Europium triundecylenate, Eu(UA)3, and terbium triundecylenate, Tb(UA)3, were prepared by the method described in our previous paper. Either Eu(UA)3or Tb(UA)3was dissolved in methacrylic acid (<20%) and copolymerized as a crosslinker with methyl methacrylate (>80) by bulk polymerization in molds made of two glass plates. The fluorescence spectroscopy of these Eu- or Tb-containing polymers under ultraviolet/visible excitation light was investigated. The fluorescence spectroscopy of solutions of Eu(UA)3or Tb(UA)3in methacrylic acid was measured and compared with that of the solid-state Eu- or Tb-containing polymers. The fluorescence excitation and emission spectra of the solutions and polymers showed the characteristic features of free Eu3+or Tb3+. The lifetime fluorescence of the solutions and polymers with Eu3+are also included.