Efeito do teor metálico em catalisadores Co/Al2O3 aplicados à reação de reforma a vapor de etanol

The development of cobalt catalysts to produce hydrogen from ethanol is the goal of this investigation. Co/Al2O3 catalysts were prepared by impregnation and characterized by atomic absorption, nitrogen adsorption, X-ray diffraction, Raman spectroscopy, temperature programmed reduction and carbon analysis. The catalysts contained Co3O4 oxide and Co3+ and Co2+ species interacting with alumina. The cobalt load affects the crystal size and the crystalline structure and higher Co loads influence the reaction mechanism, changing the selectivity of the catalysts, decreasing the amount of CO produced and avoiding the formation of products catalyzed by the support. The ethanol conversion was 50-70% with 10-<1% of CO in the hydrogen.

Avaliação do teor de metais em sedimento do rio Betari no Parque Estadual Turístico do Alto Ribeira: PETAR, São Paulo, Brasil

The subsoil of the Vale do Ribeira was the focus of mining industries for the exploration of lead, mainly inside the park - PETAR. Despite the fact that the exploration has ended, the environmental effects of those activities are still present, due to great amounts of heavy metals that are leached. Concentrations of pseudo-total and bioavailable metals were determined in sediment samples of the Betari River, using atomic absorption spectrometry. The results demonstrated that the sediments are contaminated by Pb, Zn and Cu. The findings can contribute to an efficient and environmentally and economically adequate management of the park, for the conservation and the protection of the area.

Determinação direta de molibdênio em comprimidos polivitamínicos por voltametria em meio não aquoso

Adsorptive stripping voltammetry carried out in a homogeneous ternary solvent composed of N,N-dimethylformamide, water and ethanol, with alpha-benzoinoxime (alphaBO) as the complexing agent for Mo(VI) and a 0.5 mol L-1 acetic acid - sodium acetate buffer as supporting electrolyte was successfully used for the determination of molybdenum in polyvitamin-polymineral tablets. Tablet samples were analyzed and the results were compared with those obtained both by graphite furnace atomic absorption and by recovery tests, with good correlations, indicating that this may be considered as an alternative procedure for routine determination of Mo(VI) in pharmaceutical samples.

Solid phase extraction of iron and lead in environmental matrices on amberlite xad-1180/pv

A solid phase extraction procedure using Amberlite XAD-1180/Pyrocatechol violet (PV) chelating resin for the determination of iron and lead ions in various environmental samples was established. The procedure is based on the sorption of lead(II) and iron(III) ions onto the resin at pH 9, followed by elution with 1 mol/L HNO3 and determination by flame atomic absorption spectrometry. The influence of alkaline, earth alkaline and some transition metals, as interferents, are discussed. The recoveries for the spiked analytes were greater than 95%. The detection limits for lead and iron by FAAS were 0.37 µg/L and 0.20 µg/L, respectively. Validation of the method described here was performed by using three certified reference materials (SRM 1515 Apple Leaves, SRM 2711 Montana Soil and NRCC-SLRS-4 Riverine Water). The procedure was successfully applied to natural waters and human hair.

Preparação de amostra de fígado bovino e estudo de micro homogeneidade para a determinação de Cd E Pb por espectrometria de absorção atômica com atomização eletrotérmica e amostragem direta de sólido

This work describes a systematic study for bovine liver sample preparation for Cd and Pb determination by solid sampling electrothermal atomic absorption spectrometry. Samples were prepared using different procedures: (1) drying in a household microwave oven followed by drying in a stove at 60 ºC until constant mass, and (2) freeze-drying. Ball and cryogenic mills were used for grinding. Particle size, sample size and micro sample homogeneity were investigated. All prepared samples showed good homogeneity (He < 10) even for low sample mass, but samples dried in a microwave oven/stove and ground in a ball mill presented the best homogeneity.

Estudo multivariado de solos urbanos da cidade de Teresina

The concentrations of Cu, Pb, Zn, Cr, Ni, Al, Mn and Fe were measured by atomic absorption spectrometry, of 19 topsoil samples collected in the Teresina city urban area to discriminate natural and anthropic contributions and identify possible sources of pollution. The average concentrations of Cu, Zn, Pb and Cr of the urban soils were 6.11, 8.56, 32.12 and 7,17 mg/kg-1, respectively. Statistical analysis techniques, such as principal component analysis (PCA) and hierarchical cluster analysis (HCA), were used to analyze the data. Mn, Ni and Cr levels were interpreted as natural contributions, whereas Pb, Zn and, in part, Cu were accounted for mainly by anthropic activities. High Pb levels were observed in the ancient avenues.

Incorporação de CuSO4 residual em argamassa, como método de disposição final

Residual CuSO4 was incorporated into the mass utilized for cement preparation. To a cement mass with 1:0.5:5 of cement, lime and sand to 0.25, 0.50, 0.75 and 1.00% of residual CuSO4 were added. The sulfate was mixed separately with lime and water to induce metal precipitation. The hardened test bodies were submerged in Milli-Q water for three months. No Cu was detected in the water by Atomic Absorption Spectrometry. The best proportion for mechanical resistance and porosity is 0.50%. The cement is adequate for non-structural objects.

Integração de técnicas analíticas e proposta de experimentos para cursos de graduação em análise instrumental: uso de espectrômetro de absorção atômica para medidas de absorção molecular

Simple experiments are proposed for measuring molecular absorption of chromate and dichromate ions using an atomic absorption spectrometer. The experiments can help undergraduate students in instrumental analysis courses understand important aspects involving conceptual and instrumental similarities and differences between frequently used analytical techniques. Hollow cathode lamps were selected with wavelengths in the region of molecular absorption of chromate and dichromate. Calibration curves were obtained and the linear dynamic range was evaluated. Results were compared with those obtained in a molecular absorption spectrometer. The molar absorptivities obtained were also compared.

Determinação de contaminantes em óleos lubrificantes usados e em esgotos contaminados por esses lubrificantes

A simple and reliable ashing procedure is proposed for the preparation of used lubricating oil samples for the determination of Zn, Fe, Pb, Ni and Cu by the flame atomic absorption spectrometry technique. Sulphanilic acid was added to oil samples, the mixture coked and the coke ashed at 550 ºC. The solutions of the ash were analysed by flame AAS for these metals. The quantification limits were 38.250 µg g-1 for Zn, 4.550 µg g-1 for Fe, 1.562 µg g-1 for Pb, 1.450 µg g-1 for Ni, and 0.439 µg g-1 for Cu. The determinations, in lubricating oil, showed good precision and accuracy with recoveries between 90 and 110 %, indicating a negligible matrix effect in the experiments using addition of analyte, with relative standard deviation lower than 5%. The results for analysis of wastewater contamined by theses lubricants showed a very high relative standard deviation.

Avaliação da concentração de alguns íons metálicos em diferentes espécies de líquens do cerrado Sul-Mato-Grossense

Concentrations of Fe, Mn, Co, Cr, Zn and Cu were determinated using flame atomic absorption spectrometry in nine lichen species of the Sul-Mato-Grossense cerrado. The average metal ion concentrations varied in the following ranges: Fe, 248.41-1568.01; Mn, 98.50-397.33; Co, 10.08-24.81; Cr, 18.24-44.26; Zn, 14.62-34.79 and Cu, 3.23-7.57 mg kg-1. Statistical analysis (Pearson and Cluster) applied to the metal ion concentrations indicated that the accumulation of these ions can be due to several anthropogenic sources including agricultural activities, mineral exploration, biomass burning, soil mineral composition and leather tanning processes by chromium.

Determinação de zinco em solo utilizando colorimetria

In terms of soil fertility, zinc is a micronutrient that is very important in the culture of soy, maize, rice and coffee, because it is a structural and functional component of a great number of enzymes. Therefore, diverse methods have been used to determine zinc in soil. In this work we use colorimetry as a methods of zinc determination in soil using two methodologies of sample digesting, H2SO4/H2O2 and HNO3/H2O2. In order to compare the results, atomic absorption spectrometry (AAS) was used. Results show that colorimetric methods can be used due to good sensitivity and reproducibility, since the zinc calibration curve showed good linearity. Comparing colorimetric methods with AAS we observed that the results were equivalent, as proven by the statistical values of the F and t of Student tests. Furthermore, both methods of soil digesting can be used, leading to a flexible methodology of low-cost for routine zinc analyses in soil.

Mineral and vitamin content of beef, chicken, and turkey hydrolysates mineral and vitamin content of protein hydrolysates

The purpose of this study was to assess the concentration of vitamins and minerals in meat protein hydrolysates. Calcium, phosphorus and iron were analyzed by inductively coupled-plasma atomic emission spectrophotometry; vitamin C was analyzed by the reduction of cupric ions and vitamins B1 and B2 by fluorescence. Regarding minerals, the beef hydrolysate (BH) had more iron than the turkey hydrolysate (TH) and the chicken hydrolysate (CH); TH had a little more phosphorus. BH had the largest amount of vitamin C, and similar amounts of vitamins B1 and B2. The amount of these nutrients found in the hydrolysates suggests that it is possible to use them to enrich special dietary formulations.

Análise direta de sólidos por espectrometria de absorção atômica com atomização em forno de grafite: uma revisão

This is a review of direct analysis using solid sampling graphite furnace atomic absorption spectrometry. Greater emphasis is dedicated to sample preparation, sample homogeneity, calibration and its application to microanalysis and micro-homogeneity studies. The main advantages and some difficulties related to the applicability of this technique are discussed. A literature search on the application of solid sampling graphite furnace atomic absorption spectrometry in trace element determination in many kinds of samples, including biological, clinical, technological and environmental ones, is also presented.

Electrochemical behavior of parent and photodegradation products of some selected pesticides

Electrochemical behavior of pesticides is extensively studied, but little attention has been given to the study of their degradation products (by-products) by electrochemical methods. However, the degradation products of pesticides can be even more toxic then the parent products and such studies should be encouraged. Therefore, the objective of this work was to evaluate the electroactivity of by-products of imazaquin, methylparathion, bentazon and atrazine, generated by UV irradiation and measured using cyclic and differential pulse voltammetry and UV-visible absorption spectrophotometry. Results have shown that several by-products exhibit electroactivity, allowing, in some cases, the simultaneous determination of both parent and degradation products.

Especiação redox de cromo em solo acidentalmente contaminado com solução sulfocrômica

Determination of Cr(VI) and Cr(III) was studied in soil samples accidentally contaminated with sulphochromic solution. Molecular absorption spectrophotometry based on the diphenylcarbazide method was used for the determination of Cr(VI) after its alkaline extraction. The total chromium concentration was determined using ICP OES. The quantification of Cr(III) was accomplished by subtracting the Cr(VI) concentration from the total chromium concentration. Regardless of the known contamination of the soil samples by sulphochromic solution, concentrations of Cr(VI) were below the detection limit. Addition and recovery experiments for Cr(VI) in soil samples with and without organic matter indicated its influence on the reduction of Cr(VI) to Cr(III).