Sulfur has been purified by a dynamic pyrolysis procedure that takes into account the unique viscosity-temperature relationship of the liquid. An apparatus is described that incorporates gas-bubbling and rocking to overcome diffusion-limited kinetics. For the first time, a mechanism is proposed for the pyrolytic purification of sulfur based upon Carsul formation and the H2S ↔ H2Sx equilibrium. Infrared methods are delineated for qualitative analysis and quantitative estimates of anion contaminants, including the omnipresent hydrocarbon impurities. Our purified sulfur has a total carbon, oxygen, and hydrogen impurity level of <10 μg/g.