The phosphorylated sago starch-extraction residue (P-SR) was produced for the removal of heavy metal from wastewater. The phosphoric ester in the phosphorylated residue was evaluated by means of infrared microspectrometry and solid-state NMR. In this study, the phosphorus contents of produced P-SR, phosphorylated cellulose (P-C), and phosphorylated sago starch were 31.7, 34.2, and 4.6 mg/g, respectively. The phosphorus contents of P-C and sago starch were clearly different because of the difference of each structure. The maximum sorption capacities of heavy metals (cadmium, lead, copper, and zinc) in single heavy metal sorption on P-SR were 0.20, 0.25, 0.36, and 0.24 mmol/g (Cu > Pb > Zn > Cd), respectively. On the other hand, the amount of sorbed heavy metals in coexisted heavy metal sorption on P-SR followed the order of Pb > Cu > Cd > Zn that was different from the relations of maximum sorption capacities for individual heavy metals. The heavy metal sorption behavior in single and coexisted heavy metal solution for P-SR were different and P-SR showed the intrinsic heavy metal sorption affinity, called as selective sorption. (C) 2011 Wiley Periodicals, Inc. J Appl Polym Sci, 2012