Eleven new heterocyclic mono-and diquaternary salts have been prepared by reaction of 1,2-bisazolyl- and 1,2 bisbenzazolyl-ethanes with meth;'.' sulfate or methyl fluorosulfonate. Their structure has been established by means of 1H and 1 C NMR spectroscopy. Homonuclear COSY and NOESY experiments and 2D-heteronuclear correlations have been performed when necessary to assign all NMR signals.