Freeze-Pump-Thaw

The freeze-pump-thaw method is an effective way of degassing solvents, solutions or liquid reagents.

Step 1: Close the stopcock on the Schlenk flask to seal the contents under inert gas. It is essential that the Schlenk flask is not open to a flow of inert gas whilst being frozen in liquid nitrogen (see Schlenk Line Safety for more information).

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Sealing the flask under inert gas.

Step 2 – Freeze: Freeze the Schlenk flask and its contents in a dewar of liquid nitrogen. Ensure that the stopcock remains closed during freezing.

 

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Freezing in liquid nitrogen.

Step 3 – Pump: Once the contents of the Schlenk flask have frozen, open the stopcock to evacuate the headspace. Keep under vacuum for 3-5 minutes whilst submerged in liquid nitrogen.

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Evacuating the headspace.

Step 4 – Thaw: Close the stopcock to seal the flask under vacuum and remove from the dewar of liquid nitrogen. As the solvent/solution/liquid thaws, the dissolved gas will escape into the headspace.

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Thawing the contents.

Step 5: Repeat steps 2-4 two more times for a total of three freeze-pump-thaw cycles.