Determinação de As, Bi, Sb, Se, Sn e Te por injeção em fluxo com geração de hidretos acoplada a espectrometria de massa com plasma indutivamente acoplado

Abstract

In this work it is proposed the development of flow injection systems for hydride generation coupled to inductively coupled plasma mass spectrometry (FI-HG-ICPMS) for determination of trace elements (As, Bi, Sb, Se, Sn and Te) in lead alloys employed in automotive battery. Due to the characteristics of the sample matrix, manly the presence of high concentrations of lead that can interfere in hydride generation technique, a detailed investigation of the influence of the physical and chemical parameters was made. The carrier solution concentration (HCl) reductant concentration (NaBH4 solution), reaction coil length and sample volume were evaluated. As the ICP-MS is a multielmentar technique, the parameters were optimized in order to determine simultaneously the highest number of elements. Three different configurations of FI systems were tested: a) a single channel system; b) a two channel system with one gas/liquid separator; and, c) a two channel system with two gas/liquid separators. According to the characteristics of the elements, two groups were separated: one group containing As, Bi, Se and Te were 6.0 mol l-1 HCl is necessary as sample carrier solution and another group containing Sb and Sn were 0.1 mol l-1 HCl is used as sample carrier. The compromise conditions of NaBH4 concentration, carrier gas (Ar) flow rate, sample volume and reactor coil length were 0.6% (m/v), 1.25 L min-1, 87 μL and 50 cm, respectively, for both groups of elements. Both systems with two reaction channels allow the simultaneous determination of the two groups of elements. Strong analyte signal suppression in presence of Pb, Ag, Bi and Cu was observed. However, the interference could be overcome by using the optimized conditions for hydride generation. By using the proposed FI-HG-ICP-MS systems it was possible to determine relatively low concentrations of Bi, Sb, Se, Sn and Te in lead alloys. The limits of detection were 0.34, 0.01, 0.01, 0.01, 0.01, 0.01 mg g-1 of As, Bi, Sb, Se, Sn and Te, respectively. The accuracy of the developed method was evaluated by using analyte recovery tests where the results were in range 94 to 103%.