The hydrolysis processes in the system Fe{3+} – Cu {2+} – NO[3]{–} – H[2]O have been investigated by potentiometric titration and dialysis methods. The experiment data have been obtained under the following conditions: metal ions concentration – 0,01 mol/l, molar ratio Fe{3+}:Cu{2+} = 1 : 1, ionic strength – 0.3 mol/l (NaNO[3]), temperature – (25 ±0.1)°С, pH-range – 1.5–2.4. The distribution of different Fe (III) and Cu (II) forms upon pH value has been calculated upon experimental data. It has been established that Fe (III) and Cu (II) form heteropolynuclear hydroxocomplexes.