Ion exchange with atomic absorption methods has been used to determine the anionic she concentrations of membranes and membrane-support materials: poly(vinyl chloride) (PVC) and carboxylated PVC. Total she concentrations can be determined. Impedance measurements of site-controlled membranes prove that not all sties are available to K+ In PVC-C-OOH based neutral carrier membranes. The theory of selectivity, based on the. assumption that the carrler/avallable site concentration ratio Is the most Important factor, Is thoroughly tested. New results on site concentration control by tetraphenylborate ( ) and tetrakls(p -chlorophenyl)borate emphasize the systematic variation of selectivity with carrler/slte ratio. At low carrier levels, TPB" can be spontaneously lost from membranes until the unity carrler/slte ratio Is achieved.