纳米氧化铝微柱富集ICP-AES测定大白口蘑中的痕量稀土元素

Separation/Preconcentration of Trace Rare Earth Elements in Tricholoma Giganteum by Micro-Column with Nanometer Al_2O_3 and Their Determination by ICP-AES

以负载了1-苯基-3-甲基-4-苯甲酰基-吡唑酮[5](PMBP)的纳米氧化铝为微柱吸附材料,采用电感耦合等离子体原子发射光谱法(ICP-AES),系统地研究了其在动态条件下对稀土离子Sc^(3+),Y^(3+)和La^(3+)的吸附性能,并确定了最佳吸附及解脱条件。实验结果表明:在pH为4.5时,分析物均可被上述吸附材料定量吸附;用0.5 mol·L^(-1)盐酸溶液可将吸附在微柱上的稀土离子完全解脱。该方法对Sc^(3+),Y^(3+)和La^(3+)的检出限分别为0.15,0.18和0.34μg·L^(-1);相对标准偏差(RSD)分别为2.5%,3.0%和1.7%(n=12,c=0.5μg·L^(-1))。方法应用于大白口蘑(Tricholoma giganteum)中痕量Sc,Y和La的测定,结果满意。

Using a micro-column packed with immobilized 1-phenyl-3-methyl-4-bonzoil-5 pyrazone（PMBP） on nanometer Al2O3 powder as the adsorption material, the adsorption and elution behaviors of rare earth ions（Sc^3＋ , Y^3＋ and La^3＋） on the above material under dynamic conditions were studied with inductively coupled plasma-atomic emission spectrometry. The conditions for preconcentration of rare earth ions were optimized, and the results show that the studied ions can be adsorbed quantitatively on the above material at pH 4. 5 and the analytes adsorbed on the column can be eluted with 0.5 mol · L^-1 HCl solution. The detection limits of the method for Sc, Y and La were 0.15, 0.18 and 0. 34μg · L^-1, respectively, and the relative standard deviations were 2.5%, 3.0~ and 1.7%, respectively（n=12, c=0.5 mg · L^- 1） . The proposed method was applied to the determination of trace amount of Sc, Y and La in Tricholoma giganteum with satisfactory results.