Eletroforese capilar acoplada à espectrometria de massas (CE-MS): vinte anos de desenvolvimento

CE-MS has been increasingly used for analysis of a vast array of compounds. This article reviews the different electrophoretic modes, interfaces and mass analyzers that are commonly used in the CE-MS coupling, as well as the technique advantages and performance characteristics. A large compilation of CE-MS applications is also presented. Therefore, this review is both a guide for beginners and a collection of key references for people who are familiar to the technique. Furthermore, this is the first CE-MS review published in a Brazilian journal and marks the installation of the first two commercial CE-MS units in Sao Paulo State.

Avaliação da contaminação do Igarapé do Sabino (Bacia do Rio Tibiri) por metais pesados, originados dos resíduos e efluentes do Aterro da Ribeira, em São Luís, Maranhão

This work aimed to carry out an environmental monitoring in sabino narrow river (affluent of Tibiri Basin, in São Luís - MA, Brazil), in order to verify the main environmental impacts caused by effluent residues from Ribeira landfill. Chemical analysis and bibliographic and cartographic researches on this ecosystem were also carried out. In addition, heavy metals, such as Hg, Pb and Zn, were investigated in water samples by ICP-MS technique. It was observed that the contents of such heavy metals were above the tolerance limits established by the Brazilian legislation, showing a strong impact level on the evaluated ecosystem.

Estratégias de pré-concentração em eletroforese capilar (CE): parte 1. Manipulação da velocidade eletroforética do analito

Capillary electrophoresis has become a well-established and routine-based separation technique. It is based on the differences between charged analyte mobility in aqueous or organic electrolytes. Its major limitation is the sensitivity due to small sample injection volumes and the narrow diameter of the capillaries, especially when UV detection is used. There are a number of ways to increase the concentration sensitivity. This report shows some on-line preconcentration strategies to perform it in free solution capillary electrophoresis that are based on manipulation of the analyte electrophoretic velocity during the sample introduction (stacking, field amplification and transient isotachophoresis).

Nutrientes (K, P, Ca, Na, Mg e Fe) em sedimentos (solos aluviais) e cultivares (feijão e milho) de praias e barrancos de rios de água branca: a bacia do purus no estado do Acre, Brasil

The present research highlights the macronutrient abundance in the sediments of beaches and cliffs and cultivates in the river Purus and flowing, southwest of Amazon. The concentrations found in leaves and bean seeds and corn leaves reflect the mineralogical and chemical nature of those rich sediments in K2O and Na2O, which are formed by smectite, illite and K-feldspar. The factors of transfer of the elements in the corn leaves and bean (Ca>K>Na) and bean seeds (Na>K>Ca) demonstrate that the nutrient needs of the cultivate were found appropriately in the sediments (soils) of the beaches and cliffs.

Remoção de Pb2+ e Cr3+ em solução por zeólitas naturais associadas a rochas eruptivas da formação serra geral, bacia sedimentar do Paraná

The capacity of natural zeolites and its host rock (dacite) to remove Pb2+ and Cr3+ from aqueous solutions has been investigated. Results showed that both samples prefer to remove Pb2+ instead of Cr3+. Almost 100% of Pb2+ was removed from solutions with concentration until 50 mg L-1 and 100 mg L-1 of this metal, respectively by dacite and zeolite. The equilibrium of metals adsorption process was reached during the first 30 min by both materials. Na+ can be used to recover Pb2+, but not to remove Cr3+ from the treated samples. The Sips model showed a good fit for experimental data of this study.

Avaliação da qualidade de sedimentos - estudo de caso: sub-bacia do Ribeirão Espírito Santo, afluente do Rio São Francisco

This study evaluated the environmental impact resulting from surface water and sediment contamination by metals in a watershed affected by a tailing basin that controls effluents coming from a zinc-ore beneficiation plant. The studies combined assessments of sediment chemistry (exceedances of sediment quality guidelines), benthic assemblage structure and acute and chronic ecotoxicity. The results showed that the levels of metal contamination in sediments are not yet enough to cause deleterious effects to the biota. However, the ecotoxicity tests indicated the occurrence of chronic effects, demonstrating that other factors, as the use of fertilizers, could also be a source of contamination.

Emissões naturais e antrópicas de metais e nutrientes para a bacia inferior do rio de contas, Bahia

Emission factors of anthropogenic activities and natural processes were used to estimate nutrients and metals loads to the Contas River lower basin, Southern Bahia, Brazil. Among natural sources, emission from soil leaching is larger for N, Cu and Pb. Atmospheric deposition is the major natural source of P, Zn, Cd and Hg. Among anthropogenic sources, agriculture is the major source of N, Cu and P. Urban sources are the major contributors to the other elements. Present anthropogenic land uses are already responsible for 78 and 99% of total N and P loads and about 50% of total Cu and Hg.

A qualidade de água como indicador de uso e ocupação do solo: bacia do Gama - Distrito Federal

The spread of Brasília isn't accompanied by correct support of land occupation, situation that is reflected in water quality. Under the optics of land use and occupation, working with multivariate statistics as main tool, water physical and chemical quality of Gama Catchment were assessed. During two years samples were collected and analyzed for 24 parameters. The statistical analysis showed the influence of civil buildings, agricultural activities and the best statistical parameters to a quickly assessment: nitrate, ammonia, suspended solids and aluminium.

Determination of cetirizine in tablets and compounded capsules: comparative study between CE and HPLC

A capillary electrophoresis (CE) method was developed and validated for determination of cetirizine dihydrochloride in tablets and compounded capsules. The electrophoretic separation was performed in an uncoated fused-silica capillary (40 cm x 50 μm i.d.) using 20 mmol L-1 sodium tetraborate buffer (pH 9.3) as background electrolyte, a hydrodinamic sample injection at 50 mBar for 5 s, 20 KV applied voltage at 25 °C, and detection at 232 nm. The proposed method was compared with the high performance liquid chromatographic (HPLC) method previously validated for this drug, and statistical analysis showed no significant difference between the techniques.

Distribuição de Hg total e suas associações com diferentes suportes geoquímicos em sedimentos marinhos da margem continental brasileira: Bacia de Campos - Rio de Janeiro

Mercury distribution and geochemical support on the Continental Margin was evaluated at the Campos Basin, Rio de Janeiro state, Brazil. The average concentrations for all analyzed elements were, respectively, 20 ± 5 ng g-1 (Hg); 30 ± 14 mg g-1 (Al); 16 ± 6 mg g-1 (Fe), and 254 ± 83 µg g-1 (Mn). Silt and clay content, total carbonate and Hg, and organic carbon increased with depth. Finally, the relationship between Hg and silt clay showed significant positive correlation. Total Hg concentrations are the background level described primarily (~40 ng g-1).

Avaliação e identificação de parâmetros importantes para a qualidade de corpos d'água no semiárido baiano. Estudo de caso: bacia hidrográfica do rio Salitre

Objective of this work was identifying superficial water quality parameters, significant to semi-arid hydrographic basins, minimizing costs of water monitoring. The Salitre river basin, an important sub-basin of the São Francisco river, was used as a case study. STD, Cl-, DO, BOD, pH, NO3-, PO4(3-), Al, Cu, Fe, Mn, Ni and Pb were considered the most significant parameters, with concentration levels found in some stretches of the basin not compliant with the current legislation. Some of the Salitre river basin sediments may represent a risk to the quality of the water body in relation to levels of nickel and zinc.

Composição química das águas pluviais e deposição atmosférica anual na bacia do Alto Sorocaba (SP)

Two sampling points were chosen and forty samples were collected between January and December 2006 at Alto Sorocaba basin. The rainwater pH varied from 5.46 to 6.36 (Ibiúna) and 5.26 to 6.81 (Itupararanga), being Ca2+ the main ion responsible for controlling the rainwater pH. The ionic concentrations decreased in the following order: Ca2 +>Na+> Mg2+>K+ for cations and SO4(2-)>HCO3->NO 3->Cl- >PO4(3-) for anions. The annual atmospheric deposition appeared to be controlled mostly by following sources: mining activities and cement factories (Ca2+ and HCO3-), natural soil dust (Na+, Mg2+ and HCO3-), fossil fuel burning (SO4(2-)) and agriculture activities (K+, NO3- and PO4(3-)).

Ce - promoted catalyst from hydrotalcites for CO2 reforming of methane: calcination temperature effect

Ce-promoted Ni-catalysts from hydrotalcites were obtained. The effect of calcination temperature on the chemical and physical properties of the catalysts was studied. Several techniques were used to determine the chemical and physical characteristics of oxides. The apparent activation energies of reduction were determined. Catalytic experiments at 48 L g-1h-1 without pre-reduction in CO2 reforming of methane were performed. The spinel-like phase in these oxides was only formed at 1000 ºC. The reduction of Ni2+ in the oxides was clearly affected by the calcination temperature which was correlated with catalytic performance. The catalyst calcined at 700 ºC showed the greatest activity.

Emissões naturais e antrópicas de nitrogênio, fósforo e metais para a bacia do Rio Macaé (Macaé, RJ, Brasil) sob influência das atividades de exploração de petroleo e gás na Bacia de Campos

Emission factors of natural processes and anthropogenic activities were used to estimate nutrients and metal loads for the lower Macaé river basin, which hosts the operational base for the offshore oil and gas exploration in the Campos Basin. The estimates indicated that emissions from anthropogenic activities are higher than natural emissions. Major contributing drivers include husbandry and urbanization, whose effluents receive no treatment. The increasing offshore oil exploration along the Brazilian littoral has resulted in rapid urbanization and, therefore might increase the inshore emission of anthropogenic chemicals in cases where effective residue control measures are not implemented in fluvial basins of the region.

Composição elementar do aerossol atmosférico na região central da Bacia Amazônica

The processes and sources that regulate the elemental composition of aerosol particles were investigated in both fine and coarse modes during the dry and wet seasons. One hundred and nine samples were collected from the biological reserve Cuieiras - Manaus from February to October 2008, and analyzed together with 668 samples that were previously collected at Balbina from 1998 to 2002. Particle induced X-ray emission technique was used to determine the elemental composition, while the concentration of black carbon was obtained from the measurement of optical reflectance. Absolute principal factor analysis and positive matrix factorization were performed for source apportionment, which was complemented with back trajectory analysis. A regional identity for the natural biogenic aerosol was found for the Central Amazon Basin and can be used in dynamical chemical region models.