Optical laser-based techniques and an extensive data analysis methodology have been developed to acquire flow and separation characteristics of concentrated liquid–liquid dispersions. A helical static mixer was used at the inlet of an acrylic 4 m long horizontal pipe to actuate the dispersed flows at low mixture velocities. The organic (913 kg m−3, 0.0046 Pa s) and aqueous phases (1146 kg m−3, 0.0084 Pa s) were chosen to have matched refractive indices. Measurements were conducted at 15 and 135 equivalent pipe diameters downstream the inlet. Planar laser induced fluorescence (PLIF) measurements illustrated the flow structures and provided the local in-situ holdup profiles. It was found that along the pipe the drops segregate and in some cases coalesce either with other drops or with the corresponding continuous phase. A multi-level threshold algorithm was developed to measure the drop sizes from the PLIF images. The velocity profiles in the aqueous phase were measured with particle image velocimetry (PIV), while the settling velocities of the organic dispersed drops were acquired with particle tracking velocimetry (PTV). It was also possible to capture coalescence events of a drop with an interface over time and to acquire the instantaneous velocity and vorticity fields in the coalescing drop.