A new process is described for the preparation of chito an gel beads using molybdate as the gelling agent. This new gelation technique leads to a structure different from that produced during alkaline coagulation of a chitosan solution. Instead of a morphology characterized by large open pores, gel beads produced in a molybdate solution, under optimum conditions (pH 6; molybdate concentration, 7 g(.)L(-1)), have a double layer structure corresponding to a very compact 100-mum thick external layer and all internal structure of small pores. Experimental conditions, especially pH and molybdate concentration, were selected to optimize molybdate content and the stability of the bead shape.