and temperature

Extração de bifenilas policloradas de amostras de leite materno: otimização univariada versus planejamento experimental

The convenience of the multivariate optimization of SPME procedures through ANOVA calculated using Doehlert designs has been demonstrated for twelve PCBs in the complex matrix of milk. For this study, the main parameters of the extraction were selected and valued through univariate and multivariate optimization. In addition, the analysis of variance allowed identification of the statistically significant variables in this model: high temperature (95 ºC) and ionic strength (36% m/v) proved significant for all the PCBs while intermediate time (70 min) and low methanol concentration (5% v/v) also contributed to the extraction of the majority of these PCBs.

Máscaras mecânicas de sombra por eletrocorrosão para dispositivos eletro-ópticos

Shadow masks are used in manufacturing processes for electro-optic devices to transfer patterns with different shapes and dimensions. For fabrication of organic based devices, shadow masks should be made of materials stable against organic solvents, high temperature, and robust, remaining unchanged after multiple cycles of use and fixation. Thus, stainless steel is suitable for shadow masks. A simple, cheap and quick method of obtaining shadow masks by electrochemical corrosion of stainless steel is reported. The shadow mask was used to evaporate cathode material to obtain an organic light emitting diode with active area of 9 mm². This device exhibited a turn-on voltage of 5 V and luminance of 14 cd/m².