Urinary fluoride was evaluated as an exposure index for a prospective study of asthma in an aluminum smelter. Two studies were conducted to evaluate the relationship between airborne exposure and urinary excretion over a workweek, and to describe exposures among jobs and over time. Thirty-two subjects were evaluated on Days 1 and 3 of a 3-day workweek. On each day, spot urine samples were collected prior to the start of work and again at the end of the shift. Samples were analyzed for fluoride and expressed as milligrams fluoride per gram of creatinine. Airborne exposures to total particulate, fluoride particulate, and hydrogen fluoride (HF; using a 37-mm filter cassette containing a filter and treated back-up pad) were also evaluated on each subject. In the second study, postshift urine samples were collected from asthma study volunteers in three surveys extending over 1.5 years and analyzed for fluoride. Average airborne exposures were 15.7, 4.1, and 0.7 mg/m3 for particulates, particulate fluorides and HF, respectively, and were substantially higher among carbon setters than other workers. However, average urine fluorides among the same workers were reasonably low, 1.3 and 3.0 mg/g creatinine in pre- and postshift urine samples, respectively. Carbon setters, who routinely wore respiratory protection during high exposure periods, had urinary fluoride levels similar to those of other potroom personnel. A significant variation in dose, as expressed by postshift urinary fluoride levels, was observed between potroom and nonpotroom jobs and over three survey periods. These results suggest that postshift urinary fluorides provide a reasonable exposure index for surveillance of exposure levels for an epidemiologic study, and that a substantial variation of exposure occurs between jobs and over time. Although urinary fluorides may be used for exposure surveillance, additional details on individual exposure agents and patterns of exposure over time are required for complete assessment.