电感耦合等离子体质谱法测定高纯氟钽酸钾中15种痕量杂质元素

Determination of 15 Trace Impurity Elements in High Purity Potassium Fluotantalate by Inductively Coupled Plasma Mass Spectrometry

使用硝酸及氢氟酸混合酸低温加热溶解样品,采用耐氢氟酸进样系统,应用屏蔽矩冷等离子体技术消除^(24)CC+、^(52)ArC+、^(56)ArO+等多原子离子对Mg、Cr、Fe等元素的干扰,以标准加入法定量,从而建立了电感耦合等离子体质谱法测定高纯氟钽酸钾中15种痕量杂质元素的分析方法。方法中各元素的检出限(3 s)在0.003 9μg/g～0.089μg/g之间。采用所建立的方法测定高纯氟钽酸钾中的15种痕量杂质元素,测定值的相对标准偏差(RSD,n=11)在1.08%～13.5%之间,加标回收率在91%～109%之间,可满足高纯氟钽酸钾中15种痕量杂质元素的分析要求,分析结果与电感耦合等离子体原子发射光谱法(ICP-AES)对照,结果相符。

The sample is dissolved in the mixture of HF and HNO3 by heating at low temperature,and the hydrofluoric acid-resistant sampling system is adopted.The interferences of24 CC+、52 ArC+、56 ArO+and other polyatomic ions to24 Mg+、52Cr+、56Fe+and other elements are eliminated by shield torch cool plasma technology.Based on the standard addition method,the inductively coupled plasma mass is established to analyse the 15 trace impurity elements in high purity potassium fluotantalate quantitatively.The values of detection limits(3 s)for the 15 elements are in the range of 0.003 9μg/g^0.089μg/g.The proposed method is applied for the analysis of high purity potassium fluotantalate samples,and the relative standard deviations of measured values(RSD,n=11)are in the range of 1.08%~13.5%,and the spiked recoveries are in the range 91%~109%,which can meet the analysis requirement of 15 trace impurity elements in high purity potassium fluotantalate.The analysis results are consistent with the ICP-AES.