Method for detecting ion content of fourteen trace impurity rare earth metals and ten trace impurity non-rare earth metals in ultra-high purity ytterbium compound

Abstract

The invention discloses a method for detecting the ion content of fourteen trace impurity rare earth metals and ten trace impurity non-rare earth metals in an ultra-high purity ytterbium compound. Themethod utilizes a triple quadrupole tandem inductively coupled plasma mass spectrometer to detect and comprises: 1, sample pretreatment, 2, working curve solution preparation, 3, working curve drawing, 4, measurement of the ion content of fourteen trace impurity rare earth metals and ten trace impurity non-rare earth metals in a sample solution, and 5, calculation. The method is easy to operate,has high test sensitivity, is free of mathematical formula correction data, solves the problem that the existing detection method easily causes severe mass spectrometry interference to the rare earthelement production through polyatomic ions formed by the ytterbium matrix and solves the problem that the existing detection method cannot carry out direct inductively coupled plasma mass spectrometrydetection on calcium and iron.

Description

technical field [0001] The invention relates to the technical field of trace element analysis and detection, in particular to a method for detecting the content of trace impurity metal ions in ultra-high-purity ytterbium (ytterbium content greater than 99.9999%, 6N) compounds. Background technique [0002] "High-purity rare earth" usually refers to rare earth metals and their compounds with a purity higher than 99.99%. High-power fiber lasers have higher requirements for the purity of doped rare earths, usually above 99.999% (5N). With the development of cutting-edge science and technology such as electronics, optics and optoelectronics, the demand for high-purity rare earth metal materials is increasing. In order to develop new properties of rare earth metals and their compounds, researchers have put forward higher purity requirements for raw materials, requiring The impurity content is ppm (μg / g) level or even lower, and the development of ultra-high-purity rare earth comp...

AI Technical Summary

Problems solved by technology

In fact, in the field of optical applications, non-rare earth impurity ions represented by transition metals seriously affect the optical performance of devices even at the ppb level, so the detection of non-rare earth metal impurities in high-purity rare earth metal compounds is also very important. However, due to the long-term limitation of the development of detection technology, there is currently no reliable method for all-element analysis of rare earth compounds with a purity greater than 5N in China.

[0004] At present, the analysis methods of trace rare earth metal impurities in high-purity ytterbium compounds mainly include chemical spectroscopy, inductively coupled plasma emission spectrometry (ICP-AES) and inductively coupled plasma mass spectrometry (ICP-MS), among which chemical spectroscopy There are disadvantages such as large sampling volume and long process; the ICP-AES method has complex spectral lines and low sensitivity and cannot meet the analysis requirements of high-purity ytterbium compounds with a purity of 99.999% (5N); the ICP-MS method has low detection limits and low sensitivity. It has been proved to be one of the most effective detection methods for trace rare earth elements due to its high and simple spectral lines. However, in the traditional ICP-MS determination process, due to the 168 Yb (0.13——isotopic abundance, the same below), 170 Yb(3.05), 171 Yb(14.3), 172 Yb(21.9), 173 Yb(16.12), 174 Yb(31.8), 176 As many as 7 isotopes such as Yb(12.7), among which 168 Yb and 170 Yb pair 169 Tm will produce mass spectrum peak superposition interference, 174 Yb and 176 Yb pair 175 Lu, 176 Lu produces mass spectrum peak stacking interference and isobaric stacking interference, especially 176 Yb pair 176 The interference of Lu is particularly serious, so it is usually necessary to separate the Yb matrix to effectively remove the above interference and make the test results relatively accurate. However, the method of separating the matrix is ​​cumbersome and the process is prone to pollution. At the same time, the traditional method after separation can only test the purity higher than 99.99% ( 4N) of the ytterbium compound purity, so the method cannot meet higher purity compound requirements

For the analysis of some non-rare earth metal impurities (such as V, Cr, Mn, Co, Ni, Cu, Zn, Mg, etc.) in high-purity ytterbium compounds, there is currently an inductively coupled plasma emission spectrometry (ICP-AES) And inductively coupled plasma mass spectrometry (ICP-MS), etc., the above methods can only test the purity of ytterbium compounds with a purity higher than 99.99% (4N)

For other non-rare earth metal impurities (calcium Ca, iron Fe), since their atomic weights (Ca is 40, Fe is 56) are the same as argon (Ar, 40) and argon oxygen atoms (ArO, 56) respectively, use inductively coupled plasma Mass spectrometry (ICP-MS) test will produce serious mass spectrum interference leading to test result errors, so usually these two elements are measured by inductively coupled plasma emission spectrometry (ICP-AES). On the one hand, the same compound requires multiple This test method leads to a cumbersome test process, and the test purity cannot meet the requirements of more than 99.99% (4N). Therefore, a new test method is developed that is suitable for impurities such as rare earth and non- An all-elemental analysis and detection method for the content of rare earth metal ions is very necessary

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