Organometals and organometalloids have been found in environmental samples as a result of their extensive usage and biotic and abiotic methylation processes. Alkyllead and organotin compounds are the most widely used organometals. In connection with studies of organometallic speciation, highly sensitive, and specific analytical techniques have been developed using combination analytical systems. At present, combination systems consisting of a separation technique coupled with an element-specific, atomic spectrometric detector are most satisfactory. A variety of atomic spectrometric detectors have been used in combination with gas chromatography and liquid chromatography.