Abstract SCHIRACK, ANDRIANA VAIS. The Effect of Microwave ...

7. If target pressures are not reached in 15 minutes, check for leaks. When open
fully, should get to 10 -3 and 10 -4 before proceeding.
8. Fill up dewars with liquid nitrogen.
9. Attach 2 sets of heating tape - tie to sample chamber, wrap to right of stopcock
and over neck of first trap, and use the second tape to cover the neck of the
round bottom flask. Leave access to all threads.
10. Attach water hoses – allow for a slow stream on exit to the sink.
11. Plug in heating tape and turn on.
12. Make sure all fittings tight, and make sure stopcock is closed.
13. Add sample to top chamber, then slowly open stopcock to let drops of extract into
round bottom flask.
14. After all of the extract is introduced, pour ether in as wash (~30mL). Rinse both
the glassware used, and inside of chamber.
15. Let SAFE distillation run approximately 2 hours. It is done when you can no
longer see boiling in round bottom flask.
16. Refill liquid nitrogen in dewars and cover (aluminum foil); make sure nitrogen
levels are full during entire run and periodically check waterbath temperature.
17. NOTE: Make sure the sample does not freeze during the SAFE procedure –
apply heating tape far down the neck of the round bottom flask, and make sure
water levels in the bath are sufficiently high enough.
When SAFE is completed:
1. Close blue valve.
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