Development and validation of a new method for the precise and accurate determination of trace elements in silicon by ICP-OES in high silicon matrices

A new method for the accurate and precise determination of impurities in silicon was developed and statistically validated. Particular attention was paid to the correct determination of the non-metals boron and phosphorus. Instead a time-consuming open vessel digestion under mild conditions, the dissolution of silicon took place in a microwave-assisted high-pressure system. The essential innovation of the presented method is the direct use of the concentrated digestion solution for ICP-OES measurements. This approach avoids the commonly used, time-consuming method that requires the removal of silicon and acid matrix by volatilisation, which is the most critical step in the determination of boron; however, the ICP-OES measurement in such high silicon matrices requires an entirely new optimisation of the measuring conditions, including the careful selection of emission lines with respect to selectivity and, spectral and non-spectral inferences. For quantification of the impurities contents, the methods of matrix matching (MMC) and multiple standard addition (MSA) were used. After optimisation of the spike concentrations for MSA, the qualities of both methods were compared through a statistical analysis. For the metallic impurities Al, Mg, Ca, Ti, Cr, Mn, Fe, Ni, Cu, and Zr and P, the validation was performed against certified reference materials (IPT134, IPT135, NIST57b). To validate boron, 9 silicon samples with different contents of boron from three interlaboratory comparisons were used. The new procedure allows for the determination of the impurities of 4N-silicon (12 elements).