Quantitative measurement method for trace/ultra-trace impurities in high-purity rare earth oxides

Abstract

The invention provides a method for measuring trace / ultra-trace impurities in high-purity rare earth oxides. Including: preparation of conductive auxiliary device; placing the high-purity copper cylinder loaded with rare earth oxide samples in GDMS for detection and sputtering; preparation of copper-based calibration samples by powder doping method; GDMS for the prepared copper-based calibration samples Perform analysis to obtain the relative sensitivity factor RSF, and calculate the impurity content in the rare earth oxide sample according to the formula (2) according to the relative sensitivity factor and the data detected by GDMS. GDMS is a direct measurement method for solids, so compared with the current commonly used wet method, it avoids the complicated sample processing process, greatly improves the analysis efficiency, and can avoid element loss and pollution during the digestion process; it can detect 73 elements at the same time, and The detection limit is low. For most elements, the quantitative detection limit (LoQ) is at the ng / g level, which meets the accurate measurement of trace / ultra-trace impurities.

Description

Technical field [0001] The present invention belongs to the field of elemental analysis, and more particularly to a quantitative measurement method of trace / ultra-trace impurities in high purity rare earth oxides. Background technique [0002] With the development of rare earth oxide new functional materials and its application in high-tech fields, the content of impurities in rare earth oxides is increasingly concerned. For high purity rare earth oxides, the impurity content is low, substantially in trace (1 to 100 μg / g) and ultra-trace level (<1 μg / g), which is very difficult to accurately measure. The national standard measurement method of impurities in the existing rare earth oxide is divided into two series: GB / T12690 "Rare Earth Metal and Non-Rare Earth Impurity Chemical Analysis Method", GB / T18115 "Rare Earth Metal and Rare Earth Impurity Chemistry in Oxides Analytical method". [0003] GB / T12690 is divided into 18 parts: For Al, Cr, Mn, Fe, Co, Ni, Cu, Zn,...

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Problems solved by technology

[0007] In order to overcome the problem in the prior art that it is difficult to use the GDMS method to accurately measure impurity elements in rare earth oxides, the present invention provides a conductive auxiliary device to realize the direct measurement of impurities in rare earth oxides by GDMS, and at the same time by preparing calibration samples , to realize the accurate and quantitative analysis of the content of impurity elements in rare earth oxides by GDMS method

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