The described setup was first employed to separately evaluate the effect of the milling action on the sublimation rate of three compounds with expected largely different vapor pressure (Figure ): parabenzoquinone (p-BQ), racemic 1-indanol (rac-IND) and racemic a-(trifluoromethyl)lactic acid (rac-TLA). The experiments were conducted inducing the sublimation of 80.0 mg of the analyte inside the milling jar by the action of a N2 flow alone for 90 minutes, followed by the additional activation of the milling action for further 90 minutes. For all three substances, a plateau in the sublimation rate was quickly reached without the milling. In turn, a sharp increase in the evaporation speed was observed when the milling was started. Both rac-TLA and rac-IND showed a constant linear evolution of sublimate after the grinding was started. Their slopes, however, differed being in line with their different vapor pressures. Another behavior was observed for p-BQ. There, an abrupt acceleration was followed by a sudden deceleration, resulting from first, an extremely rapid sublimation followed by, second, the complete consumption of the analyte, as verified upon opening the milling jar at the end of the 180 minutes.