The principle and experimental results of a new self-consistent calibration algorithm of wide-band polarimetric measurement system are presented. The calibration targets include a flat plate, a dihedral corner reflector, and a rotated dihedral corner reflector. The rotation angle of the third calibrator can be derived in the calibration process and used to verify the calibration performance. Based on the signal-to-noise consideration an optimal rotation angle for dihedral corner reflector is found to be 22.5°. This calibration technique is also useful in characterizing the frequency and polarization responses of dual-polarization antennas.