1. Glovebox Protocols BeatBox JukeBox
Right Handed GB (Arnaud, Charlie, Sumesh, Giulia, Chris and Peck)
JukeBox
Left Handed GB (Arron, Gemma, Tim, Alice, Ni, Frank and Tom)

2. Glovebox workstation Designed to work under inert atmosphere: under N2
oxygen-free and water–free atmosphere
Use to store and handle air-and moisture- sensitive compounds
hygroscopic compounds, B(C6F5)3…
pyrophoric compounds, (AlMe3)….
Not for toxic compounds
not necessarily caught by the purification system
directly release into fumehood (Arnaud)/ Centre console
working with toxic compounds in the glovebox is not always safer than in a fumehood

3. Only glovebox team to perform maintenance
Glovebox workstation
Only glovebox team to perform maintenance
Antechamber(s)
small port
big port
Gloves
Analysers
(Back)
Purification system
activated charcoal
“catalyst”
Freezer
-35 oC
Chiller
Vacuum pump &
pressure regulation

4. Antechambers Designed for transferring material into or out the GB
Transferring materials into the GB:
Repeated evacuation and refilling procedure
First refilling to a pressure of 200 mbar is sufficient
Cycle period :
Small port - 3 x 1min
Large Port – 3 x 30 mins (or overnight)
HOT glassware (O2 and H2O adsorbed)

5. Antechambers
Transferring materials into the GB – Large Port Operation:
Small and Large port share the same nitrogen source and vacuum
When using large port, must close small port chamber from nitrogen and vacuum sources
1. Close Small Port

6. Antechambers
Transferring materials into the GB – Large Port Operation:
Small and Large port share the same nitrogen source and vacuum
When using large port, must close small port chamber from nitrogen and vacuum sources
2. Open and Charge
Large Port
1. Close Small Port

7. Antechambers
Transferring materials into the GB – Large Port Operation:
Small and Large port share the same nitrogen source and vacuum
When using large port, must close small port chamber from nitrogen and vacuum sources
2. Open and Charge
Large Port
3. Close Port Finger tight Avoid overtightening
1. Close Small Port

8. Antechambers
Transferring materials into the GB – Large Port Operation:
Small and Large port share the same nitrogen source and vacuum
When using large port, must close small port chamber from nitrogen and vacuum sources
2. Open and Charge
Large Port
3. Close Port Finger tight Avoid overtightening
1. Close Small Port
4. Pull leaver down to apply vacuum

9. Antechambers
Transferring materials into the GB – Large Port Operation:
Small and Large port share the same nitrogen source and vacuum
When using large port, must close small port chamber from nitrogen and vacuum sources
2. Open and Charge
Large Port
5. Recharge with N2, close black leaver and open red leaver
3. Close Port Finger tight Avoid overtightening
1. Close Small Port
4. Pull leaver down to apply vacuum

10. Antechamber
Caution:
Material with enclosed inert gas (ampoules (Youngs + Rotaflow), centrifuge tubes, J.Youngs NMR tube, glass sealed ampoules) should be able to withstand the pressure difference
Schlenk Tubes must be under vacuum – risk of breaking glass
Commercial available product should be packaged under inert gas (otherwise open the lid) – if in doubt use half cycles – 30 times
Plastic stuff (syringes, filters….) : at least overnight under vacuum
Tissues: drying few days at 140°C then at least overnight under vacuum

11. Antechamber Transferring (nasty) material out
Pyrophoric compounds (dilution in toluene, closed vials, sand…then follow standard procedure to destroy it in the fume hood)
Syringes, needles, pipettes (if used for toxic and/or pyrophoric compound)
Highly Pyrophoric compounds – kill in a Schlenk tube.

12. Gloves NO Lab Coats! Glovebox work more enjoyable Improved dexterity
Must go in with CLEAN lab gloves
Change current gloves for fresh ones
Be careful with :
Needles
Broken glass
Minimize use of sharps
Solvents (Toluene, THF)
Emergency action:
In case of a hole… electrical tape
Maintenance
Need to be changed regularly (glovebox team)

13. Do / Don’t Do Fill in the log book!
Label your samples (label and ballpoint?)
Don’t leave Schlenks for ages in the GB
Minimize number of old recrystallizations
Avoid duplicate solvents/reagents
Clean after work
Top-up pipette pot and tissues when necessary
Minimize solvent use
Don’t
Open the antechamber from inside and full of air
Opening the antechamber when under vacuum
Leave pyrophoric powder / solution in vials and initiate fire when outside

14. Purification system Try to avoid/minimize use!
To use “nasty” substances :
stop the circulation
do what you have to do
quick purge
switch the circulation on

15. Regeneration
Regeneration (~16 h without GB) – both solvent and catalyst purification
Pump oil has to be checked/changed
Catalyst Regeneration – infrequent, only if required (abnormally high O2/H2O)
Solvent Regeneration – Every Thursday 6pm

16. Functions Panel Issues
Regeneration
Pressed accidentally
Only when Circulation is off DO NOT PRESS OK!
Immediately contact glovebox team
Cannot be cancelled once started
~ 2 h delay – check gases
Will start even if no forming gas (H2 in N2)

17. Functions Panel Issues
Purging
Turn off Circulation
Box Purging will become active to press
Once finishes switch circulation back on.

18. Functions Panel Issues
Freezer
Accidentally pressed
Freezer switched off
Please be careful!
Check when finished

19. Conclusion Please be considerate to us and other users!
Better atmosphere = better chemistry!