Gao Ying, Xu Mo, Sturgeon Ralph E, Mester Zoltán, Shi Zeming, Galea Raphael, Saull Patrick, Yang Lu
†Chemical Metrology, Measurement Science and Standards, National Research Council Canada, Ottawa, Ontario K1A 0R6, Canada.
‡State Key Laboratory of Geohazard Prevention and Geoenvironment Protection, Chengdu University of Technology, Chengdu, Sichuan 610059, China.
Anal Chem. 2015 Apr 21;87(8):4495-502. doi: 10.1021/acs.analchem.5b00533. Epub 2015 Mar 31.
A novel and sensitive approach for the accurate and precise determination of Pb in environmental samples is presented using transition metal ion-assisted photochemical vapor generation (PVG) for sample introduction with multicollector inductively coupled plasma mass spectrometry (MC-ICPMS) detection. A significant improvement in PVG efficiency of lead is achieved in the presence of transition metal ions (Co(2+) and Ni(2+)) in solutions of 5% (v/v) formic acid. The determination of Pb in digests of sediment or soil samples is readily achieved due to coexisting transition metal ions which facilitate the PVG reaction. The method detection limit of 0.005 ng g(-1) (3σ) using external calibration is comparable to that obtained using hydride generation (HG) ICPMS. However, PVG methodology is simpler, results in lower blanks, and avoids unstable reagents. The accuracy of the proposed method was demonstrated by analysis of several environmental certified reference materials (CRMs; SLRS-5 and SRM1640a river water CRMs and MESS-3, MESS-4, and SRM2702 sediments) with satisfying results. High precision of determination (<0.4% RSD) of Pb in river water and sediments was realized on the basis of isotope dilution calibration.
本文介绍了一种新颖且灵敏的方法,用于准确精确地测定环境样品中的铅。该方法采用过渡金属离子辅助光化学蒸气发生(PVG)进行样品引入,并结合多接收电感耦合等离子体质谱(MC-ICPMS)检测。在5%(v/v)甲酸溶液中,过渡金属离子(Co(2+)和Ni(2+))的存在显著提高了铅的PVG效率。由于共存的过渡金属离子促进了PVG反应,沉积物或土壤样品消解液中铅的测定很容易实现。使用外标法时,该方法的检出限为0.005 ng g(-1)(3σ),与氢化物发生(HG)ICPMS法相当。然而,PVG方法更简单,空白值更低,且避免了使用不稳定的试剂。通过分析几种环境标准物质(CRM;SLRS-5和SRM1640a河水CRM以及MESS-3、MESS-4和SRM2702沉积物)证明了该方法的准确性,结果令人满意。基于同位素稀释校准,实现了河水和沉积物中铅的高精度测定(<0.4% RSD)。