Figure 2
Graphical representation of the key parameters during a typical crystallization protocol [jacket temperature, T (K) (full line); vortex frequency, ω (r.p.m./2) (long dashes); pressure, P (mbar = 102 Pa) (short dashes)]. Process steps are indicated as follows. Step 1: solid and solvent(s) dosed into vessels (ω = 0 r.p.m., T = 306 K, P = 1006 mbar). Step 2: agitate at 850 r.p.m., while heating to 413 K, to facilitate solid dissolution; the suspension is held under these conditions for ca 60 min. Step 3: suspensions are vacuum-filtered through sintered glass filters into the post-filtration vessels on the right-hand side of the block, removing undissolved solid. Step 4: the temperature of the filtered solutions is increased by 5 K for ca 10 min to promote dissolution of any seed crystals that may be left after filtration. Step 5: crystallization induced, in this example, by cooling the solutions to 283 K, at a rate of ca 3 K min−1, whilst vortexing at 850 r.p.m. |