The characterization and magnetic behavior of Co(II) and Gd(III) polyacrylates prepared by organic gelation synthesis have been studied. Gd(III)-polyacrylate shows a higher thermal stability due to stronger ionic interactions. IR spectra of both compounds reveal that carboxylate groups and water molecules exist in the coordination sphere with various forms of complexation. The samples are x-ray amorphous and have complex structures with the randomly distributing metal atoms along the PAA chain. The a.c. susceptibility measurements between 4.2 K and 250 K indicated a low temperature magnetic ordering. Annealing the samples at 160 degrees C for 48 h result in the appearance of a spin-glass behavior in the in-phase and out-of-phase susceptibility curves. The presence of different sizes and shapes of clusters, however, precludes the determination of effective magnetic moments and Curie temperatures. (C) 1995 John Wiley and Sons, Inc.