Speed of sound and acoustic wave attenuation are sensitive to fluid phase composition and to the presence of liquid-liquid interfaces. In this work, the use of an acoustic array comprising 64 elements as a non-intrusive sensor for liquid-liquid interface, phase separation kinetics measurement in bulk fluids, and local composition measurement in porous media is illustrated. Three benchmark examples: the phase behaviour of methanol + mixed hexanes and methanol + heptane mixtures at 25.0 °C and 1 bar, and Athabasca bitumen + heptane in a synthetic silica porous medium at 22.5 °C and 1 bar, illustrate the accuracy of liquid-liquid interface and potential research and industrial applications of the technique. Liquid-liquid interfaces can be detected independently using both speed of sound and acoustic wave attenuation measurements. The precision of the interface location measurement is 300 μm. As complete scans can be performed at a rate of 1 Hz, phase separation kinetics and diffusion of liquids within porous media are readily tracked. The technique is expected to find application where the fluids or porous media are opaque to visible light and where other imaging techniques are not readily applied, or are too costly. A current limitation is that the acoustic probes must be cooled to less than 315 K in order for them to operate.