A direct analytical technique for measuring the solution quantum efficiencies of photoacid generators (PAGs) is presented. The technique is based on the nonaqueous potentiometric titration of the photogenerated acid and does not require separate calibrations, or the addition of sensing materials such as dyes or bases. Solutions of PAGs in acetonitrile were irradiated at 248 nm and subsequently titrated with known concentrations of triethanolamine base. The only quantities required for an accurate determination of the quantum efficiency are the incident radiation energy and the titration equivalence point. A mathematical analysis that enables this calculation is derived, and a table with calculated quantum efficiency values for three classes of PAGs having a variety of counterions is presented. The method is simple, accurate, and applicable to any class of PAG molecules. (C) 2005 American Vacuum Society.