We examined the effects of acute low-pH exposure on ion balance (Na+, Cl-, K+) in several species of fish captured from the Rio Negro, a dilute, acidic tributary of the Amazon. At pH 5.5 (untreated Rio Negro water), the four Rio Negro species tested (piranha preta, Serrasalmus rhombeus; piranha branca, Serrasalmus cf. holandi; aracu, Leporinus fasciatus; and pacu, Myleus sp.) were at or near ion balance; upon exposure to pH 3.5, while Na+ and Cl- loss rates became significant, they were relatively mild. In comparison, tambaqui (Colossoma macropomum), which were obtained from aquaculture and held and tested under the same conditions as the other fish, had loss rates seven times higher than all the Rio Negro species. At pH 3.0, rates of Na+ and Cl- loss for the Rio Negro fish increased three- to fivefold but were again much less than those observed in tambaqui. Raising water Ca2+ concentration from 10 micromol L-1 to 100 micromol L-1 during exposure to the same low pH's had no effect on rates of ion loss in the three species tested (piranha preta, piranha branca, aracu), which suggests that either they have such a high branchial affinity for Ca2+ that all sites are saturated at 10 micromol L-1 and additional Ca2+ had no effect, or that Ca2+ may not be involved in regulation of branchial ion permeability. For a final Rio Negro species, the cardinal tetra (Paracheirodon axelrodi), we monitored body Na+ concentration during 5 d of exposure to pH 6.0, 4.0, or 3.5. These pH's had no effect on body Na+ concentration. These data together suggest that exceptional acid tolerance is a general characteristic of fish that inhabit the dilute acidic Rio Negro and raise questions about the role of Ca2+ in regulation of branchial ion permeability in these fish.