Rapid and quantitative analysis of impurities in silicon powders by glow discharge mass spectrometry

Anal Bioanal Chem. 2018 Nov;410(27):7195-7201. doi: 10.1007/s00216-018-1324-z. Epub 2018 Sep 3.

Abstract

High-purity silicon power was doped with standard solutions containing 15 elements, and a high-purity indium tablet was prepared by the melting of indium pellets. An In-Si tablet, which is mechanically stable and thus suitable as a calibration sample, was prepared by our pressing the doped silicon power on the high-purity indium tablet. The matrix effect was studied by our investigating the variations of measured mass fractions (standard relative sensitivity factor, StdRSF, calibration) of doped impurities in the In-Si tablet, which provides a series of matrixes with different mass ratios of In to Si. For all the elements, the relative standard deviations of the measured mass fractions of impurities were less than 30%. The RSFs of the glow discharge mass spectrometer (Element GD) were obtained, and the results showed that three RSFs derived from the In-Si tablet with low, intermediate and high mass ratios of In to Si, respectively, agreed with the mean RSF within an uncertainty interval of 30%. The measurement of Fe and Al matrix certified reference materials further demonstrated that the RSFs generated from a matrix can be used for the calibration of another matrix, and the uncertainty was within 30%. Finally, another doped silicon powder was measured with the glow discharge mass spectrometer, which was calibrated by the mean RSFs from the In-Si tablet, and the analytical results obtained by glow discharge mass spectrometry are in good agreement with the analytical results obtained by high-resolution inductively coupled plasma mass spectrometry. Graphical abstract ᅟ.

Keywords: Glow discharge mass spectrometry; Impurities; Matrix effect; Quantitative analysis; Relative sensitivity factors; Silicon powders.