电感耦合等离子体质谱法测定农产品土壤中痕量稀土元素  

Determination of Trace Rare Earth Elements in Agricultural Soils by Inductively Coupled Plasma- Mass Spectrometry

作　　者：倪能[1] 王玉功[1] 和振云[1] 祝建国[1] 

机构地区：[1]国土资源部兰州矿产资源监督检测中心,甘肃兰州730050

出　　处：《分析测试技术与仪器》2016年第1期42-47,共6页Analysis and Testing Technology and Instruments

基　　金：甘肃矿产资源勘查与综合利用工程技术研究项目资助(1306FTGA011)

摘　　要：建立了电感耦合等离子体质谱法（ICP-MS）测定农产品土壤中15个稀土元素的分析方法．研究了溶样体系用量、标准溶液配制、质谱干扰、内标元素的选择．采用HNO3-HF—H2O2体系电热板溶解样品，稀土元素的溶出率较高．用ICP—MS同时测定土壤中的钇、镧、铈、镨、钕、钐、铕、钆、铽、镝、钬、铒、铥、镱、镥．以Rh、Re双内标在线校正，有效地降低了信号漂移对分析结果的影响．方法检出限为0．0012—0．0071ng／mL．对实际样品进行连续7次测定，方法精密度为0．2％～4．7％，回收率为97％-114％．经国家标准物质验证，结果与标准值相符．方法弥补了微波消解法的不足，且快速、准确，适合于大批量土壤样品分析．In this paper, we reported a method to determine the concentrations of 15 rare earth elements（REEs） in agricultural soils using inductively coupled plasma- mass spectrometry （ICP- MS ）. The influence of experimental conditions, such as sample dissolution system, preparation for standard solution, interference in mass spectrum and choice of internal standard, was evaluated. The dissolution rate of rare earth elements was improved using a mixed HNO3-HF- H2 02 system to dissolve samples. 15 REEs in soil concluding yttrium, lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium and lutetium were determined by the said method. The online calibration of double internal standards of Rh and Re significantly reduced the effect of the signal drift on the analysis results. The detection limit of this method was 0. 001 2 -0. 007 1 ng/mL. The actual soil samples were determined for 7 times using the recommended method, the precision and the recovery rate of which were 0.2% -4.7% and 97% - 114% , respectively. The results were in good agreement with the standard value verified by National Standard Reference Materials. The method not only overcomes the deficiency of the microwave digestion method, but also can measure samples rapidly and accurately. Therefore, the method is suitable for the analysis of samples in batches.

关 键 词：电感耦合等离子体质谱法 土壤 稀土元素 

分 类 号：O657.32[理学—分析化学]