This thesis discusses the measurement of dielectric constant and loss tangent of microwave substrates. The measurement instrument use Agilent E4991A impedance analyzer with Agilent 16453A test fixture. The measurement method is based on the principle of parallel plate capacitor to calculate the dielectric constant and loss tangent from the measured impedance values. The test fixture is calibrated using open, short and standard load compensation based on the two developed methods, RLC equivalent circuit method and ABCD matrix method, to remove the residual impedance, which is a major cause of measurement errors. In addition, a correction function based on measurement results are used to correct effect of edge capacitance. Finally, this thesis discusses the measurement accuracy of the test fixture compensation and the effect of the dielectric plate thickness on the measurement dielectric constant value.