We present a safe and efficient technique to generate HCl/DCl gas for use in the classic physical chemistry experiment that introduces students to ro-vibrational spectroscopy. The reaction involves thionyl chloride and a mixture of water and deuterium oxide to produce HCl/DCl gas with SO[subscript 2] gas as a byproduct. The entire reaction is carried out in a microscale apparatus at atmospheric pressure. (Contains 3 figures.)