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The protolytic equilibria of bromazepam, an ampholyte sparingly soluble in water, in homogeneous and heterogeneous systems were studied in the pH range 014 at 25 ?C and at ionic strength of 0.1 mol/dm3 (NaCl). On the basis of 13C-NMR spectra, the protonation site was predicted in acidic media the pyridine nitrogen of bormazepam is protonated. The acidity constants of bromazepam were determined spectrophotometrically (pKa1 2.83 and pKa2 11.60) and potentiometrically (pKa1 2.99). In the heterogeneous system the following equilibrium constants were determined: Ks0 = [HA] (pKs0 3.44), Ks1 = [H2A+]/[H3O+] (pKs1 0.61), and Ks2 = [A-][H3O+] (pKs2 15.04).