Department of Oceanography, Florida State University, Tallahassee, FL 32306, USA.
Anal Chim Acta. 2010 Apr 30;665(2):200-7. doi: 10.1016/j.aca.2010.03.027. Epub 2010 Mar 23.
A novel method, combining isotope dilution with standard additions, was developed for the analysis of eight elements (Mn, Fe, Co, Ni, Cu, Zn, Cd and Pb) in seawater. The method requires just 12 mL of sample and employs an off-line pre-concentration step using the commercially available chelating resin Toyopearl AF-Chelate-650M prior to determination by high resolution inductively coupled plasma magnetic sector mass spectrometry (ICP-MS). Acidified samples were spiked with a multi-element standard of six isotopes ((57)Fe, (62)Ni, (65)Cu, (68)Zn, (111)Cd and (207)Pb) enriched over natural abundance. In addition, standard additions of a mixed Co and Mn standard were performed on sub-sets of the same sample. All samples were irradiated using a low power (119 mW cm(-2); 254 nm) UV system, to destroy organic ligands, before pre-concentration and extraction from the seawater matrix. Ammonium acetate was used to raise the pH of the 12 mL sub-samples (off-line) to pH 6.4+/-0.2 prior to loading onto the chelating resin. The extracted metals were eluted using 1.0 M Q-HNO(3) and determined using ICP-MS. The method was verified through the analysis of certified reference material (NASS-5) and the SAFe inter-comparison samples (S1 and D2), the results of which are in good agreement with the certified and reported consensus values. We also present vertical profiles of the eight metals taken from the Bermuda Atlantic Time Series (BATS) station collected during the GEOTRACES inter-comparison cruise in June 2008.
一种新方法,将同位素稀释与标准加入法相结合,用于分析海水中的八种元素(Mn、Fe、Co、Ni、Cu、Zn、Cd 和 Pb)。该方法仅需 12 mL 样品,并采用市售螯合树脂 Toyopearl AF-Chelate-650M 进行离线预浓缩步骤,然后通过高分辨率电感耦合等离子体质谱(ICP-MS)进行测定。酸化后的样品用含有六种同位素的多元素标准溶液((57)Fe、(62)Ni、(65)Cu、(68)Zn、(111)Cd 和 (207)Pb)进行同位素稀释,这些同位素的丰度高于天然丰度。此外,还对同一批样品的一部分进行了混合 Co 和 Mn 标准的标准加入。所有样品均在低功率(119 mW cm(-2);254 nm)UV 系统中辐照,以破坏有机配体,然后进行预浓缩并从海水基质中萃取。在将螯合树脂加载到 12 mL 亚样品(离线)中之前,使用乙酸铵将 pH 提高到 6.4+/-0.2。提取的金属使用 1.0 M Q-HNO(3)洗脱,并使用 ICP-MS 测定。该方法通过分析认证参考物质(NASS-5)和 SAFe 比对样品(S1 和 D2)进行了验证,结果与认证值和报告的共识值非常吻合。我们还展示了 2008 年 6 月在 GEOTRACES 比对航次中采集的来自百慕大大西洋时间序列(BATS)站的八种金属的垂直分布。