We report the results of studies of the phase separation of solid solutions of dilute concentrations of 3 He in 4 He. The temperatures and the kinetics of the phase separation were determined from NMR experiments for 3 He concentrations 1.6 × 10 −5 < x 3 < 2.0 × 10 −3 . The experimentally observed phase separation temperatures are found to be in excellent agreement with regular solution theory as augmented by Edwards and Balibar [Phys.Rev. B39,4083(1989)]. The growth of 3 He droplets shows a t