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改进的氧瓶燃烧法结合电感耦合等离子体质谱快速测定茶叶样品中的稀土元素含量
引用本文:周舟,郭俊芳,段太成,黄楷伦,宁家贵.改进的氧瓶燃烧法结合电感耦合等离子体质谱快速测定茶叶样品中的稀土元素含量[J].分析化学,2016(9):1359-1364.
作者姓名:周舟  郭俊芳  段太成  黄楷伦  宁家贵
作者单位:1. 武汉工程大学材料科学与工程学院,武汉430000; 中国科学院长春应用化学研究所电分析化学国家重点实验室,长春130022;2. 武汉工程大学材料科学与工程学院,武汉,430000;3. 中国科学院长春应用化学研究所电分析化学国家重点实验室,长春,130022;4. 东北师范大学物理学院,长春,130022
基金项目:国家自然科学基金项目(21275138),吉林省科技创新中心(大型科学仪器装备提升)项目(No.20150623001TC)资助。
摘    要:建立了电感耦合等离子体质谱法快速测定茶叶中Y~Lu共15种稀土元素的新方法,样品处理基于改进的氧瓶燃烧法,以涂覆甘油的石英布代替滤纸作为引燃和燃烧载体,在500 mL容积燃烧瓶中实现了0.1 g样品量的有氧完全燃烧。系统优化了样品处理关键参数,以5 mL 4% HNO3+1% HF(V/V)组合试剂超声提取燃烧残渣1 min,稀土元素回收率大于90%,样品总处理周期小于3 min。6次样品平行测定值的相对标准偏差(RSD)在2.7%~5.5%之间,方法检出限(3σ)在0.001~0.006 mg/kg之间。采用本方法对3种茶叶标准参考物质进行分析,测定结果和标准值吻合良好。

关 键 词:氧瓶燃烧  电感耦合等离子体质谱  茶叶  稀土元素

Fast Determination of Rare Earth Elements in Tea Samples by ICP-MS with Modified Oxygen Flask Combustion
Abstract:A new method for accurate determination of 15 rare earth elements including Y-Lu in tea samples by inductively coupled plasma-mass spectrometry( ICP-MS) was proposed. Sample preparation was based on the modified oxygen flask combustion technique. By using quartz cloth coated with glycerol instead of filter paper as the ignition agent, a total amount of 0. 1 g sample could be completely burned in a 500-mL flask. Key factors affecting the sample preparation effect were systematically investigated, and it was found that the extraction efficiencies of over 90% for all the analytes could be realized with 5 mL of 4% HNO3+1% HF ( V/V) as the extractant for the combustion residue and the total extraction process could be finished in one minute under sonication, which resulted in a very fast sample preparation procedure that could be completed in less than 3 minutes. The relative standard deviations ( RSD) of six parallel determination values were between 2. 7% and 5. 5%, and the detection limits ranged from 0. 001 mg/kg to 0. 006 mg/kg. Three tea standard reference materials were analyzed with the method and the detection results agreed well with the standard values. The method was successfully applied to three real samples analysis.
Keywords:Oxygen flask combustion  Inductively coupled plasma-mass spectrometry  Tea samples  Rare earth element
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