Extensive use of transfer matrices (TMs) is made in determining the acoustic properties of a duct and in in-duct acoustic propagation models in the automotive industry and for musical acoustics purposes. The experimental apparatuses of classical TM measurement methods feature two measurement heads. Two microphones are flush with the walls of each head. The pressure signals are processed following the transfer function method constructed on an analytical model of acoustic propagation in measurement heads. The present paper aims at presenting a measurement method based on a three-microphone experimental apparatus and on its acoustic calibration through two reference measurements: the three-measurement two-calibration method for measuring the TM (3M2C-TM). Two microphones are flush with the measurement head walls and one is in the cap closing one side of the measured duct. 3M2C-TM proved essential for an accurate measurement of the four TM elements of two different ducts: a cylindrical duct and an expansion chamber.