This invention relates in part to a process for producing high purity acetylene by withdrawing a crude acetylene stream from a storage source, and passing said stream through an adsorbent bed that contains layered adsorption media to selectively remove moisture, solvent and carbon dioxide from the stream, thereby producing the high purity acetylene. The adsorption media is regenerated in-situ. The high purity acetylene product is useful as a source material for depositing carbon and carbon-containing films in semiconductor applications.