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

Abstract

The invention provides a measurement method for trace / ultra-trace impurities in high-purity rare-earth oxide. The measurement method comprises the following steps: preparing a conductive auxiliary device; placing a high-purity copper cylinder loading a rare-earth oxide sample in glow discharge mass spectrometer (GDMS) for detection and splashing; preparing a copper-base calibration sample by adopting a powder-doping method; analyzing the prepared copper-base calibration sample through the GDMS to obtain a relative sensitivity factor (RSF), and calculating the content of impurities in the rare-earth oxide sample according to a formula (2) based on the RSF and data obtained by GDMS detection. Compared with an existing common wet method, the GDMS adopts a solid direct measurement method, so that the complex sample treatment process is avoided, the analyzing efficiency is improved greatly, and element loss and pollution in the digestion process can be avoided. 73 elements can be detected simultaneously, the detection limit is low, the limit of quantization (LoQ) is at the ng / g magnitude specific to most elements, and accurate measurement of trace / ultra-trace impurities is met.

Description

technical field [0001] The invention belongs to the field of element analysis, and in particular relates to a quantitative measurement method for trace / ultra-trace impurities in high-purity rare earth oxides. Background technique [0002] With the development of new functional materials of rare earth oxides and their application in high-tech fields, more and more attention has been paid to the content of impurities in rare earth oxides. For high-purity rare earth oxides, the impurity content is low, basically at trace (1-100 μg / g) and ultra-trace levels (<1 μg / g), and it is very difficult to measure them accurately. The existing national standard measurement methods for impurities in rare earth oxides are divided into two series: GB / T12690 "Chemical Analysis Methods for Non-Rare Earth Impurities in Rare Earth Metals and Their Oxides", GB / T18115 "Chemical Analysis of Rare Earth Impurities in Rare Earth Metals and Their Oxides" Analytical method". [0003] GB / T12690 is di...

AI Technical Summary

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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