电感耦合等离子体质谱测定高纯仲钨酸铵中磷及其它微量元素  

Determination of Trace Impurities in High Purity Ammonium Paratungstate by Inductively Coupled Plasma Mass Spectrometry

作　　者：荆淼[1,2] 陈利琴[2] 陈成祥[2] 陈登云[2] 王小如[1,2] 

机构地区：[1]中国海洋大学化学化工学院,青岛266003 [2]国家海洋局第一海洋研究所现代分析技术及中药标准化重点实验室,青岛266061

出　　处：《分析化学》2009年第3期403-406,共4页Chinese Journal of Analytical Chemistry

基　　金：山东省自然科学基金(No.20175022)资助项目

摘　　要：本研究采用带碰撞反应池的电感耦合等离子体质谱(ICP-ORS-MS)建立了快速、直接测定高纯仲钨酸铵样品中的磷及其它20种痕量元素杂质的方法。分别采用2种不同的样品制备方法,结果表明,使用4%H2O2进行消解操作简单、基体干扰小。通过高基体进样系统与电感耦合等离子体质谱联用,每个样品的固体总溶解度达到1%,连续测定样品2h,结果表明,能够克服高钨基体对ICP-MS信号稳定性的影响。方法检出限可达到ng/g,甚至亚μg/g,完全满足实际样品的分析,可实现仲钨酸铵生产现场的实时质量监测。A simple, robust and reliable method is described for the measurement of P and over 20 trace elements in high purity ammonium paratungstate （APT） using an ICP-（ ORS）-MS system. Two sample preparation methods were studied and compared and finally APT digestion in a heated 4% H2O2 solution was chosen. Each sample with 1% total dissolved solid was analyzed directly following the simple digestion of APT by ICP-MS with Ultra Robust optimization. Signal stability over 2-hour duration demonstrated the method robustness and excellent matrix tolerance of ICP-MS, negating the need of further sample dilution. This system offers very fast sample turnaround time compared to more conventional methods of sample preparation involving matrix removal. Instrument calibration was performed using the method of external standard calibration which was converted from standard addition calibration with internal standardization. The method detection limits ran- ging from ng/g to subμg/g were also sufficient accordance with APT industrial criteria. In general, these results show that the ICP-（ ORS）-MS methodology can be used for the routine measurement of trace metals in APT.

关 键 词：电感耦合等离子体质谱 钟钨酸氨 磷 痕量元素 

分 类 号：TG115.337[金属学及工艺—物理冶金]