Physical and chemical analysis of three-component system containing water, trichloroacetic and orthophosphoric acids has been discussed. The state diagram for the system has been drawn. The region of two-phase liquid equilibrium has been found in the system. Along with the field of two-phase liquid equilibrium the following fields have been detected: those of homogeneous solutions, three-phase monotectic equilibrium, two-phase equilibrium of trichloacetic acid crystals and solutions saturated with them, two-phase equilibrium of orthophosphoric acid crystals and solutions saturated with them. The composition of equilibrium liquid phases has been determined. The separation in the system is caused by the salting-out of an organic component from the water solution. The salting-out component is, in this case, orthophosphoric acid, namely hydronium ion.