The discovery, extraction, and monopolistic control of key natural resources was a priority of New Spain's colonial administration. Managing the region's abundant resources, however, often proved difficult for the Spanish Crown. Human and environmental challenges impeded protoindustrial growth and development, and monopolistic control of resources often met resistance. In this article I examine these processes in the context of New Spain's little-known monopoly on sulphur—a yellow, powdery mineral the Crown jealously guarded as its own. Sulphur was critical for gunpowder and explosives production, yet the Crown often failed to produce enough of it to meet the growing demand by its military and the silver blast-mining industry. Colonial documents reveal administrators’ attempts to improve sulphur production through reform measures, which included advising sulphur miners on how to discover sulphur deposits and, eventually, how to develop their mines. Efforts to improve sulphur production were moderately successful, although the process was messy and inefficient.