3 D visualizations of the microstructure of flocculated particulates and sediments using optical confocal laser microscopy and high resolution X-ray microtomography methods are described. Data obtained from in situ measurements should enable direct computation of the properties of solids assembly (shape, size, contact area) and their permeability to fluids. A specific application relating to the formation of silica aggregates is described from which the behaviour of sediments containing these materials can be predicted on the basis of a bench-top test and the use of a Lattice Boltzmann simulation. It is proposed that the method can potentially be used to predict trends such as the filtration behaviour of porous structures under different states of compression. This offers a significant benefit in assisting the formulation design of flocculated materials pertinent to a number of industrial sectors wishing to design optimal filtration or relevant operations.