We report a fatal case of hydrofluoric acid (HF) ingestion with suicidal intent. Quantitation using an ion-selective electrode for fluoride in fresh bile, gastric contents, kidney, liver, skeletal muscle, urine, and vitreous humor yielded 6.5, 39.0, 10.0, 6.0, 4.5, 5.0, and 4.5 ppm, respectively. In addition to the unfixed specimens, fluoride ion was measured in the following fixed tissue: brain, heart, kidney, liver, pancreas, stomach, and heart. Tissues were measured directly and/or by using the technique of standard addition. Fluoride concentrations using either method were found to be comparable. Fluoride concentration in fresh tissue was consistent with toxicity, although the urine fluoride concentration was in the range observed for asymptomatic workers exposed to fluoride in air. Fixed tissue preparations revealed fluoride concentrations consistent with nonexposure, whereas examination of the formalin fixative revealed fluoride concentrations only slightly higher than negative control formalin. We conclude that fixed tissues are inappropriate for fluoride determination. This is the first case we are aware of that provides fluoride concentrations in skeletal muscle in a fatality involving HF ingestion.