Department of Earth, Atmospheric, and Planetary Sciences, Massachusetts Institute of Technology, Cambridge, MA 02139, USA.
Anal Chim Acta. 2011 Feb 7;686(1-2):93-101. doi: 10.1016/j.aca.2010.11.052. Epub 2010 Dec 10.
A simple and accurate low-blank method has been developed for the analysis of total dissolved copper, cadmium, lead, and iron in a small volume (1.3-1.5 mL per element) of seawater. Pre-concentration and salt-separation of a stable isotope spiked sample are achieved by single batch extraction onto nitrilotriacetate (NTA)-type Superflow(®) chelating resin beads (100-2400 beads depending on the element). Metals are released into 0.1-0.5 M HNO(3), and trace metal isotope ratios are determined by ICPMS. The benefit of this method compared to our previous Mg(OH)(2) coprecipitation method is that the final matrix is very dilute so cone-clogging and matrix sensitivity suppression are minimal, while still retaining the high accuracy of the isotope dilution technique. Recovery efficiencies are sensitive to sample pH, number of resin beads added, and the length of time allowed for sample-resin binding and elution; these factors are optimized for each element to yield the highest recovery. The method has a low procedural blank and high sensitivity sufficient for the analysis of pM-nM open-ocean trace metal concentrations. Application of this method to samples from the Bermuda Atlantic Time-Series Study station provides oceanographically consistent Cu, Cd, Pb, and Fe profiles that are in good agreement with other reliable data for this site. In addition, the method can potentially be modified for the simultaneous analysis of multiple elements, which will be beneficial for the analysis of large number of samples.
已开发出一种简单、准确的低空白方法,用于分析小体积(每个元素 1.3-1.5 毫升)海水中的总溶解铜、镉、铅和铁。通过单次批量萃取到亚氨基三乙酸(NTA)型 Superflow(®)螯合树脂珠(根据元素而定,100-2400 个珠子),可实现稳定同位素加标样品的预浓缩和盐分离。金属被释放到 0.1-0.5 M HNO(3)中,并通过 ICPMS 测定痕量金属同位素比值。与我们之前的 Mg(OH)(2)共沉淀方法相比,该方法的优势在于最终基质非常稀释,因此锥体堵塞和基质灵敏度抑制最小,同时仍然保留同位素稀释技术的高精度。回收率对样品 pH、添加的树脂珠数量以及允许样品-树脂结合和洗脱的时间长度敏感;针对每个元素优化这些因素以获得最高的回收率。该方法具有低程序空白和足够高的灵敏度,足以分析 pM-nM 开阔海洋痕量金属浓度。将该方法应用于百慕大大西洋时间序列研究站的样品,提供了与该站点其他可靠数据一致的海洋学一致的 Cu、Cd、Pb 和 Fe 分布。此外,该方法可以潜在地修改为同时分析多个元素,这将有利于大量样品的分析。