Multi-commutated flow system for inorganic selenium speciation in infusion tea samples by chemical vapor generation atomic fluorescence spectrometry.

This work proposes an automated strategy for the inorganic selenium speciation in infusion tea samples, employing an MSFIA-CVG-AFS system and sodium tetrahydroborate for chemical vapor generation. The selenium total is determined after an online prereduction step of selenium (VI) to selenium (IV) in alkaline media, using a UV reactor with a 15 W Hg lamp. Selenium (IV) is quantified directly on the sample, and selenium (VI) is determined by the difference between the total selenium and selenium (IV) concentrations. The optimization of the chemical parameters: hydrochloric acid - hydrobromide acid solution concentration, potassium iodide concentration, sodium hydroxide concentration, and sodium tetrahydroborate concentration was performed using a (24-1) two-level fractional factorial design. The validation parameters were determined for total selenium and selenium (IV), and the results found were: limits of detection and quantification of 0.05 and 0.18 µg L-1, respectively; a linear range of 0.18-5.0 µg L-1, precision expressed as the relative standard deviation of 2.1% for a sample number of 10, for both analytes. The system allows the speciation analysis with an injection throughput of 15 injections per hour. This analytical method was applied for inorganic selenium speciation in nine infusions of tea samples purchased commercially in supermarkets in Palma de Mallorca City, Spain. The concentrations of selenium (IV) and total selenium varied from 0.2 to 0.6 µg L-1 and 0.4-2.0 µg L-1, respectively. The accuracy method was evaluated using spike tests, and the recoveries achieved varied from 91 to 111%.

Sources and distribution of polycyclic aromatic hydrocarbons (PAHs) and organic matter in surface sediments of an estuary under petroleum activity influence, Todos os Santos Bay, Brazil.

The present study evaluated the origin and distribution of polycyclic aromatic hydrocarbons (PAHs) and the organic matter (OM) in the surface sediment of the São Paulo River estuary, Todos os Santos Bay (TSB), Brazil. The samples were collected in the rainy (CP1) and the dry (CP2) seasons. We analyzed the 16 PAHs from the United States Environmental Protection Agency (US EPA) priority pollutant list, total organic carbon (TOC), total nitrogen (N), and stable carbon isotope (δ13C). The total concentration of PAHs ranged from 11.45±1.28 to 1825.35±107.96ngg-1, while TOC ranged from 3.8 to 27.7gkg-1. CP1 showed the highest concentrations for all parameters. The δ13C ratio indicated terrigenous OM (-23.81 to -26.63‰). The TOC/N ratio (C/N) indicated transitional OM (12.32 to 24.39), in addition to the continental origin. The diagnostic ratios of PAHs origin revealed only pyrolytic source, although close to areas with a history of petroleum contamination.

Multivariate optimization of ultrasound-assisted extraction for determination of Cu, Fe, Ni and Zn in vegetable oils by high-resolution continuum source atomic absorption spectrometry.

An assisted liquid-liquid extraction of copper, iron, nickel and zinc from vegetable oil samples with subsequent determination by high-resolution continuum source flame atomic absorption spectrometry (HR-CS FAAS) was optimized by applying a full factorial design in two levels and the response surface methodology, Box-Behnken. The effects of the acid concentration and the amplitude, cycle and time of sonication on the extraction of the analytes, as well as their interactions, were assessed. In the selected condition (sonication amplitude = 66%, sonication time = 79 s, sonication cycle = 74%), using 0.5 mol L(-1) HCl as the extractant, the limits of quantification were 0.14, 0.20, 0.21 and 0.04 µg g(-1) for Cu, Fe, Ni and Zn, respectively, with R.S.D. ranging from 1.4% to 3.6%. The proposed method was applied for the determination of the analytes in soybean, canola and sunflower oils.

Phytoremediation in mangrove sediments impacted by persistent total petroleum hydrocarbons (TPH's) using Avicennia schaueriana.

This study evaluated the efficiency of Avicennia schaueriana in the implementation of phytoremediation compared with intrinsic bioremediation in mangrove sediments contaminated by total petroleum hydrocarbons (TPHs). The experiment was conducted for 3months at a pilot scale under conditions similar to a mangrove: the dynamics of the tides were simulated, and physical, chemical, microbiological and biogeochemical parameters were monitored. After the 90 days, it was found that the phytoremediation was more efficient in the degradation of the TPHs compared to bioremediation, reducing the initial concentration of 32.2-4.2 mg/g. A. schaueriana was also more efficient in mediating the degradation of different fractions of hydrocarbons, achieving a removal efficiency of 87%. The microbiological results consisted of a higher growth in the model with the plants, demonstrating the phytostimulation ability of the plants. Finally, the experiment showed that phytoremediation is a promising alternative in mangrove impacted by oil.

Determination and evaluation of the mineral composition of Obi (Cola acuminate).

The obi (Cola acuminate) is a native fruit from Africa, which has been mainly used in the production of soft drinks and also in rituals of African religions. In this paper, the mineral composition of obi collected in seven different cities from Bahia State, Brazil was determined and evaluated using multivariate analysis. The samples were digested using nitric acid and hydrogen peroxide and were analyzed using inductively coupled plasma optical emission spectrometry. The accuracy of the method was confirmed by analysis of a certified reference material of apple leaves, furnished by National Institute of Standard and Technology. The study involved 46 samples, being 18 of the red specie and 28 for the white specie. The results expressed as milligrams of element per 100 g(-1) of sample demonstrated that the concentration ranges varied of 21.28-548.77 for potassium, 15.73-129.85 for phosphorous, 27.95-286.92 for calcium, 7.67-134.45 for magnesium, 0.05-1.41 for manganese, 0.21-0.94 for iron, 0.11-0.39 for copper, 0.27-1.35 for zinc, and 0.025-0.517 for strontium. The principal component analysis and hierarchical cluster analysis evidenced that the mineral composition of the red specie is different of the white specie. The red obi has mineral content higher than white obi.

Determination of phosphorus, sulfur and the halogens using high-temperature molecular absorption spectrometry in flames and furnaces--A review.

The literature about the investigation of molecular spectra of phosphorus, sulfur and the halogens in flames and furnaces, and the use of these spectra for the determination of these non-metals has been reviewed. Most of the investigations were carried out using conventional atomic absorption spectrometers, and there were in essence two different approaches. In the first one, dual-channel spectrometers with a hydrogen or deuterium lamp were used, applying the two-line method for background correction; in the second one, a line source was used that emitted an atomic line, which overlapped with the molecular spectrum. The first approach had the advantage that any spectral interval could be accessed, but it was susceptible to spectral interference; the second one had the advantage that the conventional background correction systems could be used to minimize spectral interferences, but had the problem that an atomic line had to be found, which was overlapping sufficiently well with the maximum of the molecular absorption spectrum. More recently a variety of molecular absorption spectra were investigated using a low-resolution polychromator with a CCD array detector, but no attempt was made to use this approach for quantitative determination of non-metals. The recent introduction and commercial availability of high-resolution continuum source atomic absorption spectrometers is offering completely new possibilities for molecular absorption spectrometry and its use for the determination of non-metals. The use of a high-intensity continuum source together with a high-resolution spectrometer and a CCD array detector makes possible selecting the optimum wavelength for the determination and to exclude most spectral interferences.

On-line system for preconcentration and determination of metals in vegetables by inductively coupled plasma optical emission spectrometry.

A procedure has been developed for the simultaneous determination of trace amounts of cadmium, copper, chromium, nickel and lead in digested vegetable samples. The method involves solid-phase extraction of the metals using a minicolumn of Amberlite XAD-4 modified with dihydroxybenzoic acid (DHB) and detection by Inductively Coupled Plasma Optical Emission Spectrometry (ICP-OES). The elution of the metals from minicolumn was performed with 1.0 molL(-1) hydrochloric acid. Variables associated with flow preconcentration system performance, such as pH, buffer concentration, eluent concentration and sampling flow rate, were optimized. The developed procedure provides enrichment factors of 100, 72, 16, 91 and 53, for cadmium, copper, chromium, nickel and lead, respectively. Detection limits (3sigma(B)) were 0.02 (Cd), 0.23 (Cu), 0.58 (Cr), 0.060 (Ni) and 0.54 (Pb)microgL(-1). The procedure was applied for determination of metals in samples of guarana and cabbage. The accuracy of the method was checked by the analysis of a certified reference material (NIST 1571, Orchard leaves). Results found were in agreement with certified values.