In a demonstration experiment, the vapor and liquid disiributions in a hollow-cone spray have been separately photographed using laser-excited fluoresent dopants which form organic exciplexes. In color photographs, the Fluorescence from the liquid appears blue-green and the fluorescence from the vapor appears purple. With high-speed black and while film, “stopped action” pictures of the liquid and/or vapor portions of the spray were obtained. This technique may lead to the development of real-lime visualization diagnostics For evaporating fuel sprays.