A new method for the determination of free Cu²⁺,Pb²⁺ and Cd²⁺ in environmental sample using potassium hexatitanate whisker as a solid-phase extractant and inductively coupled plasma-atomic emission spectrometry (ICP-AES) as a sensitive detector has been developed.The adsorption rate of Cu²⁺,Pb²⁺ and Cd²⁺ by potassium hexatitanate whisker was 98% at pH 5.0,and Cu²⁺,Pb²⁺ and Cd²⁺ could be eluted from potassium hexatitanate whisker with HNO3 (C:3 mol·L^-1).The Cu²⁺,Pb²⁺ and Cd²⁺ in environmental samples were preconcentrated with potassium hexatitanate whisker and determined by ICP-AES,the detection limits of Cu²⁺,Pb²⁺ and Cd²⁺ (3σ,n=9) were 0.007 1,0.006 8 and 0.007 1 μg·mL^-1,and the relative standard deviations (RSD) were 0.63%,0.61% and 0.50%,respectively.The method was applied to the determination of analytes in real samples,such as chrysanthemum and loquat leaf.And good results were obtained (recoveries were 90%-102.9%).The results obtained indicate that the potassium hexatitanate whisker has good regenerate capability.