Method for the purification of a volatile metal hydride comprising obtaining a volatile metal hydride feed containing one or more acidic impurities, one of which is a sulfur-containing impurity; contacting the feed with an alkaline material and reacting at least a portion of the sulfur-containing impurity with the alkaline material to remove a portion of the sulfur-containing impurity from the feed and provide an intermediate purified material, wherein the contacting of the feed with an alkaline material is effected at a sub-ambient temperature; and contacting the intermediate purified product with an adsorbent material to remove at least a portion of the sulfur-containing impurity from the intermediate purified material and provide a purified volatile metal hydride product.