Chemistry Department, Analytical Chemistry Division, Wroclaw University of Technology, Wybrzeze Wyspiańskiego 27, 50-370 Wroclaw, Poland.
J Hazard Mater. 2010 Oct 15;182(1-3):477-83. doi: 10.1016/j.jhazmat.2010.06.057. Epub 2010 Jun 19.
A cloud point extraction (CPE) procedure for the simultaneous separation and preconcentration of Cd, Co, Cr, Cu, Mn, Ni, Pb and Zn from materials rich in calcium prior to trace element analysis by inductively coupled plasma optical emission spectrometry (ICP OES) was developed. The method is based on the formation of hydrophobic complexes of the metal ions with PAN or 5-Br-PADAP, followed by their extraction into a surfactant-rich phase using Triton X-114 as the surfactant. The main variables affecting the extraction process, such as pH, concentration of surfactant and chelating agent were optimised. Under the optimum conditions the obtained limits of detection for Cd, Co, Cr, Cu, Mn, Ni, Pb and Zn were of 4.0, 4.3, 2.1, 1.9, 0.3, 5.6, 40 and 2.0 microg L(-1), respectively. The RSD values for 10 replicates were from 1.5% for Mn to 11% for Pb. The accuracy of the procedure was verified by analysis of certified reference material NIST 1400 (Bone Ash) and by recovery tests. The optimised method was successfully applied for the simultaneous determination of trace elements in dolomites used by different fertiliser factories.
建立了一种用于电感耦合等离子体发射光谱（ICP-OES）分析前从富含钙的材料中同时分离和预浓缩 Cd、Co、Cr、Cu、Mn、Ni、Pb 和 Zn 的浊点萃取（CPE）程序。该方法基于金属离子与 PAN 或 5-Br-PADAP 形成疏水性配合物，然后使用 Triton X-114 作为表面活性剂将其萃取到富含表面活性剂的相中。优化了影响萃取过程的主要变量，如 pH 值、表面活性剂和螯合剂的浓度。在最佳条件下，获得的 Cd、Co、Cr、Cu、Mn、Ni、Pb 和 Zn 的检出限分别为 4.0、4.3、2.1、1.9、0.3、5.6、40 和 2.0μg L(-1)。10 个重复的 RSD 值从 Mn 的 1.5%到 Pb 的 11%不等。通过分析 NIST 1400（骨灰）标准物质和回收测试验证了该程序的准确性。优化后的方法成功应用于不同肥料厂使用的白云石中痕量元素的同时测定。
