Abstract: A method of removing or recovering a volatile organopolysiloxane such as octamethylcyclotetrasiloxane (D.sub.4) from a fluid stream such as air, containing the volatile organopolysiloxane and a hydrocarbon, for example, by adsorbing the volatile organopolysiloxane on dry soil contained in a column, and allowing the remainder of the fluid stream including the hydrocarbon to pass through the column. The dry soil containing the adsorbed volatile organopolysiloxane and any degradation product(s) is then wetted by passing moist air, water, or steam, through the column to desorb, vaporize, and remove the volatile organopolysiloxane from the column. The column containing the wet soil can then be regenerated by air drying the wet soil, and the separating cycle is repeated.