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. Fluctuation x-ray microscopy offers quantitative insight into medium-range correlations in disordered materials at nanometer and larger length scales. Using this novel technique we examined the influence of sol-gel process variables on medium range order in PI-b-PEO/ aluminosilicate bulk films. Nano-structuring of the inorganic materials in these hybrids was directed by polymer self-assembly. We quantitatively examined and compared the medium range correlation between the nanostructures in two different hybrids.