Almost every phase of environmental protection depends on the ability to detect and analyze specific chemical pollutants. Gas chromatography/mass spectrometry (GC/MS) has been shown to be widely applicable for separation and analysis of volatile organics, whereas liquid chromatography has been found to be useful in separating, but not analyzing, non-volatile organics. This study investigated two approaches to developing an LC/MS system that would provide the same ease and reliability for non-volatile analysis that GC/MS does for volatile analysis. In one, the chromatographic system was a high pressure liquid chromatograph (HPLC) with ultrasonic nebulization and the other, a dense (supercritical) gas chromatograph. Neither an ultrasonic vaporization LC/MS nor a dense gas chromatograph/mass spectrometer system provided the required capabilities.