The control of formation and ordering of self assembled nanostructures, with medium- to long-range order, is a challenge that limits advances in many fields of nanotechnology. We have developed a technique, which we call fluctuation x-ray microscopy, that offers quantitative insight into medium-range correlations in disordered materials at nanometer- and larger-length scales. We examined the influence of sol-gel process variables on medium range order in PI-b-PEO/ aluminosilicate bulk using this technique. The nano-structuring of inorganic materials was directed by polymer self-assembly. The medium range correlation between the nanostructures in two hybrids was quantitatively examined and compared.