RESUMO
An on-line scandium preconcentration and determination system implemented with inductively coupled plasma optical emission spectrometry associated with flow injection was studied. Trace amounts of scandium were preconcentrated by sorption on a minicolumn packed with oxidized multiwalled carbon nanotubes, at pH 1.5. The retained analyte was removed from the minicolumn with 30% (v/v) nitric acid. A total enrichment factor of 225-fold was obtained within a preconcentration time of 300 s (for a 25 mL sample volume). The overall time required for preconcentration and elution of 25 mL of sample was about 6 min; the throughput was about 10 samples per hour. The value of the detection limit was 4 ng L(-1) and the precision for 10 replicate determinations at 100 ng L(-1) Sc level was 5% relative standard deviation, calculated from the peak heights obtained. The calibration graph using the preconcentration system was linear with a correlation coefficient of 0.9996 at levels near the detection limits up to at least 10 mg L(-1). After optimization, the method was successfully applied to the determination of Sc in an acid drainage from an abandoned mine located in the province of San Luis, Argentina.
Assuntos
Análise de Injeção de Fluxo/métodos , Mineração , Nanotubos de Carbono/química , Escândio/análise , Espectrofotometria Atômica/métodos , Ácidos/química , Argentina , Concentração de Íons de Hidrogênio , Oxirredução , Reprodutibilidade dos Testes , Escândio/química , Águas Residuárias/química , Poluentes Químicos da Água/análiseRESUMO
The consistency of the published values for fission averaged cross-sections of threshold reactions induced in a nuclear reactor is analyzed. The influence of the literature data involved in the determination of these cross-sections is discussed. Renormalizations based on cross-sections value for the standard reactions, isotopic abundances of the precursors and radiation emission probabilities of the radionuclide under study and the monitor, are applied to the evaluation of the cross-sections for the reactions: (46)Ti(n,p)(46)Sc; (47)Ti(n,p)(47)Sc; (48)Ti(n,p)(48)Sc; and (64)Zn(n,p)(64)Cu.
Assuntos
Radioisótopos de Cobre/química , Nêutrons , Fissão Nuclear , Radiometria/métodos , Escândio/química , Titânio/química , Radioisótopos de Zinco/química , Radioisótopos de Cobre/efeitos da radiação , Isótopos/química , Isótopos/efeitos da radiação , Doses de Radiação , Escândio/efeitos da radiação , Titânio/efeitos da radiação , Radioisótopos de Zinco/efeitos da radiaçãoRESUMO
We describe the preparation, the crystal structure refined from neutron powder diffraction (NPD) data, and study of the permittivity of two related double perovskites, Pb2Sc(Ti0.5Te0.5)O6 and Pb2Sc(Sc0.33Te0.66)O6. These compounds were synthesized by standard ceramic procedures; Rietveld refinements from room temperature NPD data show that the crystal structures are well defined in a cubic unit cell (space group Fm3m) with double parameter, a = 2a0 ≈ 8 Å. They contain a completely ordered array of ScO6 and (B,Te)O6 (B = Sc, Ti) octahedra sharing corners; the PbO12 polyhedra present an off-center displacement of the lead atoms along the [1 1 1] directions, due to the electrostatic repulsion between the Pb(2+) 6 s electron lone-pair and the Pb-O bonds of the cuboctahedron. Both compounds present a low temperature, highly dispersive maximum in permittivity, the position of which follows the Vogel-Fulcher relation with freezing temperatures of 156 and 99 K for Pb2Sc(Ti0.5Te0.5)O6 and Pb2Sc(Sc0.33Te0.66)O6, respectively, exhibiting a typical phenomenology of relaxors.