Methods are disclosed utilizing synchrotron X-ray microscopy including x-ray fluorescence and x-ray absorption spectra to probe elemental distribution and elemental speciation within a material, and particularly a solid that may have one or more elements distributed on a solid substrate. Representative materials are relatively homogeneous in composition on the macroscale but relatively heterogeneous on the microscale. The analysis of such materials, particularly on a macroscale at which their heterogeneous nature can be observed, provides valuable insights into the relationships or correlations between localized concentrations of elements and/or their species, and concentrations of other components of the materials. Sample preparation methods, involving the use of a reinforcing agent, which are advantageously used in such methods are also disclosed.