A river ecosystem in East Java, Indonesia, fed by a volcanic lake with high concentrations of dissolved metals and a low pH, was found to support only few macroinvertebrates. To unravel the causes of toxicity and to determine the level of dilution necessary to obtain non-toxic water, a bioassay was conducted with the fairy shrimp Thamnocephalus platyurus. A partial toxicity identification evaluation (TIE) approach was used with EDTA as a chelating agent to relate toxicity to pH and metal concentrations. Three water samples were tested, with pHs ranging from 0.72 to 4.5, and diluted with water from a neutral river to different degrees. The dilution factor necessary to achieve no more than 50% mortality in the Thamnotox test (Ldf(50)) varied from >300 at the most acidic site, to 7 for water of pH 2.6 and 1.5 for water of pH 4.5. Toxicity was best explained from both low pH and high concentrations of metals, especially Al and Fe. The key role of Al and Fe in the toxicity was confirmed by relating concentrations of the different compounds in the river water to toxicity data from the literature. EDTA addition did not significantly influence Ldf(50) or the lethal pH 50% (LpH(50)), suggesting a large effect, besides cationic components and pH, of anions (F, SO(4) and Cl).