Electromagnetic material characterization is the process of determining the complex permittivity and permeability of a test sample. The primary goal of this thesis is to develop a new two-transmission material measurement method to decrease the error associated with using a reflection measurement. The transmission method uses a sample transmission measurement and an acrylic-backed sample transmission measurement. This technique is first demonstrated in a rectangular waveguide system then extended to frequency-domain and time-domain focus arch free-space systems. The frequency-domain free-space calibration process decreases accuracy at the band edges. The use of a digital oscilloscope with a time-domain reflectometer (TDR) module should increase accuracy by removing the windowing and transforming operations and is a secondary goal of this thesis. The two transmission method is compared to the NRW method to validate the two transmission method in all three measuring devices