Nanoscale Tb-active coordination polymers Tb(BTC)(H2O)(6) were facilely, rapidly and environmentally-friendly fabricated at room temperature. The structures of the samples were confirmed by powder X-ray diffraction and elemental analyses, and the morphologies were characterized by SEM. The studies of the photoluminescence properties reveal that these nanostructured coordination polymers exhibit green emission, corresponding to the D-5(4) -> F-7(J) transitions of the Tb3+ ions under UV light excitation, which represents highly selective and sensitive sensing for metal ions and acetone molecules in aqueous solution, and the probable sensing mechanisms were discussed.