SILICA MORPHOLOGY CHARACTERIZED BY SEM - THE EFFECTS OF THE SOLVENT TREATMENT AND THE DRYING PROCESS

Scanning electron microscopy (SEM) was used to investigated the effects of volatile solvents (such as water, propanone, ethanol, methanol or ethyl ether), treatment and drying processes, microwave ovens, drying ovens, and vacuum desiccators or freeze driers, on silica morphology. Silica gel was obtained from diluted sodium silicate (1:5 w/w SiO2:H2O). The results showed that the drying process based on freeze drying is more efficient for structural conservation of the precipitate. Treatment with volatile solvents does not change the shape of the aggregates, but has an important role in the determination of aggregate surface roughness.

Estudo das propriedades de troca iônica e/ou adsorção da celulose e celuloses modificadas

In this work it was studied the capacity of cellulose and chemically modified celluloses (carboxymethylcellulose, cellulose phosphate and oxicellulose) to adsorb copper(II) cations of aqueous and non aqueous solutions. The influence of the principal physical chemical parameters on the adsorption process was examined using the batch adsorption method and copper(II) perchlorate solutions, the maximum adsorption capacity determined for adsorbents were as follows (mol.g(-1)): cellulose, 0.54 . 10(-5); carboxymethylcellulose, 1.28 . 10(-4); cellulose phosphate, 1.12 . 10(-4); oxicellulose, 0.38 . 10(-4).

O comportamento fotoquímico dos complexos pentaaminas de rutênio(II) com ligantes pi insaturados

A general overview on the photochemical behaviour of [Ru(NH3)(5)L](2+) complexes (where L is a pi ligand) is presented. The proposed mechanisms and techniques employed for the study of these reactions are discussed. Emphasis is made on the mechanisms that allow the identification of the reactive excited state of the [Ru(NH3)(5)py](2+) complex.

CONTRIBUTION TO THE STUDY OF ZIRCONIUM AND HAFNIUM ALPHA-HYDROXYCARBOXYLATES

A study of both zirconium and hafnium alpha-hydroxycarboxylates for analytical applications is presented, These compounds are studied by infrared spectroscopy, thermal analysis and X-ray diffractometry. dl-Mandelic, dl-p-bromomandelic and dl-2-naphthylglycolic acids are the more adequate reagents for gravimetric determinations of zirconium and hafnium, the ligands dl-2-hydroxyhexanoic and dl-2-hydroxydodecanoic acids were used for the first time and the results showed that they are also adequate reagents for the same purpose.

Antifungal iridoids from the stems of Tocoyena formosa

A new antifungal iridoid compound, together with three active known iridoids, galioside, galioside aglucone, and apodanthoside, as well as 3-O-beta-D-glucopyranosyl-28-O-beta-D-glucopyranosyl quinovic acid and quercetin-3-O-methyl-3-O-beta-D-rhamnopyranoside, were isolated from the stems of Tocoyena formosa. This new compound was characterized by spectral data as 11-O-trans-feruloylteucrein.

Validação de métodos para determinação do teor de 3-hidroxibutirato e 3-hidroxivalerato em polímero biodegradável

The efficiency of two methods for determining 3-hydroxybutyrate and 3-hydroxyvalerate content in the biopolymer (poly(3-hydroxybutyrate-co-3-hydroxyvalerate) has been evaluated. Both methods are based on (a) the hydrolysis of polymers, (b) the esterification with methyl (method A) and isoamilic alcohol (method B) and (c) analysis of the esters by gas chromatography using flame ionization detection (GC-FID). After optimization of the analytical conditions, the main validation parameters (linearity, quantification limit, detection limit, recovery, sensitivity and precision) were determined showing that both analytical procedures can be applied to control the process of poly(3-hydroxybutyrate) production. However, method B gives better analytical results than method A and has the advantage of not using chlorinated solvents.

Decomposição de argilas em forno de microondas e determinação simultânea dos seus constituintes principais por espectrometria de emissão óptica em plasma indutivamente acoplado

ANALYSIS OF CLAYS BY INDUCTIVELY COUPLED PLASMA OPTICAL EMISSION SPECTROMETRY AFTER CLOSED-VESSEL MICROWAVE-ASSISTED ACID DECOMPOSITION. In this work a closed-vessel microwave-assisted acid decomposition procedure for clays was developed. Aluminum, Ca, Fe, K, Mg, Na, Si, and Ti were determined in clay digestates by inductively coupled plasma optical emission spectrometry. The most critical parameter for total decomposition of clays was the composition of the reagent mixture. The applied power and the heating time exerted a less critical influence. Best decomposition conditions were attained using a reagent mixture containing 4 mL aqua regia plus 3 mL HF and the heating program was implemented in 12 min. The accuracy of the results was demonstrated using two standard reference materials and a paired t-test showed a good agreement between determined and certified values at a 95% confidence level.

Influence of experimental factors on results of thermogravimetric analysis

Thermogravimetric results are influenced by a series of experimental factors, such as furnace heating rate and atmosphere, velocity of carrier gas, sample mass, etc. In this work a practical evaluation of these parameters are showed for calcium oxalate, with teaching objectives, considering that undergraduate text books discuss but do not show experimental details for these cases.

Cyclometallated compounds of intramolecular coordination.

This article supplies a review on the chemistry of cyclometallated compounds. Emphasis is given to those formed by cyclometallation reactions. In this class of complexes, called organometallic intramolecular-coordination compounds, a special attention is given to the reactivity of cyclometallated of palladium(II) due to their use in important chemical processes. Metal-carbon bonds in these palladium(II) complexes can undergo a large variety of insertion reactions and they offer a potentially important sequence in organic synthetic methodology,homogeneous catalysis and liquid crystals manufacturing.

Thermal behaviour of polymetallic metal carbonyls with Fe-Fe, Fe-Hg and Hg-Hg bonds containing Lewis bases.

The thermal behaviour of polymetallic metal carbonyls containing Fe-Fe, Fe-Hg and Hg-Hg bonds and Lewis bases, such as [Fe-3(CO)(8)(L)(2)] (L = 1,10-phenantroline,2,2'-bipyridine), [Fe(CO)(4)(HgCl)(2)] and [Fe(CO)(4)(HgCl)(2)(L)(2)] (L = 1,10-phenantroline,2-quinolinethiol), have been investigated by thermal analysis (TG), Thermal studies give evidence that the thermal decomposition mechanisms and starting temperatures are strongly influenced by the Lewis bases. The thermal decompositions under synthetic air yielded, in all cases, the final solid product Fe2O3 which presence was confirmed by X-ray powder diffraction technique.

Manganese Phthalocyanine as a Biomimetic Electrocatalyst for Phenols in the Development of an Amperometric Sensor

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)

Construction and application of an electrochemical sensor for paracetamol determination based on iron tetrapyridinoporphyrazine as a biomimetic catalyst of P450 enzyme

This work describes the construction and application of a biomimetic sensor for paracetamol determination in different samples. The sensor was prepared by modifying a glassy carbon electrode surface with a Nafion (R) membrane doped with FeTPyPz. The best performance of the sensor in 0.1 mol L-1 acetate buffer was at pH 3.6. Under these conditions, an oxidation potential of paracetamol was observed at 445 mV vs. Ag vertical bar AgCl. The sensor presented a linear response range between 4.0 and 420 mu mol L-1, a sensitivity of 46.015 mA L mol(-1) cm(-2), quantification and detection limits of 4.0 mu mol L-1 and 1.2 mu mol L-1, respectively. A detailed investigation about its electrochemical behavior and selectivity was carried out. The results suggested that FeTPyPz presents catalytic properties similar to P450 enzyme for paracetamol oxidation. Finally, the sensor was applied for paracetamol determination in commercial drugs and for the monitoring of its degradation in an electrochemical batch reactor effluent.

Synthesis, X-ray Crystal Structure and Theoretical Calculations of Antileishmanial Neolignan Analogues

Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)

Influence of Sources and Meteorology on Surface Concentrations of Gases and Aerosols in a Coastal Industrial Complex

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)