Three dimensional subsurface elemental identification of minerals using confocal micro-X-ray fluorescence and micro-X-ray computed tomography

•Coupling of confocal X-ray fluorescence spectroscopy and X-ray computed tomography•Qualitative elemental identification of surface and subsurface mineral particles•Non-destructive particle size measurements•Utilization of laboratory-based X-ray instrumentation

Current non-destructive elemental characterization methods, such as scanning electron microscopy-based energy dispersive spectroscopy (SEM–EDS) and micro-X-ray fluorescence spectroscopy (MXRF), are limited to either elemental identification at the surface (SEM–EDS) or suffer from an inability to discriminate between surface or depth information (MXRF). Thus, a non-destructive elemental characterization of individual embedded particles beneath the surface is impossible with either of these techniques. This limitation can be overcome by using laboratory-based 3D confocal micro-X-ray fluorescence spectroscopy (confocal MXRF). This technique utilizes focusing optics on the X-ray source and detector which allows for spatial discrimination in all three dimensions. However, the voxel-by-voxel serial acquisition of a 3D elemental scan can be very time-intensive (~ 1 to 4 weeks) if it is necessary to locate individual embedded particles of interest. As an example, if each point takes a 5 s measurement time, a small volume of 50 × 50 × 50 pixels leads to an acquisition time of approximately 174 h, not including sample stage movement time. Initially screening the samples for particles of interest using micro-X-ray computed tomography (micro-CT) can significantly reduce the time required to spatially locate these particles. Once located, these individual particles can be elementally characterized with confocal MXRF. Herein, we report the elemental identification of high atomic number surface and subsurface particles embedded in a mineralogical matrix by coupling micro-CT and confocal MXRF. Synergistically, these two X-ray based techniques first rapidly locate and then elementally identify individual subsurface particles.