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.
Dioxins, which are thermally produced from several precursor molecules, were investigated by supersonic jet/multiphoton ionization/time-of-flight mass spectrometry (SSJ/MPI/TOF-MS). Dibenzofuran and dibenzo-p-dioxin were efficiently generated from o-chlorophenol and also from phenol after a chlorination reaction with FeCl3. The present technique was employed for the continuous monitoring of a specified isomer, e.g., m-chlorophenol, which is formed at relatively low temperatures by chlorination of phenol with FeCl3. A dimerization reaction that forms a dibenzo-p-dioxin, e.g., dichlorodibenzo-p-dioxin from 2,4-dichlorophenol, at relatively high temperatures was also investigated. The number of chlorine atoms in the dioxin molecule was largely correlated with the number of chlorine atoms in the precursor molecule. However, some unexpected compounds, which probably occur by dechlorination and rearrangement reactions, were also found. Thus, the SSJ/MPI/TOF-MS technique represents a sensitive, as well as selective, analytical method for monitoring thermally generated dioxins.
This study verified that laser ionization time-of-flight mass spectrometry (LI-TOFMS) is applicable to the evaluation of a local microenvironment in an emulsion.
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