The present work describes the use of 1-(2-thiazolylazo)-2-naphthol (TAN) as a spectrophotomeric reagent for iron determination. TAN reacts with iron(II) forming a brown complex with absorption maximum at 575 and 787 nm. The following parameters were studied: complex stability, pH effect, amount of the TAN, buffer selection, amount of acetate buffer, reductor effect, order of addition of reagents and adherence to Beer's Law. The results demonstrated that iron can be determined with TAN in a pH range of 4.0-6.2 with an apparent molar absorptivity of 1.83 x 10(4) 1 . mol(-1) . cm(-1) (at 787 nm) and 1.41 x 10(4) 1 . mol(-1) . cm(-1) (at 575 nm). Beer's Law is obeyed for at least 3.00 microg/ml. The TAN reacts with other cations, but at 787 nm only the iron(II)-TAN complex absorbs. So, iron can be determined selectively in the presence of several cations. A procedure based on the direct mixture of the sample and a chromogenic solution is proposed, where iron can be determined rapidly and easily. Such procedures were used for the determination of iron in several geological matrices. No significant differences were obtained for TAN method and certificate results.
Contamination by oil spills in coastal ecosystems, especially in mangrove zones, has been common in countries with oil industry. The aim of this study was, therefore, to evaluate the efficiency of application of the two models developed for pilot-scale remediation, intrinsic bioremediation (indigenous microorganisms), and phytoremediation (Avicennia schaueriana). The degradation of hydrocarbons was determined by gas chromatography (GS) with flame ionization detector. The metals Al, Fe, Pb, Cr, Cu, Zn, and Ni were determined by flame atomic absorption spectrometry in the mangrove simulated with sediment of Todos os Santos Bay, Brazil. These models also monitor other biogeochemical parameters (nitrogen, phosphorus, total organic carbon, pH, redox potentioal, dissolved oxygen, salinity, temperature, bacterial density). The integrated assessment of data showed that both techniques were effective in degrading organic compounds from oil but that phytoremediation is the most efficient (89% removal). The intrinsic bioremediation model has no direct correlation with metal concentrations, but a positive correlation with Al and Ni was found in the hydrocarbon removal by phytoremediation. Avicennia schaueriana represents efficiency in phytoextraction and phytostimulation. The results suggest that the phytoremediation model, through its various mechanisms, may become a technique for the removal of petroleum hydrocarbons in the presence of metals in mangrove ecosystems near industrial areas.
The quantitative determination of chemical elements in organic or biological samples is an important analytical problem. Normally the elements to be determined in the organic matrix must be transformed into a simple inorganic form. A digestion method by heating on a block digestor has been developed for the determination of Al, As, Ba, Ca, Cd, Co, Cu, Fe, Mg, Mn, V and Zn in Oyster tissue by ICP OES. A simplex centroid statistical mixture design has been used to study the effects of changing HNO(3), HCl and H(2)O(2) reagent proportions on the digestion of these samples. Response surface and principal component analyses show that the species Ca, Cd, Cu, Fe, Mg, Mn and Zn have very similar analytical tendencies under this experiment. By means of mixture modeling maximum recoveries for these ions were predicted using 19%, 18% and 63% of the HCl, HNO(3) and H(2)O(2) pseudocomponent mixtures, respectively. This corresponds to 21.4%, 30.8% and 47.8% of the HCl, HNO(3) and H(2)O(2) commercial solutions. Furthermore the As, Co and V ions present large recoveries for these mixtures as well. The Al and Ba ion recoveries are seen to be independent of the mixture proportions. The analysis of Oyster tissue reference material (SRM 1566b - NIST) under optimized conditions at the selected wavelengths resulted in ion recoveries between 90% and 100%.
The development of nutritious, low-cost snacks has become increasingly important due to consumer demand for healthier diets. In this study, sensory and physical-chemical parameters and mineral compositions (P, Ca, Na, K, Mg, Fe, Zn, Al, Cu, Mn, Ni and Ba) of cereal bars were evaluated. The bars were made with flours of Lablab purpureus L. Sweet (mangalo), Vigna unguiculata L. Walp (cowpea) or Cajanus cajan L. Huth (pigeon pea) and the desirability function was used to attain the best formulation for maximising the content of protein, fibre, ashes and essential elements. Sensory analysis revealed satisfactory acceptability. Acidity did not change significantly (p > 0.05), and water activity values did not exceed 0.557 over 90 days, indicating stability. Principal component analysis revealed no significant differences when comparing the mineral content between the bars. The desirability function indicated that the cowpea-based bar had a higher nutritional quality, with a protein content of 4.91 ± 0.25 g 100 g−1, P content of 187.7 ± 3.6 mg 100 g−1, Mg content of 87.37 ± 1.19 mg 100 g−1 and Mn content of 2020 ± 130 µg 100 g−1, than the other bars. The overall sensory evaluation also yielded a high score for the cowpea-based bar (overall quality equal to 6.23 ± 1.10). Therefore, pulse flours could be potential nutritional ingredients for making snacks, and in particular, cereal bars containing them could be a viable product alternative for small rural cooperatives.
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