Rapid determination of technetium-99 in large volume seawater samples using sequential injection extraction chromatographic separation and ICP-MS measurement.
Rapid determination of technetium-99 in large volume seawater samples using sequential injection extraction chromatographic separation and ICP-MS measurement.
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DOI：
10.1021/ac301319a
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发表时间：
2012-07
影响因子：
7.4
通讯作者：
K. Shi;J. Qiao;Wang-suo Wu;P. Roos;X. Hou
中科院分区：
文献类型：
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作者：
K. Shi;J. Qiao;Wang-suo Wu;P. Roos;X. Hou
建立了一种快速测定大容量海水样品中~(99)Tc的自动化方法。分析程序包括用共沉淀法预富集锶，用顺序进样装置中的萃取色谱(两个Teva柱)在线分离，并用电感耦合等离子体质谱(ICP-MS)测量(99)Tc。研究了Te、Mo、Ru的层析行为，并探讨了TCO(4)(-)在Teva柱上用HNO(3)吸附和洗脱的机理。结果表明，Teva树脂对TCO(4)(-)的吸附和解吸不仅受NO(3)(-)的影响，而且还受负载或洗脱液的酸度(或H(+)浓度)的影响。Ru的去污系数大于1×10(6)，钼的去污系数大于5×10(5)。根据样品体积的不同，整个过程中氚的化学产率在60%-75%之间，对200个L海水的检出限为7.5MBq/m(3)(或11.5pg/m(3))。与常规分析方法相比，该方法大大缩短了分析时间。该方法可在24 h内完成一批样品(n>；4)的分析，并已成功地用于大容量海水样品中低水平~(99)Tc的快速自动测定。在丹麦采集的海水样品的分析结果表明，与用常规方法获得的值很好地吻合。
An automated method was developed for rapid determination of (99)Tc in large volume seawater samples. The analytical procedure involves preconcentration of technetium with coprecipitation, online separation using extraction chromatography (two TEVA columns) implemented in a sequential injection setup, and measurement of (99)Tc by inductively coupled plasma mass spectrometry (ICP-MS). Chromatographic behaviors of technetium, molybdenum, and ruthenium were investigated, and the mechanism of adsorption and elution of TcO(4)(-) on a TEVA column using HNO(3) was explored. The results show that not only NO(3)(-) but also acidity (or concentration of H(+)) of the loading or eluting solution affect the adsorption and desorption of TcO(4)(-) on TEVA resin. Decontamination factors of more than 1 × 10(6) for ruthenium and 5 × 10(5) for molybdenum are achieved. Chemical yields of technetium in the overall procedure range from 60% to 75% depending on the sample volumes, and a detection limit of 7.5 mBq/m(3) (or 11.5 pg/m(3)) for 200 L of seawater was obtained. Compared with the conventional analytical procedure, the developed method significantly reduces analytical time. A batch of samples (n > 4) can be analyzed within 24 h. The method has been successfully applied for rapid and automated determination of low level (99)Tc in large volume seawater samples. The analytical results of seawater samples collected in Denmark show a good agreement with the values obtained using the conventional method.