Pré-concentração de nitrosaminas a partir de amostras aquosas por extração em fase sólida e cromatografia capilar eletrocinética micelar

This paper describes the development of a methodology for solid phase extraction (SPE) and pre-concentration of nitrosamines from aqueous samples using granular activated charcoal as stationary phase. micelar electrokinetic capillary Chromatography (MEKC) was used for the separation and identification of the nitrosamines in the extracts. Using a sample with 50 µg l-1 of each nitrosamines standards (dimethylnitrosamine, DMN; diethylnitrosamine, DEN; N-nitrosopyrrolidine, NPYR; N-nitrosopiperidine, NPIP; N-nitrosomorpholine, NMOR), the methodology showed a range of recuperation from 29 to 107% with a linear zone between 10 and 500 µg l-1. The developed methodology can be applicable to the determination of these analytes in different aqueous samples.

Avaliação do nível da vulnerabilidade do solo devido à presença de termelétrica a carvão (Figueira, PR- Brasil)

Rainwater samples were analyzed during a one-year period (June 1999 - June 2000) and presented concentration of pH = 4.9 (volume weight mean). The ions concentrations results showed a high sulfate concentration (35 µmol L-1), followed by the cations concentration of sodium, calcium and ammonium (35, 16 and 30 µmol L-1, respectively). Due to the great contribution of these cations in the sulfate neutralization action, the rainwater of this region had only a light acid characteristic. The soil characteristic was acid and the bioavailable concentration of the alkaline cations (Ca, Mg and K) presented high calcium concentrations (1001 ± 357 mg kg-1) compared with the other cations. The determination of soil sensitivity to acid rain was calculated by the ratio BC/Al3+ (BC = Ca2+ + Mg2+ + K+) and presented the average value of 5.1 ± 3.3. This preliminary evaluation of soil susceptibility by the ratio BC/Al3+ showed that the local soil and vegetation type (tropical Savannah) were sensitive to acid deposition. The long term of this impacting condition (acid rain, high sulfate deposition) could be harmful to the soil and vegetation quality.

Aspectos regio- e estereoquímicos da adição de Michael assimétrica via iminas quirais com centros estereogênicos pré-existentes

The asymmetric Michael addition reactions using chiral imines, under neutral conditions (deracemizing alkylation process), constitute one of the main methods for the stereocontrolled elaboration of quaternary carbon centers. This protocol is based on the conjugate addition of secondary chiral enamines to electron-deficient alkenes. The focus of this report deals with the discussion of regio- and stereochemical aspects of the deracemizing alkylation process concerning enamines bearing a resident chiral center.

O uso de radiação ultravioleta para o pré-tratamento de amostras em análise inorgânica

The basic principles of UV irradiation as sample pre-treatment step and its potential for inorganic analysis are illustrated and discussed through significant examples from the literature. Not only does this overview cover the classical applications of this technique in the decomposition of organic matter in electroanalysis, but it also presents recent trends, including the increasing interest in employing UV irradiation in flow analytical systems, successful attempts to enhance its effectiveness and the coupling with chromatographic and spectroscopic methodologies. Furthermore, a number of relevant cases of UV-driven derivatization reactions involving photo-sensitive inorganic species are presented, showing some convenient options to perform fast and reliable determination of inorganic and organic analytes.

Tratamento dos resíduos gerados na síntese de polianilina em escala pré-piloto

Polyaniline (PAni) is one of the most studied conducting polymer. It can be synthesized by two methods: electrochemical or chemical oxidation. The chemical oxidation is more adequate to produce large quantities of polymer. Regardless of the synthesis scale, the treatment of the residues before its final destination is very important and necessary because it contains toxic aniline derivatives (carcinogens in some cases), acids and inorganic salts, both with low toxicity. In this work we discuss the methods used to treat these residues and to eliminate and discard the toxic substances. These were extracted from the reaction residues by using activated coal and the pH of the residue was neutralized.