Systems that are capable of removing highly toxic anions from wastewater effluents, even at extremely low concentrations, are a major need in the defense industry. This study reports on the features of two new batch and continuous-flow sorption processes with regard to ultimate removal and recovery of the perchlorate (ClO4-) anion from ammonium perchlorate (NH4ClO4) wastewater. The sorbent developed is a crosslinked poly(allylamine hydrochloride) (PAA . HCl) polymeric hydrogel. The pH-sensitive PAA . HCl hydrogels were synthesized by chemically crosslinking a solution of linear PAA . HCl chains with epichlorohydrin (EPI). The perchlorate-binding capacity of the polymer gels was measured in standard solutions and studied as a function of gel synthesis parameters. Equilibrium perchlorate loadings of 5770 +/- 870 mg ClO4-/g gel were calculated from measurement of the decrease in perchlorate concentration in aqueous standard solutions using UV-Vis spectrophotometry. Batch experiments in wastewater originating from the Naval Surface Warfare Center (NSWC) Indian Head Division showed that perchlorate concentrations decreased by 85% Preliminary lab-scale packed-column experiments in wastewater achieved up to 40% reduction in total perchlorate content. The regeneration ability of the gels was demonstrated by release of the bound perchlorate anions, upon washing with a LN NaOH solution, providing opportunities to recover and reuse the hydrogel over multiple regeneration cycles. The PAA . HCl hydrogels are demonstrated to be appropriate materials for treating wastewaters that contain ammonium perchlorate.