液体阴极辉光放电原子发射光谱法分析硅酸钇镥中痕量杂质元素  

Determination of Trace Metals in Lutetium-Yttrium Orthosilicate by Solution-Cathode Glow Discharge-Atomic Emission Spectrometry

作　　者：盖荣银 汪正[2] 贺岩峰[1] 李青[2] 邹慧君[2] 张国霞[2,3] 

机构地区：[1]长春工业大学化学工程学院,长春130012 [2]中国科学院上海硅酸盐研究所,上海200050 [3]华东理工大学,上海200237

出　　处：《分析化学》2014年第11期1617-1622,共6页Chinese Journal of Analytical Chemistry

基　　金：上海科委项目(No.12142200200);中国科学院上海硅酸盐研究所创新项目(No.Y37ZC4140G)资助

摘　　要：采用液体阴极辉光放电原子发射光谱(Solution-cathode glow discharge-atomic emission spectrometry,SCGD-AES)法测定了硅酸钇镥(Lutetium-Yttrium Orthosilicate,LYSO)闪烁晶体材料中痕量元素Ca,Fe,K,Li,Mg和Na。最佳实验条件是溶液pH为1的HNO3,直流电压为1080 V,溶液流速为2.0 mL/min。本方法对LYSO基体的耐盐量为10 g/L。硅酸钇镥晶体使用HNO3,HF,HClO4溶解后经SCGD-AES分析测定,结果同电感耦合等离子体发射光谱(Inductively coupled plasma-atomic emission spectroscopy,ICP-AES)和电感耦合等离子体质谱(Inductively coupled plasma-mass spectroscopy,ICP-MS)分析结果比对,具有较好的一致性。在运用SCGD-AES对LYSO的测定中,未观察到Lu、Y元素的激发谱线,因此测定LYSO中痕量元素时测定的光谱干扰少,Ca,Fe,K,Li,Mg和Na的检出限分别为:1.0,3.0,0.02,0.01,0.02和1.0 mg/kg。The Lutetium-Yttrium Orthosilicate （LYSO） is a kind of scintillating crystal material with the best comprehensive properties. In this work, the trace elements Ca, Fe, K, Li, Mg and Na in LYSO were determined by solution-cathode glow discharge-atomic emission spectrometry （ SCGS-AES ） . The optimal conditions included 0. 1 mol/L HNO3 sample solutions and operation at a voltage at 1080 V with a flow rate of 2. 0 mL/min. The LYSO matrix concentration tolerance of the SCGD source was determined to be 10 g/L. Sample solutions dissolving from several LYSO samples with HF, HNO3 and HClO4 were examined by SCGD-AES. For LYSO samples, the values obtained by SCGD-AES agree well with those obtained by axial inductively coupled plasma-atomic emission spectroscopy （ ICP-AES ） and inductively coupled plasma-mass spectroscopy （ICP-MS）. The emissions of Lu and Y were not observed, so that the determination of trace elements in LYSO matrices could be conducted with little interference. The detection limits of Ca, Fe, K, Li, Mg and Na in LYSO were 1. 0, 3. 0, 0. 02, 0. 01, 0. 02 and 1. 0 mg/kg, respectively.

关 键 词：液体阴极辉光放电原子发射光谱 硅酸钇镥 痕量元素 

分 类 号：O657.31[理学—分析化学]