The use of a sulfur-impregnated organoclay provides a mercury or arsenic removal media having increased reactivity, stability, and mercury removal ability. The Hg/As removal media described herein is prepared by impregnating an organophilic clay with elemental (free state) sulfur. Alternatively, the clay can be made organophilic by onium ion reaction prior to or simultaneously with impregnating the organoclay with sulfur.