The present study focuses on the adsorption of Pb(II) by the H-form of titanosilicates (ETS-4, GTS-1) and clinoptilolite. The H-forms were prepared by first exchanging the extra-framework cations—Na+, K+, Ca2+, etc.—with NH4+, and by subsequent thermal treatment for obtaining H-forms. The purity and thermal behaviour of the initial, NH4+, and H-forms of ETS-4, GTS-1, and clinoptilolite were analysed by powder XRD, while the morphology and size of the particles were determined by SEM. The chemical composition of the solids and the solutions was obtained by WDXRF and ICP-OES, respectively. The kinetics research of the Pb(II) adsorption processes was based on WDXRF and ICP-OES. The H-forms of the materials displayed favourable properties for the adsorption of Pb(II). The best behaviour in this respect was demonstrated by GTS-1 when compared to ETS-4 and clinoptilolite.