The skin/gills and the kidneys of aquatic amphibians are potential sites of acid-base regulation. The roles of these organs in acid-base balance were examined in larval Ambystoma tigrinum following gastric infusion of ammonium salts. A single dose of 1.75 mEq NH4Cl·100 g-1 produced a mixed acidosis by 1 h after gavage. By 8 h after ingestion, pH and HCO 3 − had increased and PCO2 had decreased as the animals recovered. A prolonged acidosis was developed in a second group by gavage of an initial dose (1.5 mEq·100 g-1), followed by periodic maintenance doses (0.25 mEq·100 g-1) to prolong the disturbance for 8 h. The magnitude of the acidosis during this period was similar to that seen at 1 h after ingestion in the time-course study. A third group of larvae were given NaCl as a control for salt loading, which induced a small but significant respiratory acidosis. Unidirectional fluxes of Na+ and Cl- were examined during these serial ingestions. Salt loading inhibited the influx of the ingested ion. Na+ influx increased during the NH4Cl-induced acidosis. A fourth group of larvae were used to partition acid and ammonia excretion between the skin and the kidneys. These animals were given (NH4)2SO4 to allow re-examination of Cl- flux rates under non-Cl--loaded conditions. The ensuing acidosis had a reduced respiratory component and, therefore, pH did not decrease as much. Cl- influx rates did decrease significantly under these conditions. In both control and acidotic conditions, the majority of the acid efflux was as ammonia and the skin was the primary site of acid excretion. However, both the skin and the kidneys increased total acid excretion, although the efflux across the skin showed a much greater increase. This suggests a primary role for the skin in acid-base regulation in aquatic amphibians.