A method is described for the quantitative determination of residual methylene chloride (MC) and trichloroethylene (TCE) in decaffeinated instant and ground roasted coffees. The residual solvents were isolated by a closed system vacuum distillation technique with toluene as a carrier solvent, chromatographed on Chromosorb 102, detected by both electron capture and electrolytic conductivity detectors, and quantitated by comparison with an internal standard. Average recoveries of MC from instant and ground coffees spiked at 1, 10, and 25 ppm were 100.0 (88-113), 93.2 (92-95), and 97.7% (94-102%); and for TCE, 97.2 (92-101), 96.2 (95-99), and 96.5% (92-100%), respectively. The results from both detectors are compared. At lower attenuations, levels less than 1 ppm can be readily measured. The procedure developed was applied to domestic and imported coffee samples.