Pilarização de esmectita brasileira para fins catalíticos. Emprego de argila pilarizada na alquilação de benzeno com 1-dodeceno

Al-pillared clay was prepared with a Brazilian bentonite from the Campina Grande region (Paraíba, BRAZIL). It was intercalated at 298 K, during 48 hours, with a solution containing [Al3+] = 0.10 mol/L and molar ratio OH/Al = 2.0 prepared at 333 K, and was calcined at 773K. The catalytic activity was evaluated by alkylation of benzene with 1-dodecene. The characterization methods were: X-ray fluorescence and diffraction analysis; 27Al, 29Si and 23Na MAS NMR and textural analysis by N2 adsorption. The thermal stability of the natural clay was improved by the pillaring procedure, as well as the catalytic activity. The intercalated clay presented the highest initial rate of reaction among the systems tested.

Extração de ferro de esmectita brasileira com emprego do método ditionito-citrato-bicarbonato

A natural clay from Campina Grande region (Paraíba, Brazil), with 8.57% of Fe2O3, was used to study the most appropriate condition to carry out the iron extraction, without altering the clay structure in a significant way. Samples were treated with the Dithionite-Citrate-Bicarbonate method (DCB) for 30 and 120 minutes (pH=9.1), and also with citric acid (pH=1.8; time=15min), at 75°C. Conductivity measurements, X-ray fluorescence, X-ray diffraction, energy-dispersive spectrometry, electron-diffraction with transmission electron microscopy and textural evaluation by nitrogen adsorption were done. The treatment in a basic medium was more selective for iron removal than in acid condition. The time of 30 minutes, with 1.6 g Na2S2O4/10 g clay, was the best condition for the iron extraction.

Emprego da amostragem de suspensão na determinação de Cu e Zn em lapa antártica e Ni em sedimento de rio por espectrometria de absorção atômica com chama

In order to demonstrate the feasibility of slurry sampling for environmental studies, different methodologies were developed for Cu and Zn in antarctic limpets and Ni in river sediment with FAAS detection. Studies focusing particle size, acid concentration, slurry stability, selectivity, among others were carried out in order to define the better conditions for slurry analysis. A study related to the depth profile for Ni in the Atibaia River sediment was made after optimization conditions for this element. For accuracy check, certified reference material was used as well as decomposition with microwave oven.

Emprego de planejamento fatorial para a otimização das temperaturas de pirólise e atomização de Al, Cd, Mo e Pb por ETAAS

This work describes a factorial design for the optimization of pyrolysis and atomization temperatures in ETAAS. As examples, Cd and Pb were determined using lower pyrolysis and atomization temperatures and Al and Mo with higher pyrolysis and atomization temperatures. Good results were obtained for Cd employing Rh (m o = 1.4 pg) as a permanent modifier with pyrolysis and atomization temperatures of 640 and 1500 °C, respectively. For Zr, W or Zr+W, the Cd pyrolysis and atomization temperatures were 500 and 1500 °C, respectively, with m o = 1.4 pg using Zr or W and 1.5 pg using Zr+W. The best results for Pb were those using Rh, Zr, W and Zr+Rh, obtaining characteristic masses of 42, 37, 34 and 36 pg, respectively. Pyrolysis and atomization temperatures of 910 and 1850 °C, respectively, were achieved for this metal. For Al, the best results were obtained when Zr or Zr+W were used. Mo was also tested as a possible permanent modifier for Al, but the results were not satisfactory. The results obtained for Mo without modifier were similar to those with conventional modifiers (Mg or Pd+Mg) and the results obtained using permanent chemical modifiers were not satisfactory. In all situations, the experiments were performed faster than those using the univariate procedure.

Emprego de reagente em suspensão em sistema de injeção em fluxo: determinação espectrofotométrica de sulfato em águas naturais

This paper presents an automatic procedure employing a reagent in the form of a slurry in a flow-injection system. The feasibility of the proposal is demonstrated by sulphate determination in water using the Barium Chloranilate method, which is based on the precipitation of barium sulphate. The release of a stoichiometric amount of highly colored chloranilic ions is monitored at 528 nm. The reaction is carried out in alcoholic medium in order to reduce the solubility of the reagent. A considerable improvement in the sensitivity is attained by adding ferric ions to the released chloranilic ions. An on-line filtration step to separate the excess reagent from the released chloranilic ions was necessary. In addition, a column containing a cation exchange resin was included in the manifold to remove potentially interfering ions. The proposed procedure is suitable for 30 determinations per hour and the relative standard deviation is less than 2%. The analytical curve is linear between 0.0 and 40 mg L-1 and the determination limit is about 2.0 mg L-1SO4(2-). Accuracy was confirmed by running several samples already analysed by a standard turbidimetric procedure.

Emprego de monocamadas auto-organizadas no desenvolvimento de sensores eletroquímicos

Self-assembled monolayers (SAMs) modified electrodes exhibit unique behavior that can greatly benefit electrochemical sensing. This brief review highlights the applications of SAM modified electrodes in electroanalytical chemistry. After a general introduction, which includes the approaches for SAM development, different electrochemical systems for detecting inorganic and organic species are described and discussed. Special attention to the coupling of biological sensing element to the SAM is given, which can selectively recognize the analyte. Future prospects are also evaluated.

Síntese do isobutileno e seu emprego em reações de esterificação: propostas de aulas práticas de química orgânica para a graduação

An experiment for the synthesis of isobutylene from tert-butanol dehydratation using oxalic acid as catalyst, followed by preparations of tert-butyl benzoate and tert-butyl cinnamate is described. The synthesis are simple, requiring two periods of 4 hours and are suitable for undergraduate organic chemistry experimental courses.

Emprego de padrão único para a construção de curvas analíticas em sistema de análise por injeção em fluxo associado à espectrofotometria em fase sólida

In this work two procedures were proposed for analytical curves construction using a single standard solution employing a flow injection system with solid phase spectrophotometric detection (FI-SPS). A flow cell contends the chromogenic reagent 1-(2-tiazolylazo)-2-naphtol was positioned on the optical path. The first procedure was based on controlled concentration of analyte on solid phase and the relations between absorbance and the total volume of injected allowed the calculation of analyte concentration. The second procedure was developed employing controlled dispersion/retention in flow system where analyte concentration was obtained by exploiting the relation between transient signals of samples and single standard solution at equivalent reading time. The procedures were successfully applied for zinc determination in synthetic solutions with good precision and accuracy at 95% confidence level.

Emprego de óxidos tipo perovskita nas oxidações do propano e CO

Simultaneous oxidation/co-precipitation of an equimolar mixture of La(III) and Co(II) nitrates and La(III) nitrate and Mn(II) chloride afforded a hydroxide gel, which was converted to LaCoO3 and LaMnO3 on calcination at 600 °C. After calcination, the obtained perovskites have been characterised by X-ray diffraction (XRD), X- ray photoelectron spectroscopy (XPS), thermogravimetric analysis (DTA - TGA) and BET specific surface determination. Specific surface areas of perovskites were 12 - 60 m²/g. XRD analysis showed that LaCoO3 and LaMnO3 are simple phase perovskite - type oxides. Traces of LaOCl, in addition to the perovskite were detected in the LaMnO3. The catalytic behavior was examined in the propane and CO oxidation. The LaCoO3 catalyst was more active to CO2 than the LaMnO3 catalyst.

O emprego de fermento de pão, Saccharomyces cerevisiae, na síntese de feromônios

The use of pheromones in integrated pest management has been increasing in the last years due to environmental concern. This development is accompanied by the search for simple, efficient and less aggressive synthetic methodologies for the preparation of pheromones. One of these methodologies includes microbiological reactions, more specifically biocatalytic reduction of carbonyl compounds using baker's yeast (Saccharomyces cerevisiae). This review presents the use of baker's yeast as an easy and cheap alternative to obtain enantiomerically enriched compounds employed in the synthesis of pheromones.

Emprego de catalisadores à base de níquel para homo- e copolimerização de estireno

This review deals with the homo- and copolymerization of styrene with nickel catalysts. The catalytic activity, polymer stereoregularity, polymer molecular weight and polydispersity are dependent upon nickel ligands and reaction parameters. Catalysts supported on silica, treated with methylaluminoxane (MAO), have shown higher stereospecificity and activity compared to homogeneous ones. The influence of these parameters is discussed focusing on the elucidation of some aspects of the polymerization mechanism.

Emprego de compostos organometálicos mononucleares de paládio(II) na ativação de macrófagos peritoneais de camundongos

The immune responses are mediated by a variety of cells that, when activated, produce a number of molecules. Macrophages are the first cells to take part in the immune response releasing many compounds in the extracellular environment such as H2O2. Taking into account this aspect we evaluated the activation of an immunological system, in vitro, by determining the H2O2 released in cultures of peritoneal macrophage cells from Swiss mice in the presence of organopalladated compounds of the type [Pd(dmba)(X)(dppp)], dmba = N,N-dimethylbenzylamine, dppp = 1,3-bis(diphenylphosphine)propane, X = Cl, N3, NCO, NCS. An excellent activation of macrophages by the [Pd(dmba)(X)(dppp)] compounds was observed and the influence of the X ligand on the immune response could be verified.

Emprego do carvão ativado para remoção de cobre em cachaça

Copper content is of great concern among sugarcane-spirit producers. It is released from copper-made distillers, during the distillation process. Activated carbon has been used to remove copper. However, depending on the amount of carbon and the duration of reaction, it can also remove higher alcohols and esters, which are important in the final product. A sugarcane spirit with 9 mg L-1 of copper was shaken with 2 to 26 g L-1 of activated carbon, during 10 to 1440 minutes. Then, copper and organic compounds were measured. At least 12 g L-1 of carbon and 60 min shaking time were necessary to decrease copper bellow 5 mg L-1. However, other components of the product were also affected.

O emprego de quitosana quimicamente modificada com anidrido succínico na adsorção de azul de metileno

The adsorption capacity of alpha-chitosan and its modified form with succinic anhydride was compared with the traditional adsorbent active carbon by using the dye methylene blue, employed in the textile industry. The isotherms for both biopolymers were classified as SSA systems in the Giles model, more specifically in L class and subgroup 3. The dye concentration in the supernatant in the adsorption assay was determined through electronic spectroscopy. By calorimetric titration thermodynamic data of the interaction between methyene blue and the chemically modified chitosan at the solid/liquid interface were obtained. The enthalpy of the dye/chitosan interaction gave 2.47 ± 0.02 kJ mol-1 with an equilibrium constant of 7350 ± 10 and for the carbon/dye interaction this constant gave 5951 ± 8. The spontaneity of these adsorptions are reflected by the free Gibbs energies of -22.1 ± 0.4 and -21.5 ± 0.2 kJ mol-1, respectively, found for these systems. This new adsorbent derived from a natural polysaccharide is as efficient as activated carbon. However 97% of the bonded dye can be eluted by sodium chloride solution, while this same operation elutes only 42% from carbon. Chitosan is efficient in dye removal with the additional advantage of being cheap, non-toxic, biocompatible and biodegradable.