We describe (207)pb NMR spectra and Al-27-(207)pb double resonance data that derive from a series of lead-containing zeolites. We propose that lead cations are strongly affected by the sorption of water, with the NMR spectra of the resulting material consistent with a chemical equilibrium between Pb2+ cations and PbOH+ cations. Double resonance experiments on dehydrated samples yield Pb-Al distances consistent with reported X-ray structure.