Spray drying, the evaporation of liquid solution droplets to dry particles, is crucial to the formation of particles for a variety of industries including pharmaceutical, food and cosmetic. Additionally, the aerodynamic properties of dried particles are important to the nuclear industry for the evaluation of contamination risk and safety precautions. The final structure of a dried particle is determined by a variety of factors during the drying stage including the nature of the droplet components and the drying conditions. Thus, characterising the drying process and its governing factors provides insight into nature of microparticles formed though spray drying. There are a limited number of techniques to make measurements on droplets during their evaporative lifetime. Observation of droplets from droplet generation to dry particle formation is rarely achieved and instruments are often limited by the temporal resolution or ability to collect dried particles for further analysis.