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Salt formation is often used to improve solubility of acidic drugs at low pH. When studying the dissolution of acidic active pharmaceutical ingredient (API) salt forms, results are often hard to interpret using a single technique due to their varying stability and eventual solid form conversion. Raman spectroscopy has been used in parallel with the Pion SDi2 to study the real-time surface dissolution of compacted diclofenac Na and monitor an associated solvent-mediated form transition.