Researchers have performed evaluations on Nafion membranes for many years. An important aspect of the membranes is their chemical composition and uniformity. One technique that could provide accurate and fast quantitative measurements of the chemical composition and water within the membranes is prompt-gamma neutron activation analysis (PGAA). In this work, PGAA was applied to the chemical characterization of Nafion membranes in various forms. The evaluation confirmed the necessity of pretreatment of the membranes for the elimination of contamination. A series of counterion-exchanged membranes were examined so that we could determine the degree of conversion achieved under different conditions and residual water levels. The results indicated that the type of counterion was an important factor determining conversion levels, that partial conversion could be achieved, and that counterion displacement could be forced to occur in certain environments. (C) 2003 Wiley Periodicals, Inc.