Off-gases from industrial prodn. of superphosphate by acid treatment of Ca(3)(PO)(2) were analyzed by gas chromatog. for alkanes cycloalkanes and org. S compds. The highest emissions of Et(2)CHMe and Me(2)CHEt (1791 and 1690 mg/t of P(2)O(5) produced, resp.) were obsd. Odorous MeS(Me)CHEt and MeS(Me)ChPr were also identified (425 and 367 mg/t of P(2)O(5), resp.).