Fluorocarbons are one of the most promising hydrophobic phases for future pharmaceutical production processes and various biomedical applications. Yet, because of their specific characteristics such as high density and refractive index similar to water, analysis of water‐in‐fluorocarbon (w/fc) nanoemulsions remains a challenge. The present work examines w/fc nanoemulsions stabilized with phospholipids as natural emulsifiers and tackles the measuring problems of photon correlation spectroscopy (PCS) when used for investigation of fluorocarbon nanoemulsions. These emulsions are suitable to form liposomes via centrifugation and thus, are required to meet certain criteria such as stability and size. The results imply a stability of up to 4 weeks with an average size of 180 nm. The intensity mean diameter gained from PCS measurements shows large scattering directly after sonication which is due to gas bubbles from sonication. The number mean is not influenced by gas bubbles and gives a more accurate depiction of the produced nanoemulsions. These findings are supported by small‐angle X‐ray scattering data, which are additionally applied for liposome analysis measuring a size of approximately 60 nm.