RESUMO
In the present study, a flow injection system using dual mini-columns, SiO(2)/Al(2)O(3)/TiO(2) and silica gel functionalized with [3-(2-aminoethylamino)propyl] trimethoxysilane (SiO(2)/AAPTMS) for the sequential preconcentration of Cr(III) and Cr(VI), respectively, from water samples with FAAS detection was proposed. A two-level full factorial design (2(4)) and desirability function were employed for the optimization of variables related to the system performance. The detection limits of 0.66 and 0.27 µg L(-1) for Cr(III) and Cr(IV), respectively, were obtained under the optimized preconcentration conditions (flow rate of 7.0 mL min(-1)), pH 5.0, buffer concentration (acetate buffer) of 0.01 mol L(-1), and eluent (2.5 mol L(-1) HCl) flow rate of 5.0 mL min(-1). The other parameters including preconcentration factor (PF), consumptive index (CI), and concentration efficiency (CE) were found to be 17.62/32.98, 1.13/0.6 mL, and 6.2/11.54 min(-1) for Cr(III)/Cr(VI), respectively. The developed method was applied to the Cr(III) and Cr(VI) determination in water samples [tap, lake and mineral water, artificial saliva and parenteral solutions (physiological serum, water for injection, and glucose physiological solution)]. The method accuracy was checked by the analysis of standard reference materials (trace elements in water).
Assuntos
Métodos Analíticos de Preparação de Amostras/métodos , Cromo/análise , Cromo/química , Dióxido de Silício/química , Espectrofotometria Atômica/métodos , Análise de Injeção de Fluxo , Concentração de Íons de Hidrogênio , Análise Multivariada , Fatores de TempoRESUMO
The interaction of Pt(II)(dppf)-complex, namely [Pt(dppf)(H(2)O)(2)](2+) with DNA was investigated by DPV and (1)H-NMR techniques. The results showed that the interaction process has been characterized by changes in the electrochemical parameters of both compounds and the formation of a new anodic current peak close to the anodic current peak of the [Pt(dppf)(H(2)O)(2)](2+). In addition, the (1)H-NMR spectra show that the coordination of Pt(II)(dppf)-complex to dsDNA occurs via N(7) of guanine. Others parameters like pH and ionic strength that affect the interaction process were also investigated.