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)

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

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

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)

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

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

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

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

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

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

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.

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)

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

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

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 Evening @ 6pm

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)

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

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

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