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Molecular gels represent a case of hierarchical self-assembly of low molecular weight compounds into well ordered fibrillar architectures through non-covalent interactions. The resulting nanomaterials have found applications in multiple fields. In order to facilitate these applications, detailed study of their self-assembly mechanisms and properties at different length scales is required. The hierarchical nature of these materials means that a wide and multidisciplinary set of techniques have been developed and applied for the fundamental study of molecular gels. Different techniques are optimal for characterising aspects of the gel on each length scale – molecular, nano, microscopic and macroscopic. The present chapter uses selected examples to describe the different techniques that have been applied so far for a complete characterization of these systems. In particular, we focus on spectroscopy for probing molecular assembly, microscopy & diffraction/scattering to probe the nanoscale structuring, and calorimetric & rheological studies to provide insight into macroscopic performance. This chapter also focuses on aspects of gel characterisation such as chirality, kinetics and solvent effects.

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