Abstract The organophosphorus insecticide azinphos-methyl was applied once to the surface of 12 of 18 littoral enclosure mesocosms (5×10 m) constructed in a 2-ha pond near Duluth, Minnesota. Water, sediment, macrophytes, and adult fathead minnows were analyzed for residue to determine the persistence, distribution, and mass balance of azinphos-methyl. Nominal treatment concentrations were 0, 0.2, 1, 4, and 20 μg/liter active ingredient. The maximum residue concentration in the water was measured 1h after treatment. The half-life in the water column ranged from 1.2 to 2 days and 95% of the residue dissipated in 5.4 to 10.2 days. Measurable residues were found in the sediment, macrophytes, and fish. Maximum residues in these media were measured at 4, 1, and 0.12 days. respectively. The water and sediment were the most important sorptive compartments for azinphos-methyl residue. The macrophytes and fish were of minor importance, containing only trace amounts of the mass applied.