RESUMO
Among the "traditional" hydride-forming elements, lead is probably the most difficult, and its determination in this form has rarely been reported in the literature. In this paper a simple and rapid method, axial-view inductively-coupled plasma optical-emission spectrometry using on-line hydride generation (HG-ICP-OES) from samples prepared as slurry, is proposed for determination of lead in environmental samples. The samples (20-50 mg, particle size
RESUMO
A method for the determination of Ag, Cd, Cu, Pb and Tl in fuel alcohol by isotope dilution electrothermal vaporization inductively coupled plasma mass spectrometry (ID ETV-ICP-MS) is proposed. The analytes were separated in two groups: Ag and Cu were determined without modifier and Cd, Pb and Tl with the use of Pd as chemical modifier. The employed ETV operational conditions were pyrolysis temperature of 800 degrees C for Cd, Pb and Tl and of 900 degrees C for Ag and Cu and vaporization temperature of 2400 degrees C for both groups. Seven common, one with additive and one anhydrous fuel ethanol samples were analyzed. The spiked and reference isotopes were, respectively, (109)Ag and (107)Ag, (112)Cd and (111)Cd, (63)Cu and (65)Cu, (206)Pb and (208)Pb and (203)Tl and (205)Tl. The added amounts of the enriched isotope material were the same for all samples: 4.6 ng of (109)Ag, 5 ng of (112)Cd, 21.1 ng of (63)Cu, 9 ng of (206)Pb and 0.21 ng of (203)Tl. The blank was bi-distilled ethanol, acidified with 0.3% (v/v) nitric acid, as the samples. The limits of detection (LODs) were calculated as three times the standard deviation of the concentrations in the blank (n=10) and were, in microg L(-1), for Ag: 0.02, for Cd: 0.08, for Cu: 0.1, for Pb: 0.05 and for Tl: 0.001. The obtained concentrations in the samples were in agreement with those obtained by external calibration (EC), according to the paired t-test. The isotope dilution (ID) showed to be a robust, fast and simple calibration technique for the analysis of fuel ethanol.
