三重串联四极杆等离子体质谱法测定激光光纤用超高纯铈螯合物中痕量金属杂质离子  

Determination of Trace Metal Impurities in Ultra-high Pure Cerium Chelate Used for Laser Optical Fiber by ICP-MS/MS

作　　者：张衍[1,2] 潘忠奔 焦鹏冲[1,2] 居佳 何亭[1,2] 蔡华强 ZHANG Yan;PAN Zhong-ben;JIAO Peng-chong;JU Jia;HE Ting;CAI Hua-qiang(Institute of Chemical Materials,China Academy of Engineering Physics,Mianyang 621900,China;Sichuan Research Center of New Materials,Chengdu 610000,China)

机构地区：[1]中国工程物理研究院化工材料研究所,四川绵阳621900 [2]四川省新材料研究中心,四川成都610000

出　　处：《分析测试学报》2019年第3期307-311,317,共6页Journal of Instrumental Analysis

基　　金：国家自然科学基金资助项目(21702194);中国工程物理研究院化工材料研究所科技创新基金(KJCX-201502)

摘　　要：该文建立了三重串联四极杆电感耦合等离子体质谱法(ICP-MS/MS)测定激光光纤用超高纯铈螯合物中14种稀土及4种非稀土痕量金属杂质离子含量的新方法。采用低压密闭湿法消解,0.1 g样品以1 mL HNO_3处理30 min即可获得澄清溶液,实现了样品高效、清洁的前处理。在MS串接检测模式下,通过优化耐高盐进样系统(HMI)参数获得了低至0.3%的CeO^+/Ce^+产率,并进一步结合氧气及氨气反应池技术充分消除了基体Ce对超痕量La、Pr、Gd、Tb、Dy导致的典型强复合离子干扰和质谱拖尾,实现了2～3个数量级的干扰程度改善;基于冷等离子体技术并结合氢气及氦气碰撞反应池技术在高基体浓度下充分消除了Ar对超痕量Ca、Fe导致的同质异素及多原子离子干扰。在优化条件下,针对6N超高纯铈螯合物中所有杂质元素测定的长期稳定性RSD<5%(2 h,4.0 g/L),加标回收率为92.6%～108%,方法检出限为0.001 2～0.071 5μg/g,表明所建立的方法适用于6N超高纯铈螯合物样品的快速批量分析。A new method of inductively coupled plasma-triple quadruple mass spectrometry(ICP-MS/MS) was developed for the determination of 14 trace rare earth metal and 4 trace other metal impurities in cerium chelate with ultrahigh purity.0.1 g sample was digested by low-pressure autoclaves with 1 mL HNO3 for 30 min at 120 ℃.Under the MS/MS detection mode,typical strong poly-atomic and overlapping interferences on La,Pr,Gd,Tb and Dy from the matrix of Ce were fully eliminated(about 2-3 orders of improvement in comparison with conventional detection modes),when the O2 and NH3 based dynamic reaction cell(DRC) technique was used and a low ratio of 0.3% for CeO+/Ce+ was accomplished by using the high matrix introduction(HMI) sample introduction system;Similarly,isotopic and poly-atomic interferences on Ca and Fe from Ar under high matrix concentration levels were successfully eliminated by using the cool plasma detection mode plus the H2 and He based DRC technique.Under the optimized detection conditions,a RSD with long-term stability was less than 5%(2 h,4.0 g/L),the recoveries of 92.6%-108% and the detection limits(3s) of 0.001 2-0.071 5 μg/g for all of the analytes were obtained,indicating that the method could be applied in the rapid batch analysis of cerium chelate with 6 N purity.

关 键 词：三重串联四极杆电感耦合等离子体质谱(ICP-MS/MS) 高纯铈螯合物 激光光纤 痕量金属杂质离子 

分 类 号：O657.7[理学—分析化学]