Integrated Three-Dimensional Microanalysis Combining X‑Ray Microtomography and X‑Ray Fluorescence Methodologies

• Published in: Analytical chemistry (Washington) 2017-10, Vol.89 (19), p.10617-10624
• Main Authors: Laforce, Brecht, Masschaele, Bert, Boone, Matthieu N, Schaubroeck, David, Dierick, Manuel, Vekemans, Bart, Walgraeve, Christophe, Janssen, Colin, Cnudde, Veerle, Van Hoorebeke, Luc, Vincze, Laszlo
• Format: Article
• Language: English
• Subjects: Analysis; Case studies; Chemical elements; Chemistry; Computed tomography; Fluorescence; Integration; Morphology; Perlite; Spatial distribution; Tomography; X ray fluorescence analysis; X ray microtomography; X-ray fluorescence
• ISSN: 0003-2700; 1520-6882
• DOI: 10.1021/acs.analchem.7b03205

A novel 3D elemental and morphological analysis approach is presented combining X-ray computed tomography (μCT), X-ray fluorescence (XRF) tomography, and confocal XRF analysis in a single laboratory instrument (Herakles). Each end station of Herakles (μCT, XRF-CT, and confocal XRF) represents the state-of-the-art of currently available laboratory techniques. The integration of these techniques enables linking the (quantitative) spatial distribution of chemical elements within the investigated materials to their three-dimensional (3D) internal morphology/structure down to 1–10 μm resolution level, which has not been achieved so-far using laboratory X-ray techniques. The concept of Herakles relies strongly on its high precision (around 100 nm) air-bearing motor system that connects the different end-stations, allowing combined measurements based on the above X-ray techniques while retaining the coordinate system. In-house developed control and analysis software further ensures a smooth integration of the techniques. Case studies on a Cu test pattern, a Daphnia magna model organism and a perlite biocatalyst support material demonstrate the attainable resolution, elemental sensitivity of the instrument, and the strength of combining these three complementary methodologies.