This work describes a novel method for fast esterification of spent grain to enhance its cationic adsorption capacity. The esterification of spent grain with citric acid was achieved by using sodium hypophosphite monohydrate (NaH(2)PO(2)center dot H(2)O) as a catalyst in N,N-dimethylformamide (DMF). Fourier transform infrared (FTIR) spectroscopic analysis revealed the formation of ester groups after esterification, demonstrating that spent grain was successfully esterified with citric acid. The adsorption capacity of esterified spent grain (ESG) for each metal ion was greatly improved as compared with that of raw spent grain (RSG). Typically, Pb(2+) adsorption capacity increased from 125.84 mg g(-1) of RSG to 293.30 mg g(-1) of ESG. This increase can be attributed to both the formation of ester linkage and the grafting of carboxyl groups on spent grain. The results suggest that a fast process for esterification of spent grain has been realized and ESG has strong ability to adsorb heavy metal ions. (C) 2010 Elsevier Ltd, All rights reserved.