激光剥蚀-电感耦合等离子体质谱法测定高纯金属镱中锂镁  

Determination of lithium and magnesium in high purity ytterbium metal by laser ablation-inductively coupled plasma mass spectrometry

作　　者：刘春[1,2] 李志强 任旭东[1,2] 包香春 LIU Chun;LI Zhiqiang;REN Xudong;BAO Xiangchun(State Key Laboratory of Baiyunobo Rare Earth Resource Researches and Comprehensive Utilization,Baotou Research Institute of Rare Earths,Baotou 014030,China;Rui Ke National Engineering Research Centre of Rare Earth Metallurge and Function Materials Co.,Ltd.,Baotou 014030,China)

机构地区：[1]包头稀土研究院白云鄂博稀土资源研究与综合利用国家重点实验室,内蒙古包头014030 [2]瑞科稀土冶金及功能材料国家工程研究中心有限公司,内蒙古包头014030

出　　处：《冶金分析》2023年第4期41-47,共7页Metallurgical Analysis

摘　　要：锂、镁是真空蒸馏法生产高纯金属镱工艺的重要质控指标,是影响材料性能的关键杂质。实验通过优化激光剥蚀参数,建立了激光剥蚀-电感耦合等离子体质谱法(LA-ICP-MS)测定高纯金属镱中痕量锂和镁的方法。通过试验确定的激光剥蚀工作参数如下:能量密度为8 J/cm^(2),剥蚀孔径为160μm,扫描速率为25μm/s,载气流量为500 mL/min,脉冲频率为10 Hz。在优化的条件下,对高纯金属镱质控样品进行测定,根据参考值计算各元素的相对灵敏度因子(RSF)分别为0.32μg/g和0.21μg/g。11次载气空白检测确定锂和镁的方法检出限分别为0.020μg/g和0.014μg/g。将实验方法用于高纯金属镱样品中锂和镁的测定,结果的相对标准偏差(RSD,n=6)均小于5.0%。采用实验方法和电感耦合等离子体质谱法(ICP-MS)分别对高纯金属镱样品中的锂和镁进行定量分析,并对两种分析方法进行一致性检验。结果表明,锂、镁元素的t值均小于t0.05,10,说明LA-ICP-MS和ICP-MS两种方法结果一致性较好。Lithium and magnesium are important indexes for quality control of high purity ytterbium metal produced by vacuum distillation technology,and they are also the key impurities effecting the material performance.A method for the determination of lithium and magnesium in high purity ytterbium metal by laser ablation-inductively coupled plasma mass spectrometry(LA-ICP-MS)was established by optimizing the laser ablation parameters.The following working parameters for laser ablation parameters were obtained by experiment:the energy density was 8 J/cm2,the ablation spot size was 160μm,the scan rate was 25μm/s,the carrier gas flow rate was 500 mL/min,and the pulse frequency was 10 Hz.The quality control sample of high purity ytterbium metal was determined under the optimized experimental conditions,and the relative sensitivity factors(RSFs)of lithium and magnesium were 0.32 and 0.21μg/g,which calculated based on the reference values.The limit of detection of lithium and magnesium was 0.020μg/g and 0.014μg/g,which were indicated by 11 times of carrier gas blank experiments under the same conditions.The proposed method was applied for the determination of lithium and magnesium in high purity ytterbium metal sample,and the relative standard deviations(RSDs,n=6)of determination results were less than 5.0%.The contents of lithium and magnesium in high purity ytterbium metal sample were quantitatively analyzed according to the experimental method and inductively coupled plasma mass spectrometry(ICP-MS).The consistency test of two methods was also conducted.The results showed that the values of t for lithium and magnesium were lower than t0.05,10,indicating that LA-ICP-MS and ICP-MS methods had good consistency.

关 键 词：激光剥蚀-电感耦合等离子体质谱法(LA-ICP-MS) 高纯金属镱 相对灵敏度因子(RSF) 锂 镁 

分 类 号：O657.63[理学—分析化学] TF845[理学—化学]