The effect of cryogenic and heating treatment on the solution properties of rigid polymer nitrocellulose (NC) in dilute tetrahydrofuran solution were studied with a sealed viscometer and a size exclusion chromatograph (SEC),respectively. The experimental results show that the relative viscosity of NC solution decreases after repeated freezingthawing treatment. The decreased viscosity value of NC could not be restored but decreased further after the solution being re-heated. The experimental results of SEC are fully consistent with that of viscosity measurements. It is believed that the effect of two treatments on NC solution both causes the apparent hydrodynamic volume to decrease. But they are assumed to be ascribed to different mechanisms.