三重四级杆-电感耦合等离子体质谱法测定高纯三氧化二铈中14种稀土元素

Determination of 14 rare earth elements in high purity cerium oxide by triple quadrupole inductivity coupled plasma mass spectrometry

在高纯稀土分析中,通常利用C272微型柱分离或TODGA分离基体富集待测元素,但此方法效率低、操作难度大,容易引入外部杂质和洗脱不完全导致结果出现偏差。本文建立了三重四级杆电感耦合等离子体质谱(ICP-MS/MS)对高纯三氧化二铈(Ce_(2)O_(3))中杂质稀土元素测试方法,利用碰撞模式测定稀土氧化铈中的Y、La、Nd、Sm、Eu、Dy、Ho、Er、Tm、Yb、Lu,质量转移模式测定氧化铈中的Pr、Gd、Tb。测试采用0.1%基体进样,在MS/MS模式下,以笑气(N2O)为反应气,通过O原子和N原子的质量转移反应,可以有效克服高基体对待测元素带来质谱干扰,实现高纯Ce_(2)O_(3)中14种杂质稀土元素准确测定。试验结果表明,在优化试验条件下,14种元素的检出限为0.001~0.020 mg/kg,加标回收率在81.2%~105.3%之间。该方法仅使用N2O一种反应气,且无需基体分离,可以快速、准确测定高纯稀土氧化物中杂质元素,为高纯稀土杂质元素分析提供思路。

In the analysis of high purity rare earth element,C272 microcolumn separation or TODGA separation matrix is usually used to enrich the element to be measured,but this method is inefficiency and difficult to operate,and it is easy to introduce external impurities and incomplete elution,leading to deviations in results.In this paper,a test method for rare earth elements in high purity cerium trioxide(Ce_(2)O_(3))by inductively coupled plasma mass spectrometry(ICP-MS/MS)was established.The collision mode was used to determine Y、La、Nd、Sm、Eu、Dy、Ho、Er、Tm、Yb、Lu and the mass shift mode was used to determine Pr、Gd and Tb in the Ce_(2)O_(3).The test used 0.1%matrix injection in the MS/MS mode,and nitrous oxide(N2 O)was used as the reaction gas through mass shift reaction of O and N atoms.It can effectively overcome the mass spectrum interference caused by high matrix and achieve accurate determination of 14 impurity rare earth elements in high purity Ce_(2)O_(3).Under optimized experimental conditions,the detection limits of fourteen elements were in the range of 0.001~0.020 mg/kg,the recoveries were in the range of 81.2%-105.3%.The developed method can determine impurity elements in high purity rare earth oxides quickly and accurately,and provide a way for the analysis of impurities in high purity rare earth oxides.