A surface-enhanced Raman scattering (SERS) substrate containing silver particles was prepared by an acid-catalyzed sol-gel method. Silver nitrate was first doped into the sol-gel film followed by chemical reduction of the silver ions with sodium borohydride to produce silver particles. This silver-doped sol-gel substrate exhibits strong enhancement of Raman scattering from adsorbed uranyl ions with a detection limit of 8.5 x 10(-8) M, which is comparable to existing methods of uranyl detection such as spectrophotometry, fluorometry, and a SERS method based on ligand-modified solution silver colloids. However, in the present method, no preconcentration steps, chromogens, or complexing ligands are needed. Compared with the SERS method using Ag colloidal sols, the silver-doped sol-gel film has the advantage that the silver particles trapped in the sol-gel matrix are much more stable than Ag colloids in liquid media. Furthermore, porous silica sol-gel materials are known to have affinities toward many inorganic and organic molecules. The enhanced adsorption affinities could also lead to the increased SERS sensitivity. The performance of the new silver-doped sol-gel substrate was evaluated with uranyl ions and compared to that of a SERS substrate based on silver-coated silica beads prepared by vacuum deposition. The detection limit for the silver-doped sol-gel film was 104 times lower than that for the silver-coated silica beads. The sol-gel substrate was further used to obtain, for the first time, the surface-enhanced Raman spectrum of neptunyl ions in dilute aqueous solutions.