Figure 2.

One‐dimensional ¹H NMR spectrum of a sample removed from a titration experiment at pH 5.0 before nucleation. The peaks were assigned to the ibuprofen molecule, while the additional peaks correspond to ibuprofen in the separated dense liquid phase (labeled with *). The sample was drawn from the titration of S‐IbuNa solution (3 mm) with 15 mm HCl solution and 6 mm S‐IbuNa solution added at a rate of 0.2 mL min⁻¹ using the double‐dosing technique. The spectral range of 0.4–1.9 ppm (grey area) was used for two‐dimensional ¹H‐¹H NOESY NMR spectroscopy (Figure 5).