Larvae of Ambystoma maculatum (Amblystoma punctatum) and Triturus (Notophthalmus) viridescens at stage 42 were used to study gill resorption and the role of acid phosphatase in this phenomenon. Concentrations of 8 × 10 −2 μg/ml, 8 × 10 −3 μg/ml, 4 × 10 −3 μg/ml and 8 × 10 −4 μg/ml of 3,5,3-triiodothyronine were administered in the water surrounding the animals. It was found that beginning on day 3 of treatment the animals in the highest concentration group began to respond and that by day 7 gill resorption was complete. The animals in the 8 × 10 −3 μg/ml concentration group began resorption on day 7 and completed resorption by day 30. Animals receiving 4 × 10 −3 μg/ml were seen to proceed only to resorption of filaments by the end of the 30-day period. Those in the lowest concentration showed a response identical to the controls which received no T 3 treatment. A second group of animals was treated with 8 × 10 −2 μg/ml of T 3 and were killed at daily intervals, the gills were removed, homogenized, clarified, and subjected to polyacrylamide gel electrophoresis at 4°C. The gels were stained for acid phosphatase activity, and the reacted gels were quantified. Animals at day 7 showed a 13-fold increase in acid phosphatase activity.