We have four gloveboxes (one double box, two single boxes). Due to issues with the previous Argon glovebox freezer, the majority of the commonly used chemicals are currently located in the Nitrogen gloveboxes.
The environment in the glovebox is both warmer than the lab, and has substantially more static electricity. There are automatic static discharging devices, but there's also a static gun that can help remove static electricity from weigh papers and samples. These are operated by slowly pulling the trigger while pointing it at the object you want to discharge static electricity from.
Short glass pipettes that are oven dried are a good tool for weighing out multiple samples. Since you cannot wash anything inside of the dry box you have to bring in a separate spatula or pipette for each thing you want to mass out.
Cleaning inside the dry box is difficult as there are no solvents. Whenever you use the box try to wipe around with some kimwipes and take them out of the box with your reaction and other waste.
¶ Standard operating Procedure.
Before using the glovebox please have an older student personally train you. This is to serve as a reference for proper technique and not an introductory guide.
As of now the general glovebox etiquette is to use the box with gloves, and without your lab coat. There should be a nearby spray bottle of isopropanol to wipe down the gloves after use to keep them sanitary.
- Check that the N2 tank is connected and not empty before doing anything with the box.
- Log your entry time and the current O2 ppm before touching the box.
- To enter the glovebox, fill the antechamber with N2. Place any materials you need inside the antechamber. Any chemicals/vials/containers must be uncapped or under a complete inert atmosphere (eg: evacuated and backfilled multiple times on Schlenk or with Argon).
- Slowly turn the knob to place antechamber under vacuum for a minimum of 5 minutes. After 5 minutes slowly and carefully refill the antechamber halfway. Repeat this for a total of 3 cycles, resulting in 15 minutes of vacuum time total. On the final backfill, fill theantechamber fully. FOR NAPKINS/PIPETTES/CORKS these should be pumped in overnight. Use the in-use sign and message the groupme.
- Enter the glovebox (you can do this with one arm), open the antechamber. Remove all your contents from the antechamber and then close it. Return the antechamber to vacuum before you begin setting up reactions.
- At this point if you intend to use any wet, highly volatile, or coordinating solvents, turn off the circulation while setting up your reaction. In general, assume the circulation should be off unless you are using hydrocarbon or ethereal solvents.
- After setting up your reactions slowly refill the antechamber with N2 and then open it and place anything you’re removing from the box inside. THIS INCLUDES ANY KIMWIPES OR PIPETTE TIPS YOU USED. Remove solvent bottles when they are empty / very low.
- If there has been a spill in the glovebox, use a dry kimwipe (drybox) or a kimwipe wetted with THF (wetbox) to clean up the spill.
- Remove your items from the antechamber, return the antechamber to vacuum and make sure both doors are properly sealed.
- If you had turned off the circulator, or if you’ve left it on but noticed a spike in oxygen, purge the glovebox for 10-15 minutes. Set a timer and make sure turn the purge off and everything back on (circulation reactor 2 and vacuum).
- Wipe down the exterior of the gloves using isopropanol solution.
- Log your exit time and the O2 ppm. Do this after your purge if you’re purging, the O2 readout is only accurate when the circulator is on.
If you encounter any issues using the glovebox, please contact Liam or Quan.
Liam: laf2187@columbia.edu 802-735-3021, Quan: qlt2003@columbia.edu 559-312-8521