Practically, the liquid trapping and NMR block of the setup (Figure ) were disconnected from each other, and a homemade small cooling trap was attached to the outlet tube of the milling jar, allowing the collection of recondensed fractions of the sublimate at intervals of 5 to 10 minutes (see Section 3 of the Supporting Information for a detailed description of the new setup and its operation). The modified apparatus was then used to collect fractions of the accelerated sublimation repeated on the same TLA scalemates analyzed so far. With the different fractions in hand, their enantiomeric excess was then evaluated by NMR ex situ analysis in CDCl3 using (S)-aziridinyl diphenylmethanol [(S)-ADM] as chiral solvating agent (Figure ). Figure -(a) Accelerated sublimation of (S)-TLA scalemic mixtures of 30% ee (azure), 20% ee (teal), 16% ee (lavender), 10% ee (brown) and racemic (cerise). The experiments were conducted on 50.0 mg of solid at the milling speed of 10 Hz and argon flow of 1.5 L/min. (b) Sublimation, collection, and NMR analysis of sublimate samples of TLA. (c) Analysis of sublimate fraction of (S)-TLA scalemates of 90% ee (black), 60% ee (green), and 30% ee (azure) The experiments were conducted on 50.0 mg of solid at the milling speed of 10 Hz and argon flow of 1.5 L/min, the fractions were collected at 8-10 minutes intervals. (d) Analysis of sublimate fraction of (S)-TLA scalemates of 90% ee (black), 60% ee (green) and 30% ee (azure) The experiments were conducted on 50.0 mg of solid at the milling speed of 10 Hz and argon flow of 1.5 L/min, the fractions were collected at 8-10 minutes intervals. The curves reported in graphs (c) and (d) are for visual reference and not the result of a data fitting.