Current approaches for assessing a confocal micro-X-rayfluorescence–probing volume involve the use of sharp knife edges, thin films, or wires, which are moved through this volume. The fluorescence radiation excited in the material of the object is measured, and profiles are built to enable the determination of the full width at half maximum in any of the three axes of the excited volume. Such approaches do not provide information on the shape of the volume, and the consequent alignment of both used lenses is made based on the position of the maxima of the registered intensity measurements. The use of particles that are smaller than the interaction volume (isolated enough to prevent the influence of nearby particles) and translated through the interaction volume (3D scan) is presented as an alternative methodology to determine the confocal probing volume. Spherical shaped uranium particles with diameter of 1–3 μm originally produced for scanning electron microscopy analysis calibration purposes were used in this study. The results obtained showed that the effectively probed confocal volume has a distinct prolate spheroidal shape that is longer in the axis of the confocal detector than it is wide on the axes of the plane perpendicular to it. The diameter in the longest axis (tilted accordingly to the angle between the two silicon drift detectors) was found to be approximately 25 μm, whereas the shorter was found about 15 μm each, with a volume of about 3,000 μm3.
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