In this study, we used a technique based on pulsed Raman spectroscopy to determine the average concentration in the liquid phase and concentration distribution in the gas phase surrounding desorbing linear arrays of binary microdroplets. For this study, monodisperse microdroplets consisting of acetylene dissolved in acetone were generated by a modified vibrating orifice aerosol generator (VOAG). The 2-dimensional concentration fields of acetylene desorbed from the droplets were determined with a spatial resolution of about 40 mu m both along the direction of the droplet chain and perpendicular to it. The detection limits for the gas and liquid phase concentrations were about 100 ppm and 1 mmol/l, respectively.