电感耦合等离子体质谱法测定铈及富铈烧结永磁体中镓  

Determination of gallium in cerium and cerium-rich sintered permanent magnet by inductively coupled plasma mass spectrometry

作　　者：包香春[1,2] 于勇海[1,2] 郝茜[1,2] 高立红[1,2] BAO Xiang-chun;YU Yong-hai;HAO Qian;GAO Li-hong(State Key Laboratory of Baiyunobo Rare Earth Resource Researches and Comprehensive Utilization, BaotouResearch Institute of Rare Earths, Baotou 014030, China;Ruike National Engineering Research Center ofRare Earth Metallurgy and Function Materials, 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,内蒙古包头014030

出　　处：《冶金分析》2020年第7期77-81,共5页Metallurgical Analysis

摘　　要：铈及富铈烧结永磁体中镓的含量可影响其磁性能,因此准确测定铈及富铈烧结永磁体中镓的含量对其应用意义重大。采用硝酸(1+1)-过氧化氢低温溶解样品,以2%(V/V)硝酸为测定介质,建立了电感耦合等离子体质谱法(ICP-MS)测定铈及富铈烧结永磁体中镓含量的分析方法。考虑到试样中主量元素铈和杂质元素镧的双电荷干扰,选择69Ga+作为测定同位素,并采用双电荷离子干扰校正公式进一步校正了138La2+(0.089%)和138Ce2+(0.25%)对69Ga+的质谱干扰;以10.00ng/mL的103Rh为内标校正了基体效应和仪器信号漂移。实验表明,镓质量浓度和镓与铑内标元素响应值的比值呈良好的线性关系,镓校准曲线的线性相关系数为0.99991。方法检出限为0.07ng/mL,定量限为0.23ng/mL。采用实验方法测定铈及富铈烧结永磁体中镓,其质量分数为0.0181%和0.0221%时,测得结果的相对标准偏差(RSD,n=11)分别为2.5%和2.1%,加标回收率为99%~104%。The content of gallium in cerium and cerium-rich sintered permanent magnet can affect their magnetic properties.Therefore,the accurate determination of gallium content in cerium and cerium-rich sintered permanent magnet has great significance for their applications.The sample was dissolved with nitric acid(1+1)-hydrogen peroxide at low temperature.A method for the determination of gallium in cerium and cerium-rich sintered permanent magnet by inductively coupled plasma mass spectrometry(ICP-MS)was established using 2%(V/V)nitric acid as the determining medium.In consideration of double charge interference by main element(cerium)and impurity element(lanthanum)in the sample,69Ga+was selected as the determination isotope.Meanwhile,the double charge ion interference correction formula was used to further correct the mass spectral interference of 138La2+(0.089%)and 138Ce2+(0.25%)with the determination of 69Ga+.The matrix effect and signal shift of instrument were effectively corrected using 10.00ng/mL 103Rh as the internal standard.Experiments showed that the mass concentration of gallium and the ratio of the response value of gallium to rhodium had a good linear relationship.The linear correlation coefficient of gallium calibration curve was 0.99991.The limit of detection was 0.07ng/mL,and the limit of quantification was 0.23ng/mL.The content of gallium in cerium and cerium-rich sintered permanent magnets was determined according to the experimental method.When the mass fraction was 0.0181%and 0.0221%,the relative standard deviation(RSD,n=11)was 2.5%and 2.1%,respectively.The spiked recoveries were between 99%and 104%.

关 键 词：电感耦合等离子体质谱法(ICP-MS) 铈及富铈烧结永磁体 镓 

分 类 号：O657.63[理学—分析化学]