On-line mercury and methylmercury pre-concentration by adsorption of their dithiophosphoric acid diacyl ester chelates on a C₁₈ column and cold-vapor atomic-absorption detection

Abstract.

The pre-concentration of mercury(II) and methylmercury by adsorption of their dithiophosphoric acid diacyl ester (DDTP) chelates on a C₁₈ column, then detection with cold-vapor atomic-absorption spectrometry was investigated. Conditions such as sample pH, reductant and chelating agent flow and concentration, and eluent and carrier gas flow were optimized. Optimization was performed by use of evolutionary operation with a proper factorial design. At a sample flow of 5.3 mL min^–1 and a loading time of 4.5 min, column adsorption efficiency ranged from 88 to 93% for both species. Detection limits down to 10 ng L^–1 were obtained at a sample throughput of 12 h^–1. There was good agreement between found and certified values in the analysis of certified reference materials after their microwave-assisted mineralization with HNO₃ and H₂O₂.