以电感耦合等离子体原子发射光谱法(ICP-AES)为检测手段,研究了新型吸附剂六钛酸钾晶须对环境样品中Cu(Ⅱ),Pb(Ⅱ),CA(Ⅱ)的分离/富集行为以及解脱的主要因素,并考察了共存离子的干扰影响。在pH值为5.0,振荡时间为5min,静置时间为30min时,吸附率可达到95%以上。以3mol·L^-1,HNO3作为解脱剂,沸水浴加热40min,振荡5min,静置40min,可将吸附在六钛酸钾晶须上的Cu(Ⅱ),Pb(Ⅱ)。Cd(Ⅱ)定量洗脱。测定Cu(Ⅱ),Pb(Ⅱ),CA(Ⅱ)的检出险分别为0.0071,0.0068,0.0071μg·mL^-1,相对标准偏差(RSD)为0.63%,0.61%,0.50%。在优化的实验条件下,将其用于菊花和琵琶叶中Cu(Ⅱ),Pb(Ⅱ),CA(Ⅱ)含草的测定,加标回收率在90%~102.9%之间。
A new method for the determination of free Cu^2+ , Pb^2+ and Cd^2+ 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 Cu^2+ , Pb^2+ and Cd^2+ by potassium hexatitanate whisker was 98% at pH 5.0, and Cu^2+ , Pb^2+ and Cd^2+ could be eluted from potassium hexatitanate whisker with HNO3 (C 3 mol· L^-1 ), The Cu^2+ , Pb^2+ and Cd^2+ in environmental samples were preconcentrated with potassium hexatitanate whisker and determined by ICP-AES, the detection limits of Cu^2+ , Pb^2+ and Cd^2+ (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,