A method for the selective determination of Se4+ and Se6+ using solid phase
microextraction (SPME) and GC/MS analysis is presented. Se4+ is selectivel
y derivatized by reaction with 4,5-dichloro-1,2-phenylenediamine to form th
e corresponding piazselenolo complex, extracted by the SPME fiber, and dete
rmined by GC/MS. The RSD at a 5 mu g/L concentration was 9.88% and the theo
retical detection limit 6 ng/L. The method was employed to test real matric
es; tap and river water were analyzed before and after spiking giving a rec
overy rate of 102% in river mater and 97% in tap water.