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X-ray Powder Diffraction, Fourier Transform Infrared Spectroscopy and Differential Scanning Calorimeter were used to study the effect of the manual grinding in an agate mortar of the diclofenac acid polymorphs HD1 and HD2. In particular, we have tried to highlight how the HD2 form is more sensitive than the HD1 to the grinding process to achieve a nanometric crystal size. HD1 shows no change, while in the case of the HD2, changes in the molecular conformation and the formation of a new metastable form of the polymorph are observed after
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