Multiphoton ionization time-of-flight mass spectrometry was applied to the measurement of an oil-in-water emulsion that contained toluene as a dispersed phase. Before the measurement, the sample was sufficiently creamed, and then stirred for a short period of time for dispersion. As a result, several intense spikes appeared on the time profile constructed from the peak area for toluene. In the present study, an optical microscope was used to observe the capillary column for sample introduction, and small toluene droplets along with their aggregates were found in the images of the emulsion flowing through the capillary. The aggregates produced intense spikes comprised of multiple plots, which could be easily marked by applying a moving median filter. In the present study, droplets with minimum diameters as small as 2.9 μm, which corresponds to 13 fL, could be calculated as detectable spikes.

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