D.I.S.T.E.M. Department, Università di Palermo, via Archirafi, 36, 90123 Palermo, Italy.
Talanta. 2013 Nov 15;116:1085-90. doi: 10.1016/j.talanta.2013.08.019. Epub 2013 Aug 23.
Very low concentrations (pg mL(-1) or sub-pg mL(-1) level) along with the high salinity are the main problems in determining trace metal contents in seawater. This problem is mainly considered for investigations of naturally occurring YLOID (Y and Lanthanides) and Zr and Hf in order to provide precise and accurate results. The inductively coupled plasma mass spectrometry (ICP-MS), both in high and low resolution, offers many advantages including simultaneous analyses of all elements and their quantitative determination with detection limits of the order of pg mL(-1). However in the analysis of YLOID in seawater, a better determination needs an efficient combination of ICP-MS measurement with a pre-concentration technique. To perform an ultra-trace analysis in seawater, we have validated an analytical procedure involving an improved modified co-precipitation on iron hydroxides to ensure the simultaneous quantitative recovery of YLOID, Zr and Hf contents with measurement by a quadrupole ICP-MS. The validity of the method was assessed through a series of co-precipitation experiments and estimation of several quality control parameters for method validation, namely working range and its linearity, detection limit, quantification limit, precision and spike recoveries, and the methodological blank choice, are introduced, evaluated and discussed. Analysis of NASS-6, is the first report on the latest seawater reference material for YLOID, hafnium and zirconium.
极低的浓度(pg/mL 或亚 pg/mL 水平)以及高盐度是测定海水中痕量金属含量的主要问题。这个问题主要是为了研究天然存在的 YLOID(Y 和镧系元素)和 Zr 和 Hf 而考虑的,目的是为了提供精确和准确的结果。电感耦合等离子体质谱(ICP-MS),无论是在高分辨率还是低分辨率下,都具有许多优势,包括同时分析所有元素及其定量测定,检测限可达 pg/mL 级。然而,在海水中 YLOID 的分析中,为了更好地测定,需要将 ICP-MS 测量与预浓缩技术有效地结合起来。为了在海水中进行超痕量分析,我们验证了一种分析程序,该程序涉及在铁氢氧化物上进行改进的改良共沉淀,以确保同时定量回收 YLOID、Zr 和 Hf 的含量,并通过四极 ICP-MS 进行测量。通过一系列共沉淀实验和对几种方法验证质量控制参数的评估,介绍、评估和讨论了方法的有效性,即工作范围及其线性、检测限、定量限、精密度和加标回收率以及方法空白的选择。对 NASS-6 的分析是对最新的 YLOID、铪和锆海水参比物质的首次报告。