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Analysis of 14 Rare Earth Impurities in 99.99998% Ultra High Purity Rare Earth Cerium Oxide (Ce ₂ O3)
Date: 2025-12-31Read: 5
rare earthIt is one of the cornerstones of modern technology industry, and high-purity rare earth products directly affect the performance of the final product. From green energy to intelligent electronics, from cutting-edge weapons to medical equipment, this series of "industrial gold" is indispensable. Its preparation process is a manifestation of chemical separation technology and an important symbol of a country's strength in materials science and fine chemical industry. Currently, China is the world's largest producer and supplier of high-purity rare earths, with a complete industrial chain from mining to separation and purification.
►High-purity rare earthUsually refers to single rare earth oxides or metals with a purity higher than 99.9%, rather than mixed rare earths. Purity is its most critical indicator, as even trace impurities (other rare earth elements or non rare earth elements) can seriously affect its application performance in high-tech fields. With the continuous improvement of refining technology, the purity of rare earth oxides can reach 6N or 7N, which puts forward higher requirements for the determination of trace rare earth impurities.
►At present, the detection methods for impurity elements in high-purity rare earths are mainly based onInductively Coupled Plasma Optical Emission Spectroscopy (ICP-OES) and Inductively Coupled Plasma Mass Spectrometry (ICP-MS) in the national standard GB/T 18115.1-15For rare earth oxides with a purity of less than 99.99%, matrix matching method can be used for ICP-OES testing. For rare earth oxides above 99.99%, internal standard calibration method and ICP-MS testing are required.
►When using ICP-MS for high-purity rare earth detection, rare earth elements are prone to mass spectrometry interference from multi atomic ions such as oxides, hydrides, and hydroxides. Therefore, instruments with strong interference removal capabilities are required to remove mass spectrometry interference. Otherwise, C272 microcolumns are used for matrix separation to reduce mass spectrometry interference. In addition, due to the high sublimation temperature of rare earth elements, they are prone to accumulate on the water-cooled interface cone, causing blockage of the cone mouth and drifting of the instrument signal. Therefore, the instrument needs to have a larger cone mouth aperture to facilitate long-term analysis of such samples.
PerkinElmer Corporation'sNexION 5000G Multi quadrupole ICP-MSEquipped with a new second-generation three cone (industry's largest aperture) interface technology using OmniRing technology and a plasma RF generator with LumiCoil RF coils, it can stably analyze high-purity rare earth and other high matrix samples for a long time. More importantly, in the removal of mass spectrometry interference, the front quadrupole (Q0) of NexION 5000G uses mass spectrometry scanning technology synchronized with the main quadrupole to remove matrix ions, allowing target ions to enter Q1 for screening to the maximum extent possible and reducing space charge effects. Single mass (resolution<0.3 amu) ions filtered by the first stage mass analyzer (Q1) enter the axial accelerated quadrupole collision reaction cell (Q2) for interference ion removal or target ion mass transfer.
PerkinElmer NexION 5000G ICP-MS
NexION 5000GThe quadrupole collision reaction poolIt is a specialized universal tank used to control chemical reactions within the reaction tank. This is achieved by using dynamic bandwidth tuning within the reaction pool. Dynamic bandwidth tuning can prevent by-products of the reaction from forming new interferences in the reaction gas or impurities that may have been introduced into the reaction pool. A mixture of 100% pure reaction gas or highly reactive gas can be used in the reaction tank, and the bandwidth of the reaction tank can easily remove predictable and reproducible interference. After passing through the universal pool, the target ion enters the second stage mass analyzer (Q3) to screen out interference and perform final mass screening of the target ion, which then enters the detector for detection.
Practical Exercise: Determination of 14 Rare Earth Impurities in 99.99998% High Purity Rare Earth Cerium Oxide (Ce2O3)
At present, the detection methods for rare earth impurities in cerium oxide are mainly based on GB/T 18115.2-2020Inductively Coupled Plasma Spectroscopy and Inductively Coupled Plasma Mass Spectrometry.
InUsing ICP-OESDue to the sensitivity and resolution of the spectrometer, the detection range of impurity rare earths is limited to 0.001% -0.1% during testing, which cannot meet the detection requirements of high-purity rare earths.
InUsing ICP-MSDuring analysis, Ce+combines with O+and H+to form multi atomic ions, which affects the detection of La, Pr, Gd, Tb, and Lu. Especially when analyzing Gd and Tb, it is necessary to separate the Ce matrix through C272 microcolumns for analysis and testing.
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Mass spectrometry interference in Ce matrix
NexION 5000G Multi quadrupole ICP-MSWithout using any matrix separation methods, it is possible toEasy removal of mass spectrometry interference generated in Ce matrixProvide strong support for the detection of high-purity rare earths. In the detection of high-purity Ce, NexION 5000G introduces highly active reaction gases high-purity ammonia and high-purity oxygen into a universal cell to form special mass ion clusters of target ions, avoiding the interference of multi atomic ions formed by the Ce matrix. By controlling the axial acceleration electric field and RPq in the collision reaction cell, the direction of reactant generation is accurately controlled, and the production of by-products is avoided.
Schematic diagram of Pr detection and CeH interference removal in Ce matrix
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Schematic diagram of Tb detection and CeOH interference removal in Ce matrix
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After interference removal, the detection results of 14 impurity rare earths in high-purity rare earths were obtained.
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Conclusion
NexION 5000G Multi quadrupole ICP-MSFeaturing multiple sets of quadrupole designsWithout the need for complex rare earth matrix separation techniques, high-purity rare earth samples can be accurately analyzed for a long time. By introducing pure high activity reaction gas into the quadrupole collision reaction cell, mass spectrometry interference is reduced to a very low level. In this paper, ammonia gas is introduced into the quadrupole collision reaction cell to remove the interference of CeO, CeOH on Tb and Gd, and oxygen is introduced into the quadrupole collision reaction cell to remove the interference of CeH and CeO2H on La, Pr, and Lu, in order to meet the detection requirements of high-purity Ce.