The recently reported Co4Cat process is a synthesis method bearing ecological and economic benefits to prepare precious‐metal nanoparticles (NPs) with optimized catalytic properties. In the Co4Cat process, a metal precursor (e.g., H2PtCl6) is dissolved in an alkaline solution of a low‐boiling‐point solvent (methanol) and reduced to NPs at low temperature (<80 °C) without the use of surfactants. Here, the Co4Cat process to prepare Pt NPs is described in detail. The advantages of this new synthesis method for research and development but also industrial production are highlighted in a comparison with the popular “polyol” synthesis. The reduction of H2PtCl6 from PtIV to PtII and further to Pt0 is followed by UV/Vis and XANES/EXAFS measurements. It is demonstrated how the synthesis can be accelerated, how size control is achieved, and how the colloidal dispersions can be stabilized without the use of surfactants. Despite being surfactant‐free, the Pt NPs exhibit surprisingly long‐term (up to 16 months) stability in water over a wide pH range (4–12) and in aqueous buffer solutions. The Co4Cat process is thus relevant to produce NPs for heterogeneous catalysis, electro‐catalysis, or bio/medical applications.