Masking agents in the determination of selenium by hydride generation technique

The effects of several masking agents in the determination of selenium by hydride generation was studied using a continuous flow hydride generator coupled with atomic absorption spectrometry. A miniature argon hydrogen diffusion flame was employed as the atomizer. The effects of masking agents (KI, NaSCN, thiourea, L-cysteine, 1,1,3,3 tetramethyl-2-thiourea) were studied both in the absence and in the presence of selected interfering species (Cu, Ag, Au, Ni, Co, Pd, Pt and Fe) and using different addition strategies of the masking agents to the reaction system: in batch mode, either to sample or NaBH4 reducing solution; in on-line mode, to the sample either before or after the HG step). The combined effect of some masking agents was also investigated. The addition mode of the masking agent to the reaction system could play a decisive role in the control of interfering processes both in the absence and in the presence of concomitants. The addition of NaSCN to the reducing solution of NaBH4 produced a moderate catalytic effect, similar to the one obtained in the presence of KI, and improved the tolerance limits for Cu, Ni, Co and Pd. Linearity of calibration graphs was unaffected by the on-line addition of 1,1,3,3 tetramethyl-2-thiourea to sample solution, while under similar conditions thiourea produced dramatic curvature of calibration graphs. The combined use of KI (added to reducing solution) and 1,1,3,3 tetramethyl-2-thiourea (added on-line to the sample) exhibited masking properties comparable but not superior to those of thiourea, except for Pt and Pd for which good tolerance limits were achieved. In the absence of KI in the reductant solution the masking efficiency of 1,1,3,3 tetramethyl-2-thiourea was considerably lowered. The addition of some masking agents such as thiourea, L-cysteine and 1,1,3,3 tetramethyl thiourea on-line to reaction solution after the NaBH4+KI reduction step, could be highly effective in the control of Cu and Ag interferences. The method was applied to determination of trace of selenium in pure copper standard reference materials. (C) 2002 Elsevier Science B.V. All rights reserved.