In this study, a new method was developed based on aqueous phenylation, purge-and-trap preconcentration, gas chromatography (GC) separation, and detection by atomic fluorescence spectrometry (AFS) or inductively coupled plasma mass spectrometry (ICPMS). Using the developed method, both monomethylmercury and monoethylmercury were detected in a number of soil and sediment samples collected from the Florida Everglades. The identity of monoethylmercury was verified by purge-and-trap-GC/MS analysis. The possibility of analytical artifact was excluded by using stable isotope tracer technique in...