Entering the Glovebox:

Items intended to enter the gloveboxes can enter through two antechambers (large and small). These chambers must not be used at the same time. All chemicals entering the glovebox must be degassed and/or rigorously dried. All glassware entering the glovebox must also be dried in the drying oven for a minimum of 1 hour. All empty vessels and dried solids should be vented so no positive pressure is created inside a flask. If a liquid or a flask containing dry reagents is entering the glovebox in a sealed vessel, the vessel must be evacuated on a Schlenk line prior to placing in the antechamber. If this is not done, it is an explosion hazard. If a vessel is sealed at atmospheric pressure, when the antechambers are evacuated to nearly 0 torr the glassware will likely explode due to the extremely high positive pressure within the flask compared to outside the flask. Unopened chemicals packaged under an inert atmosphere may be brought directly into the glovebox. Kimwipes should be dried in the vacuum oven for several hours (>3 h) after the sides of the box have been cut and the plastic opening has been removed (this ensures complete drying of all the Kimwipes). All disposable glassware should be in the oven for a minimum of 3 hours, although up to 8 is preferred.

Aqueous solutions, alcohols, acetone may never be brought into the glovebox. As they compromise glove lifetime and/or the H2O/O2 free atmosphere.

Entering the small antechamber:

When bringing items into the glovebox through the small antechamber, it is imperative that the chamber has been evacuated at least 5 minutes if an item has been removed through that chamber. Refill the evacuated chamber by turning the valve from “Evacuate” to “Refill.” The pressure in the chamber will rise to atmospheric pressure. Turn the valve to “closed” and open exterior of the chamber to insert materials. After sealing the chamber, turn the valve cautiously to “Evacuate.” Be patient when turning the valve so the pressure decreases slowly. This will reduce the likelihood of glassware shattering if there is a small positive pressure within a flask. Evacuate the chamber for a minimum of 5 minutes. During this time, you must perform 3 backfills. A backfill is accomplished by turning the valve to “Refill” to refill the chamber until the gauge moves approximately 1/8 of the way. After 5 minutes, the chamber is returned to atmospheric pressure.

Entering the large antechamber:

The large antechamber should be used for items that do not fit into the small chamber. In order to use the large chamber, the small chamber must be closed under static vacuum. If an item has recently been removed from the large antechamber (on the log), the chamber must be evacuate for a minimum of 30 minutes prior to bringing anything new into the glovebox through the large antechamber. The touch screen located on the front of the glovebox controls the large antechamber. First, select “Manual Refill” from the “Antechamber” menu. Then open the chamber and place items entering the glovebox into the chamber. An item entering the large antechamber must be evacuated and refilled 3 times over a 30 min cycle. Once the evacuate/refill process has been completed, the chamber can be manually refilled and the item(s) can be brought into the glovebox. Finally, the empty chamber should be manually evacuated immediately after emptying the chamber by selecting “Manual Evacuate” from the 5 “Antechamber” menu.

Working in the Glovebox:

All individuals working in the glovebox must remove all jewelry and watches from hands and wrists. White nylon liner gloves must also be worn whenever using the gloves. This preserves the glove lifetime.

When working in the glovebox with solids, the catalyst should be open. All solid waste should be disposed in the open container. Avoid contacting solid chemicals with the gloves and clean up spills after using solid chemicals.

Different solvents and materials affect the catalyst differently. Some catalyst poisons bind irreversibly to the catalyst whereas others bind reversibly. If working with a solvent that binds irreversibly, the catalyst must be closed. Reactions running in the glovebox should be stoppered or capped regardless of the solvents being used to reduce atmosphere or catalyst contamination.

Liquid waste should be placed in the capped bottle. The liquid waste bottle should be open for as brief a duration as possible. It is particularly important that the glovebox catalyst is closed, as all solutions (including solvents that poison the catalyst) are discarded here.

While working in the glovebox, the atmosphere must be checked constantly. This is done by tipping and jostling the vial of diethyl zinc. If smoke or white vapors appear, the atmosphere is bad and the box must be purged. If the diethylzinc vial is caked with zinc oxide, it is time for the vial to be changed. Also, to effectively test the atmosphere, there must be a minimum of 1 mL of diethyl zinc in the vial, although up to 3 mL is preferred.

All chemicals in the glovebox must be properly labelled on the outside of the vials. When any waste jar is full, it should be removed from the glovebox, and a new bottle should be pumped in.

Exiting the Glovebox:

Items intended to exit the gloveboxes can exit through two antechambers (large and small). To remove items from the glovebox, “Refill” the desired chamber, open the chamber, place in items to be removed and reseal the chamber. Turn the chamber to “closed,” and open chamber outside the glovebox to remove the items. After removing items, reclose the chamber and turn to “Evacuate.” Put the items in the hood.

After Working in the Glovebox:

After working in the glovebox, ensure that all work spaces/glassware used has been thoroughly cleaned or removed for cleaning. Furthermore, if solvents were used and are no longer open to the glovebox atmosphere, the glovebox must be purged. Purging the glovebox is necessary to ensure any chemicals remaining in the atmosphere have been removed prior to re-exposing the 6 catalyst to the glovebox atmosphere (see below).