Abstract: A method for preparing compounds of sulfur, selenium, and tellurium includes the formation of the compound from the elements in a closed environment which excludes oxygen, and then the purification of the compound by contacting it with carbon or carbon monoxide. Oxygen, the principal contaminant in conventionally prepared compounds of this group, is excluded from the formation of the compound in the formation step by using a closed reactor, preferably made of vitreous silica. Oxygen in the initial elemental reactants remains in the compound made in this way, and the purification step eliminates the oxygen originally present in the elemental reactants from the compound. Arsenic triselenide made by this approach, glassy and of high purity, is suitable for use in applications requiring infrared transparency.