Department of Chemistry, Art and Science Faculty, Balikesir University, Turkey.
Anal Chim Acta. 2011 Mar 18;689(2):184-9. doi: 10.1016/j.aca.2011.01.049. Epub 2011 Feb 1.
An off-line column preconcentration technique using a micro-column of 2,6 diacetylpyridine functionalized Amberlite XAD-4 with inductively coupled plasma mass spectrometry (ICP-MS) as a means of detection has been developed. The aim of the method was to determine rare earth elements (REEs) (La, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb and Lu) in seawater. Sample solutions (2-10 mL) were passed through the column which was then washed with ultra-pure water to remove residual matrix. The adsorbed cations on the resin were eluted by using 2 mL of 0.1 mol L(-1) HNO(3) containing 10 ng mL(-1) indium as an internal standard. The eluent was analyzed for the metal concentrations using ICP-MS. Sample pH as well as the sample and eluent flow rates were optimized. The sorption capacity of resin was determined by the batch process, by equilibrating 0.05 g of the resin with solutions of 50 mL of 25 mg L(-1) of individual metal ions for 4h at pH 6.0 at 26°C. The sorption capacities for the resin were found to range between 47.3 μmol g(-1) (for Lu) and 136.7 μmol g(-1) (for Gd). Limits of detection (3σ), without any preconcentration, ranged from 2 ng L(-1) to 10.3 ng L(-1) (for Tm and Lu respectively). The proposed method was applied to the determination of REEs in seawater and tap water samples.
已开发出一种使用 2,6 二乙酰基吡啶功能化 Amberlite XAD-4 微柱与电感耦合等离子体质谱 (ICP-MS) 作为检测手段的离线柱预浓缩技术。该方法旨在测定海水中的稀土元素 (REEs)(La、Ce、Pr、Nd、Sm、Eu、Gd、Tb、Dy、Ho、Er、Tm、Yb 和 Lu)。将样品溶液(2-10 mL)通过柱,然后用超纯水冲洗以去除残留基质。将树脂上吸附的阳离子用 2 mL 含 10 ng mL(-1) 铟作为内标物的 0.1 mol L(-1) HNO(3)洗脱。使用 ICP-MS 分析洗脱液中的金属浓度。优化了样品 pH 值以及样品和洗脱液流速。通过批处理过程确定树脂的吸附容量,将 0.05 g 树脂与 50 mL 50 mg L(-1) 的单个金属离子溶液在 pH 6.0 和 26°C 下平衡 4 h。树脂的吸附容量范围为 47.3 μmol g(-1)(对于 Lu)至 136.7 μmol g(-1)(对于 Gd)。无需预浓缩,检测限 (3σ) 范围为 2 ng L(-1) 至 10.3 ng L(-1)(分别对应于 Tm 和 Lu)。该方法已应用于海水和自来水样品中 REEs 的测定。