[en] Work designed to assess the potential of using a single material to sorb highly charged metal ions from aqueous solution and then microencapsulate and chemical fix those sorbed metal ions in vitreous silica is described. The basis for these studies is a chemically functionalized porous silica that is termed Diphosil. Diphosil was created by Chiarizia and coworkers (Solv. Extr. Ion Exch. 1996, 14(6), 1977-1100) as an ion exchange resin that strongly sorbs actinide and other highly charged metal ions from acid solutions. We have determined the maximum metal ion loading for Diphosil and shown that it sorbs trivalent ions from concentrated phosphoric acid. Using FT-IR analysis, we have shown that heating metal ion-loaded Diphosil in air converts its organic content primarily into carbon dioxide and water vapor. We have carried out studies on luminescence dynamics and spectroscopy, powder x-ray diffraction, and optical microscopy of metal ion-loaded Diphosil prior to and following heating in air. All of the results of our investigations are consistent with microencapsulation and chemical fixation of metal ions sorbed into Diphosil when that material is heated to 1273 K. In consequence, Diphosil is a promising basis for a single material approach to reducing nuclear waste volume by removing longlived alpha emitters from high level liquid radioactive waste and generating a vitreous silica nuclear waste form for the removed radionuclides that is suitable for geologic disposal.