Always use a stir bar, not boiling stones.
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Grease all joints.
Use a Claisen adapter, as solutions tend to bump under vacuum.
Connect thick-walled hosing at the vacuum adapter to a trap, then to the vacuum source (water aspirator or vacuum pump).
Turn on the vacuum first, before heating, to remove very volatile components.
When confident the apparatus is maintaining a reduced pressure, then heat the sample.
Use glass wool or foil insulation if the sample is stubbornly refluxing instead of distilling.
Record temperature and pressure if using a manometer during active distillation.
Pure compounds may not distill over a constant temperature due to changes in pressure.
If multiple fractions will be collected, the system needs to be vented and cooled in between (or a cow receiving flask used).
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To stop the distillation, remove the heat and cool the flask in a tap water bath.
Then open the apparatus to the atmosphere by opening the pinch clamp on the trap, or removing the tubing on the vacuum adapter.
Lastly turn off the vacuum.
Correct order: cool, open to atmosphere, then turn off vacuum.
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I am preparing to do a vacuum distillation and am unsure exactly how to manage the vacuum. The vacuum pump I have is a two-stage rotary vane pump which is capable of 250 microns or lower. It has a triple inlet, one 1/4", 3/8" and 1/2".
My glassware is typical distillation glassware including a Graham condenser and a vacuum takeoff joint that connects between the condenser and the receiver.
My concern is that if I apply too much vacuum that it will cause a glass implosion. Is this not a concern and I can just operate the vacuum pump freely, or do I need to take special steps to limit the degree of vacuum?
I watched a YouTube video of a guy doing a vacuum distillation and I noticed that he did not use a capillary bubbler. Under what circumstances can the bubbler be dispensed with?
Another concern is the need for a manometer. I have read that I need to use a closed-end manometer (very expensive) to measure the pressure in a vacuum distillation. Why can't I use a normal vacuum gauge? Also, if I am doing an azeotropic separation such as a water-ethanol separation, is it critical I monitor the pressure? I am assuming it is.
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