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Abstract: Microfluidic devices are successfully in use for several applications in chemical engineering and biotechnology. Nevertheless, there is still no breakthrough for microprocess engineering because of a huge lack in understanding of the mechanisms on microscales for momentum transfer, hydrodynamics and mass transfer. Some important questions concern the design of a junction to reach acceptable mixing qualities with minimum pressure drop and narrow residence time distribution even under laminar flow conditions. The micro-particle image velocimetry (µ-PIV) in conjunction with confocal laser scanning microscopy (CLSM) have been used for the characterization of momentum and mass transfer at the Institute of Environmental Process Engineering to evaluate microfluidic devices. The calculation of three-dimensional flow and concentration fields is possible with two-dimensional measurement data for common stationary cases. Streamlines out of velocity gradients and isosurfaces out of fields of the same concentration are providing a helpful impression of the performance of microdevices based on highly reliable measurement data. A quantitative analysis of the velocity and concentration fields allows the calculation of residence-time distribution and mixing quality, which enables the adjustment of microreactor geometries for the demands of chemical, and biochemical reactions.