Vacuum in the Glovebox

Introduction

In some instances it can be convenient to have a vacuum setup in the glovebox. This setup is for the evaporation of small amounts of solvents only, and by no means an invitation to perform prep-scale reactions inside the glovebox. It can be used to dry crystals obtained during a crystallization attempt or samples for element analysis.

The setup contains:

  • vacuum pump, which is situated outside of the glovebox;
  • feed through the back wall of the glovebox;
  • trap to protect the pump when bumping solvents as a result of boiling delay (figure 1a);
  • two types of connectors that allow you pump down the contents of aspirin tubes or scintillation vials (figure 1b).
trap.jpg adapter.jpg
Figure 1a Figure 1b

Mode of operation

Using vacuum in the box is very straightforward. You switch on the pump, attach your flask to the vacuum, open the main valve (the black valve in Figure 1a) and start pumping down your mixture. Once finished, it is important to close the main valve again and to switch off the vacuum pump.

In order to pump down an aspirin tube, you can use the adapter which is depicted on the left in figure 1b. It consists of a B24 cap with a B24 hose adapter and the two together fit an aspirine tube. For scintillation vials you can use a B14 hose adapter with a pierced septum attached. The end of the septum has the same size as a scintillation vial (depicted on the right in figure 1b).

Remarks:

  1. Don’t forget to switch off the vacuum pump when you are done and close the valve inside the glovebox
  2. Keep the setup clean. If you bump solvents or the setup is no longer clean, take out the setup, clean it and put it in the oven next to the glovebox. After one hour bring it back in.
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