Kinetics of phase separation of poly(p-phenylenebenzobisoxazole) (PBO) in methanesulfonic acid are examined by the time-resolved small angle light scattering and turbidity measurements. Thin films of polymer solutions are spin-coated on microscope slides and observed in a controlled environment light scattering cell. These solutions appear to undergo a spinodal decomposition-like phase separation, following Cahn-Hilliard type phase separation kinetics upon exposure to water vapor. An exponential increase in the scattered light intensity at short times is found. Transmittance measurements are used to determine the effects of molecular weight and coagulation medium on the rate of coagulation.