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Rapid Determination of Technetium-99 in Large Volume Seawater Samples Using Sequential Injection Extraction Chromatographic Separation and ICP-MS Measurement

机译:顺序进样萃取色谱分离和ICP-MS快速测定大量海水样品中的of 99

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摘要

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 X 10~(6) for ruthenium and 5 X 10~(5) for molybdenum are achieved. Chemical yields of technetium in the overall procedure range from 60percent to 75percent 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.
机译:开发了一种自动方法,用于快速测定大量海水样品中的〜(99)Tc。分析程序包括involves与共沉淀的预浓缩,使用萃取色谱法(两个TEVA柱)的在线分离(在连续进样设置中实施)以及通过电感耦合等离子体质谱法(ICP-MS)测量〜(99)Tc。研究了,、钼和钌的色谱行为,探讨了使用HNO_(3)在TEVA柱上吸附和洗脱TcO_(4)〜(-)的机理。结果表明,加载或洗脱溶液中的NO_(3)〜(-)不仅会影响酸度(或H〜(+)的浓度),还会影响TEVA在树脂上吸附和解吸TcO_(4)〜(-)。 。钌的去污因子大于1 X 10〜(6),钼的去污因子大于5 X 10〜(5)。整个过程中of的化学收率取决于样品量,从60%到75%不等,对于200 L的海水,检出限为7.5 mBq / m〜(3)(或11.5 pg / m〜(3))。 。与常规分析程序相比,该方法大大减少了分析时间。可以在24小时内分析一批样品(n> 4)。该方法已成功地用于快速,自动测定大量海水样品中的低水平〜(99)Tc。丹麦收集的海水样品的分析结果与使用常规方法获得的值显示出很好的一致性。

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