Total mercury in a variety of substances is determined rapidly and precisely by direct sample combustion, collection of released mercury by amalgamation, and photometric measurement of mercury volatilized from the heated amalgam. Up to 0.2 g fish tissue is heated in a stream of O2 (1.2 L/min) for 3.5 min in 1 tube of a 2-tube induction furnace. The released mercury vapor and combustion products are carried by the stream of O2 through a series of traps (6% NaOH scrubber, water condenser, and Mg(CIO4)2 drying tube) and the mercury is collected in a 10 mm diameter column of 24 gauge gold wire (8 g) cut into 3 mm lengths. The resulting amalgam is heated in the second tube of the induction furnace and the volatilized mercury is measured with a mercury vapor meter equipped with a recorder-integrator. Total analysis time is approximately 8 min/sample. The detection limit is less than 0.002 μg and the system is easily converted for use with other biological materials, water, and sediments.