Freeze-Pump Thaw for degassing Ni Yi 11/11/2016

Principles Remove dissolved gases from a liquid Performed under reduced pressure It takes advantage of the pressure dependence of gas solubility in a liquid. Lowering the pressure of the gas above the liquid causes the solubility of the dissolved gas in the liquid to decrease The dissolved gas is released from the liquid as a bubble

Safety Carefully check all glassware for cracks or defects (Vacuum suitable glassware: round bottom, not conical) Do not fill the ampoule > 60% Ensure that Young’s tap creates an effective seal Use a vacuum gauge Person performing this procedure must be in the vicinity of the vessel at all times and alert neighbors in the lab to the procedure Never open the ampoule to argon during freezing

Glassware required Solvent should be stored preferably in a Young’s flasks rather than a Schlenk flask Teflon tap provides a better seal The greased joint seal of a Schlenk flask can degrade over time

Method Note: this picture is for demonstration, please use the ampoule when you are degassing a large amount of solvent It is important not to fill the solvent ampoule to more than 60% of its volume (to avoid the build-up of an overpressure) If an argon atmosphere is used, the solvent ampoule must be sealed and the Schlenk line tap closed, prior to freezing (otherwise gas can be condensed, this presents a significant risk of overpressure) The solvent ampoule should be kept inside the dewar of liquid nitrogen until all of the solvent has frozen

Method Note: this picture is for demonstration, please use the ampoule when you are degassing a large amount of solvent Quickly open and then shut vacuum to apply partial static vacuum as it is freezing. Place under dynamic vacuum for 10-15 min once completely frozen. Remove ampule from liquid nitrogen, and close tap to vacuum. Always be aware of vacuum gauge in case of any leaks.

Method Note: this picture is for demonstration, please use the ampoule when you are degassing a large amount of solvent Keep the fume cupboard sash lowered as far as possible whilst warming The flask is to remain closed under static vacuum as it is warmed with occasional application of dynamic vacuum until the solvent has completely melted. Repeat x3 for general needs After the last cycle the flask is backfilled with N2/Ar at room temperature Dry solvents can be stored over suitable drying agents, such as molecular sieves to prolong their life.