Samples of Mn(II) Nafion, MN(II)-A zeolite, and various Co(II)-ZSM-5 zeolites were prepared by aqueous ion exchange techniques. Co(II)- and Mn(II)-containing ZSM-5, erionite, and mordenite were obtained from other sources. Co(II)-containing samples were studied by diffuse reflectance spectroscopy in the dehydrated state and after exposure to NO atmosphere. In addition, the magnetic susceptibilities of these samples were determined. It was shown that two NO molecules were adsorbed onto each Co(II) ion in ZSM-5 and erionite. The visible spectrum of these materials was complex and contained absorption bands corresponding to Co(II) ions in different coordination states. NO desorbed from Co(II) high silica zeolites at temperatures under 190{degrees}C, while it completely desorbed from Co(II) Nafion below 160{degrees}C. The catalytic activity of Co, Cu, and Mn Nafion samples for NO decomposition was probed, but no activity was observed. Optical absorption and luminescence studies are being initiated with Mn(II)-containing samples.