Citation: CHEN Wen, FAN Xiao-Wei, GUO Cai-Nv, SONG Xu-Dong, LIU Yi-Qiang, XU Na. Determination of Iron Content in High Purity Rare Earth by Inductively Coupled Plasma-Tandem Mass Spectrometry[J]. Chinese Journal of Analytical Chemistry, ;2019, 47(3): 403-409. doi: 10.19756/j.issn.0253-3820.181724 shu

Determination of Iron Content in High Purity Rare Earth by Inductively Coupled Plasma-Tandem Mass Spectrometry

CHEN Wen ^1, ,
FAN Xiao-Wei ^1,2 ,
GUO Cai-Nv ³ ,
SONG Xu-Dong ¹ ,
LIU Yi-Qiang ¹ ,
XU Na ¹

1.
National Tungsten & Rare-earth Product Quality Supervision Testing Center, Ganzhou 341000, China;
2.
Faculty of Materials Science and Engineering, Jiangxi University of Science and Technique, Ganzhou 341000, China;
3.
Jiangxi South Rare Earth Hi-Tech Co., Ltd, Ganzhou 341000, China

Received Date: 20 November 2018
Revised Date: 16 December 2018

Fund Project: This work was supported by the National Natural Science Foundation of China (No. 21471070).

Because inductively coupled plasma mass spectrometry(ICP-MS) could not be used for determination of trace Fe in high purity rare earths, an inductively coupled plasma-tandem mass spectrometry (ICP-MS/MS) method was proposed. The mass spectral technique based on the oxygen reaction cell was used to optimize the instrument parameters, the flow rate of O₂ was adjusted to 2.0 mL/min, and the matrix injection concentration was determined to be 3.00 g/L, as well as the internal standard In was used for the calibration. Then, the isotope ⁵⁶Fe⁺ ion with abundance of 91.68% was selected as the analysis target. With Q₁=56/Q₂=72, the collision reaction of O₂ with ⁵⁶Fe⁺ was carried out to generate the target product of ⁵⁶Fe¹⁶O⁺, which performed effectively to eliminate the mass spectrum interference of polyatomic ion of ⁴⁰Ar¹⁶O⁺, ⁴⁰Ca¹⁶O⁺ and ³⁷Cl¹⁸OH⁺. So that it could accurately determine the trace impurities of Fe content in 15 kinds of high purity rare earth oxide and 4 kinds of high purity rare earth metals of cerium, neodymium, yttrium, and praseodymium-neodymium. According to the selected analysis conditions, the linear correlation coefficient of the calibration curve was greater than 0.9999, the detection limit was 68 μg/g, the relative standard deviations (RSD, n=11) were 2.1%-4.3%, and the recoveries were 95%-105%. This method is simple and environmentally friendly, and suitable for the rapid determination of trace of Fe in high purity rare earth metals and their oxides.
- Inductively coupled plasma-tandem mass spectrometry,
- High purity rare earths,
- Iron,
- Polyatomic ion interference
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