The classic methods for characterizing transport of individual ions in membranes, such as steady-state streaming potential and membrane potential, apply in a straightforward way only to thick single-layer membranes. Application of these techniques to industrial composite RO and NF membranes has been largely unsuccessful, since these membranes have a multilayer structure, in which the in situ-prepared active layer is only a tiny fraction of the total diffusion resistance [1,2]. As a result of the polarization in the supporting layers, the “salt” phenomenological parameter, e.g., the permeability ws and reflection coefficient s deducible from filtration experiments, cannot be split into individual parameters of ions. Still more difficult is splitting the ionic permeabilities into the partitioning and diffusional factors. Such information could be however highly useful, both from the fundamental viewpoint of understanding the ion exclusion in membranes and from a practical viewpoint of developing predictive models of electrolyte separation for multicomponent salt mixtures. It has been pointed out that non-steady-state techniques, e.g., potential transients after rapidly changing the concentration or pressure gradient across the membrane, should have advantages over steady-state measurements [2,3]. The use of transients allows observation of different phenomena at various timescales and getting separate information on the partitioning and diffusion components of the permeability (cf. the popular time lag method). A novel technique presented in this study combines the use of a single layer in absence of external polarization with the use of a non-steady-state technique. The measurements employ a free-standing single layer of polyamide isolated from a genuine commercial membrane and placed on a solid electrode, which is characterized by means of electrochemical impedance spectroscopy (EIS) [4]. This approach effectively eleiminates both the polarization in support and ion coupling, which has been the main problems so far, and is capable of producing a comprehensive picture of ion transport in the polyamide layer.