As part of the Avogadro constant re-determination, the molar mass of a highly-enriched 28Si crystal is being determined using various mass-spectrometry techniques. These calculations rely on the silicon material having high chemical purity, which has been initially assessed by infrared spectrometry. APT is uniquely suited to assess isotopic purity and distribution within a sample, thus ensuring the homogeneity required for precise measurements. In this study, Atom Probe Tomography (APT) is employed to further investigate isotopic composition and elemental purity within the mono-isotopically highly-enriched 28Si crystal (AVO28) and ultra-highly-enriched 28Si (UHP) and contrasted with natural silicon isotopes samples (WASO04, PSM, and SRM990). Reliable silicon isotope ratios are obtained from standard samples through a data processing procedure which utilizes automated mass ranging, background and deadtime corrections. The 29Si/28Si isotope ratios for WASO04, PSM and SRM990 agree with published values. AVO28 and UHP analysis reveals no impurities detected above 2 µg/g, with a uniform distribution of 28Si and 29Si at the nanometer scale. AVO28 exhibits 29Si content of 41 ± 2 µg/g, with no detection of 30Si below 2 µg/g, consistent with SIMS and other international comparisons. This work demonstrates APT’s capability for impurity detection and high-precision isotope analysis, reinforcing the silicon molar mass calculations and supporting Avogadro’s constant redefinition.
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