电感耦合等离子体质谱法直接测定有机相中痕量锆

Determination of Trace Zirconium in Organic Phase by ICP-MS

  • 摘要: 采用配备有机进样器的电感耦合等离子体质谱(ICP-MS)建立了快速、直接测定有机相(选取30%磷酸三丁酯/煤油作为研究体系)中痕量锆的方法。选择适宜的表面活性剂以增强有机相在水相中的溶解度,对ICP-MS在有机进样条件下的工作参数进行了优化和选择,并以锶和铟作为内标消除干扰。研究表明,表面活性剂的加入可使有机相与水相互溶,该方法的检出限为0.017 ng/g(3 S,n=11),样品加标回收率在97.0%~102.5% 之间,方法精密度均小于3.0%。该方法能满足实际样品的分析需求,可实现PUREX流程有机相中痕量锆的直接测定。

     

    Abstract: A simple, reliable and feasible method was built for determining of trace Zirconium in organic phase by inductively coupled plasma mass spectrometry(ICP-MS) equipped with an sampler for organic phase. The surfactant of Triton X-100 was used to improve the organic phase solubility in aqueous solution, and the instrumental operating parameters and experimental conditions were optimized with the standard solution of organic-aqueous phase mixture.The effect of matrix on determination of Zirconium was discussed in detail by ICP-MS. The internal standard element of Sr or In was employed to eliminate the signal suppression effect induced by matrix and instrument signal drift. The results suggest that the addition of surfactant can make the organic phase to dissolve in aqueous phase. The detection limits (3S, n=11) of the method are no greater than 0.017 ng/g. Satisfied recoveries varied from 97.0% to 102.5% are achieved. The relative standard derivations (RSDs) are less than 3.0%. In short, the method is very promising in determination of trace Zirconium in organic phase.

     

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