The fumes and dust of trace elements and their compounds are very toxic and have been related to an increase in the incidence of diseases. Occupational exposure to toxic metals and metalloids can be determined by means of workplace air measurements and biological monitoring. The aim of our investigation was to determine the concentrations of As, Hg, and Se in urine samples under routine clinical laboratory conditions. To assess the reliability of these methods, critical factors such as detection limit(s), calibration range(s), cost, accuracy, and precision were studied. The method was employed for the quantitative determination of arsenic, mercury, and selenium in urine samples from steel production and quality control workers and healthy unexposed controls. After pretreatment with acids, the samples were digested by means of a microwave oven. Arsenic was determined by hydride atomic absorption spectrometry and mercury was determined by cold vapor atomic absorption spectrometry, whereas selenium was determined by a graphite furnace atomic absorption spectrometry. The results indicate those urinary arsenic, mercury, and selenium levels of the exposed workers are significantly higher than those of the controls. The possibility that these elements are involved in the etiology of diseases is discussed and recommendations are made to improve workplace ventilation and industrial hygiene practices.