Analytical requirements for quantitative X-ray fluorescence nano-imaging of metal traces in solid samples

Quantitative nano-imaging of metal traces in a solid is a recent capability arising from the construction of hard X-ray nanoprobes dedicated to X-ray Fluorescence (XRF) imaging on upgraded third generation synchrotrons. Micrometer sample preparation valid for trace analysis is a fundamental part of the required developments to capitalize on the reduced Minimum Detection Limits. Practical guidelines lead us to propose a customized use of Focused Ion Beams (FIB) backed by state of the art Monte Carlo XRF modeling to initiate preparations of new samples and certified standards. The usefulness of these developments is illustrated by the first detection of Ni traces (4.57E+07 ± 3.2E+06 (7.1%) at μm⁻³) in a 3.35 Ga old microstructure of putative microbial origin from Barberton (South Africa). A list of feasibility checks provides a way of getting below 5 ppm MDLs for acquisition-times of 10 s with an analytical precision better than 10%.