Phase equilibria and critical phenomena in the water-i-butyric acid binary system were studied by the visual polythermal method over the temperature range –10–30°C. The system is characterized by delamination with an upper critical solution temperature (UCST) equal 25.8°C. In the system at –1.8°C, these occurs a nonvariant monotectic equilibrium whose solid phase are ice crystals. The phase diagram of the system is plotted.