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Summary Diverse methodologies are available for the characterization of cellulose nanocrystals (CNCs), but care must be taken in their application. The main techniques used for structural characterization include electron microscopy, scanning probe microscopy (AFM), scattering techniques such as dynamic light scattering (DLS), multi-angle light scattering (MALLS), small angle neutron scattering (SANS), and small angle X-ray scattering (SAXS), powder diffraction and solid-state NMR. Techniques common in solution chemistry such as NMR, mass spectrometry, and single crystal diffraction are not widely applicable here due to the insolubility of the products and the size of the crystals involved. Chemical characterization of CNCs is predominantly carried out using FTIR, elemental analysis, and X-ray photoelectron spectroscopy. Electron microscopy uses accelerated electrons as a source of illumination and either the scattered and emitted or transmitted electrons can be used to analyze the morphology of CNCs.