Copper was determined in environmental matrices following generation, separation, and atomization of a volatile species formed by the merging of an acidified sample solution with an aqueous sodium tetrahydroborate solution at room temperature. The copper species, as yet unidentified, was phase separated in a conventional gas-liquid separator and directed via a stream of Ar carrier gas to an inductively coupled plasma atomic emission detection system. Optimum conditions for generation were investigated. The efficiency of generation/transfer was estimated to be 50%, and no interference from the presence of 1000 mg/L concentration of As, Cd, Co, Ni, Fe, Cr, Mn, Pb, Se, and Zn concomitants was evident. Simple aqueous standards were used for calibration purposes, and good agreement was obtained with certified values in the analysis of National Research Council of Canada marine sediment BCSS-1 and lobster hepatopancreas tissue TORT-1.