In this study, the luminescent macromolecular lanthanide complexes Ln-PSt/AA (Ln = Eu and Tb; St = styrene; AA = acrylic acid) have been synthesized, and an extensive characterization has been carried out by means of elemental analysis, FTIR, thermal analysis, and fluorescence determination. The results showed that the carboxylic groups on the chain of the polymers acted as bidentate ligands coordinated to lanthanide ions; and the coordination degree of -COO-/Ln(3+) in the macromolecular complexes was closely dependent on both the pH value of the solution and the molar ratio of St to AA in the polymeric ligands. Thermal analysis manifested that these Ln-PSt/AA (Ln = Eu and Tb) complexes had high thermal stability and solvent resistance, and these macromolecular complexes were highly crosslinked. The fluorescence determination indicated that Ln-PSt/AA complexes could emit characteristic fluorescence with comparatively high brightness and good monochromaticity, and the fluorescence intensity changed with increasing lanthanide ions content. (C) 2009 Wiley Periodicals, Inc. J Appl Polym Sci 114: 1064-1069, 2009