Crystallization has attracted more and more attention from scientists and engineers in the field of pharmaceutics and foods. In order to understand crystals, many instrumental analytical techniques have been developed and applied in this field. In this work, recent application progress of instrumental analytical techniques for the characterization of crystal forms in pharmaceutics and foods has been reviewed and discussed. These techniques include X-ray diffraction, thermal analytical techniques, molecular vibrational spectroscopy, microscopy observation techniques, solid-state nuclear magnetic resonance spectroscopy, nuclear quadrupole resonance spectroscopy, etc. This work will provide a comprehensive guide to scientists and engineers in this field to characterize crystals in pharmaceutics and foods.