adsorption from saturated dichloromethane (VWR, The Netherlands) onto
molecular sieve 3A beads, 2 mm diameter (Sigma–Aldrich), were
measured at 25 and 40 °C. Molecular sieves were dried in an oven
at 200 °C for 48 h. Adsorbent was then cooled to room temperature
in a glovebox (MBraun MB 200B) kept in a dry nitrogen atmosphere (<0.3
ppm of water). Between 0.02 and 0.50 g of dry adsorbent was weighed
and transferred into 60 mL vials capped with PTFE septum caps. 60
g of DCM saturated with demineralized water (Veolia Water Elga Purelab
S7, 0.1 μS cm–1) was injected into the same
vials through the septum. A dry DCM sample was prepared in the same
manner to detect potential contamination of the samples with water.
The prepared samples were then placed inside a shaker (IKA) at 100
rpm at a preset temperature. Samples were taken at fixed time intervals
with 2 mL syringes through the septum, to avoid water adsorption from
air. The water content was measured with a coulometric Karl Fischer
titrator (Metrohm Applikon Coulometer KFT 899). The equilibrium between
the adsorbent and the liquid was reached within 2 days. The average
mass loss of DCM was <1% (w/w).