Abstract A realistic description of fluid mechanical and acoustic processes requires the volume viscosity of the medium to be known. This work describes how the volume viscosity of pure fluids can be determined by measuring acoustic absorption with the pulse-echo method. The challenge in realizing such a measurement method lies in the separation of the different dissipative effects that superimpose on absorption. Diffraction effects ultimately cause a dissipation of acoustic energy and acoustic reflector surfaces have a small, but finite transmission coefficient. Further, influences of the transducer (in particular its frequency response), as well as the system’s electrical components have to be taken into account. In contrast to the classical approach relying on the amplitude ratio, the absorption is determined by the moments of the amplitude spectrum. The measurement system applied is originally designed for precision measurements of the sound velocity by means of the propagation time difference of two acoustic signals.