Conventionally, elemental gradients are quantified using SEM-EDS line (i.e., 1D) scans across crosssections of particles, prepared by mechanical cross-sectioning. Running a 1D scan along a single plane can introduce bias and uncertainty, especially when the depth of probing of EDS is considered. Furthermore, statistical significance is low with such small data sets. Complementary qualitative information is often acquired with elemental (color) maps in 2D, but quantification demands long measurement times that are rarely pursued. Lastly, determination of the location of the measured crosssection within the original secondary particle demands additional particle size measurements. Ultimately, the homogeneity of elemental gradients in secondary particles cannot be confidently established without quantifying the entire 3D volume. FIB-SEM can be used for this purpose but still requires slow, mechanical techniques that may damage the internal morphology and induce redistribution of fragments that introduce uncertainty.