Multidisciplinary lab experiments combining microfluidics, nanoparticle synthesis, and characterization are presented. These experiments rely on the implementation of affordable yet efficient microfluidic setups based on perfluoroalkoxyalkane (PFA) capillary coils and standard HPLC connectors in upper undergraduate chemistry laboratories. Fundamental principles and concepts as well as practical tips for the rapid deployment of microfluidics are presented. In-line membrane separation, the segmented-flow regime, high-temperature experiments, and in-line analytical techniques are illustrated by the preparation of inorganic nanoparticles (silver, gold, and cadmium selenide or telluride) in microreactors. Besides microfluidics, analytical techniques for nanoparticle analysis are also illustrated.