A new, simple, rapid, and sensitive method was developed for the direct determination of trace bismuth (Bi) in sulfur samples by hydride generation atomic fluorescence spectrometry with microwave digestion in closed Teflon vessels. In the microwave oven, the samples were completely digested in 35 minutes using 3 mL concentrated nitric acid and 1 mL hydrogen peroxide at a pressure of 0.2-1.5 MPa. The analytical parameters, such as argon flow rate, acidity of the medium, the amount of NaBH4 and interfering ions on the recovery of bismuth were inv...