The<b> </b>measurement of ²¹⁰Pb is significant in environmental studies. Lead separation in HCl solution is a vital procedure but suffers from poor efficiency with high labor and time costs. To overcome this problem, a novel anion exchange resin was synthesized and characterized by different techniques followed by studies on the adsorption behaviors towards lead in HCl solution. The results suggest that SiPS-N(CH₃)₃Cl was successfully prepared with small

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... size, low water swelling rate, and large specific surface area. The maximum anion exchange capacity resulted from quaternary amine groups was determined to be 1.0 mmol (Cl^-)/g.The adsorption activities reached equilibrium within 3 min under selected conditions offering extremely fast adsorption kinetics. The synergistic adsorption mechanism, the multilayer adsorption mechanism, and the competition from co-existing chloride anions were found to be responsible for the lead adsorption performance of SiPS-N(CH₃)₃Cl. Column experiments showed that the feeding volume of lead and HCl had impact on the chemical yield regardless of the co-existence of high concentrations of FeCl₃ (90 mM) and a high flow speed (4.0 mL/min). Based on these results, a separation process integrating SiPS-N(CH₃)₃Cl and the matched parameters was finally developed and tested. Our work greatly raised the lead separation efficiency in HCl solutions with implications for measuring ²¹⁰Pb in environmental samples.