Sulfur was determined in plants and lichens by combustion of the sample and infrared detection of evolved sulfur dioxide using an automated sulfur analyzer. Vanadium pentaoxide was used as a combustion accelerator. Pelletization of the sample prior to combustion was not found to be advantageous. Washing studies showed that leaching of sulfur was not a major factor in the sample preparation. The combustion-IR analysis usually gave higher sulfur content than the turbidimetric analysis as well as shorter analysis time. Relative standard deviations of less than 7% were obtained by the combustion-IR technique when sulfur levels in plant material ranged from 0.05 to 0.70%. Determination of sulfur in National Bureau of Standards botanical reference materials showed good agreement between the combustion-IR technique and other instrumental procedures. Seven NBS botanical reference materials were analyzed.