In this work, the dispersion of triphenylsulfonium metal-fluoride salts in polymer films modeling chemically amplified resist systems has been characterized by solid-state 19F multiple-quantum nuclear magnetic resonance (MQ-NMR). Previously, this technique has been used to characterize 1H distributions on a length scale of approximately 20 angstroms in various materials. In agreement with differential scanning calorimetry, metal- fluoride salts were shown to be immiscible with the nonpolar polymers, poly-n- butylmethacrylate (PnBMA) and poly-isobutylmethacrylate (PiBMA), with no indication of individual salt molecules solubilized within the polymer matrix. Metal-fluoride salts in poly- methylmethacrylate (PMMA) were observed to be dispersed on a molecular scale even at a salt loading of 20% wt/wt. Although observed by electron microscopy, evidence of larger aggregates is absent in the MQ-NMR data of the salt/PMMA films, indicating that these aggregates represent a small fraction of the total salt in these films. In addition, unlike electron microscopy, MQ-NMR is nondestructive with respect to the photosensitive salt and polymers comprising resist systems.