Determination of mercury in gasoline by cold vapor atomic absorption spectrometry with direct reduction in microemulsion media

The determination of Hg in gasoline by cold vapor atomic absorption spectrometry, after direct aqueous NaBH4 reduction in a three-component (microemulsion) medium, was investigated. Microemulsions were prepared by mixing gasoline with propan-1-ol and 50% v/v HNO3 at a 20:15:1 volume ratio. A long-term homogeneous system was immediately formed this way. After reduction, the Hg vapor generated in a reaction flask was transported to an intermediate K2Cr2O7/H2SO4 trap solution in order to avoid poisoning of the Au-Pt trap by the gasoline vapors. A second reduction step was then conducted and the generated Hg vapor transported to the Au-Pt trap, followed by thermal release of Hg-0 and atomic absorption measurement. Purified N-2 was used as purge and transport gas. After multivariate optimization by central composite design calibration graphs showed coefficients of correlation of 0.9999 and a characteristic mass of 2 ng was obtained. Typical coefficients of variation of 5% and 6% were found for ten consecutive measurements at concentration levels of 1 and 8 mu g L-1 of Hg2+, respectively. The limit of detection was 0.10 mu g L-1 (0.14 mu g kg(-1)) in the original sample. A total measurement cycle took 11 min, permitting duplicate analysis of 3 samples per hour. The results obtained with the proposed procedure in the analysis of commercial gasoline samples were in agreement with those obtained by a comparative procedure. Gasoline samples of the Rio de Janeiro city have shown Hg concentrations below 0.27 mu g L-1. (c) 2005 Elsevier B.V All rights reserved.