Glove Boxes

Key features of a glovebox The Antechamber

A glovebox is not much good if you don't have a way of getting your materials in and out. If you look at the pictures above, you'll notice that there is a sealed chamber on the right side of the glovebox. This chamber is called the antechamber (or "port" by some) and it has two doors -- one that can be opened only from the inside of the box and one that can be opened only from the outside. As you can see in the photo on the left, the outer door to the antechamber is open, ready for glassware to be placed inside. See below to see how the antechamber is used. The antechamber can be evacuated with a pump or filled with nitrogen gas. Never have both doors open at the same time!!

The Photohelic Gauge

The photohelic gauge controls the upper and lower pressure limits in a glovebox. Modern gloveboxes use a solid state controller or touch screen interface, but the function is the same. If the pressure in the box gets too high, the controller automatically opens a valve to the vacuum pump to relieve the excess pressure and prevent the gloves from blowing off. Likewise, if the pressure is too low, the controller fills the box with nitrogen. You can set these upper and lower limits by turning the two small knobs below the gauge. The two red needles on the gauge indicate the current

settings and the black one (coincident with the lower setting in this photo) indicates the current pressure. Having the glovebox at a negative pressure with respect to the atmosphere is a Bad Thing because air will be drawn into the box through any small pinholes or leaks. Therefore, one tends to operate a glovebox at a slight positive pressure (i.e. both the cutoffs should be to the left side of zero).

The Pedatrol
The pedatrol is a foot pedal that allows one to manually adjust the pressure inside the glovebox. The high and low limits set on the photohelic gauge still apply, but you can use the pedatrol to open the box to the vacuum pump or the nitrogen supply to get the pressure to a comfortable working level. Notice that the pedatrol is sort of like a two-button computer mouse. Pressing on the left side decreases the pressure in the box and pressing on the right side increases it. No, you can't press both sides at once!

The Gloves
The gloves are obviously an important component of the glovebox. The gloves on a glovebox are usually sized large so that anyone can get their hands in. This makes life a bit difficult for people with small hands, but one quickly learns how to deal with oversized gloves. The biggest threat to the atmospheric integrity of the glovebox comes from pinholes and cuts in the gloves. The most common ways of damaging the gloves involve the use of razor blades, copper wire (sharp ends), syringe needles and scissors inside the box. If you do use any of these BE EXTREMELY CAREFUL!! Gloves are rather expensive and replacement is required if there are more than three or four pinholes on either glove (depending on size).

The Drytrain
On a research grade glovebox, the atmosphere is purified to less than 1 ppm H2O and less than 5 ppm O2 by circulating it through a catalyst bed (also called a "dry train"). The catalyst bed contains Q5 catalyst to remove oxygen as well as zeolites to remove water. After a period of use, the dry train is regenerated by isolating it from the box, exposing it

to hydrogen gas and heating it. The adsorbed oxygen is converted into water and the water is easily removed in vacuo.

Schlenk Lines and Vacuum Lines

One or two manifolds?

A Schlenk or high vacuum line consists of a glass manifold that has several stopcocks, valves or openings in addition to a connection to a vacuum source (typically a mechanical and/or diffusion pump). Having several ports on the line is convenient because several different flasks or reaction vessels may be used simultaneously. For example, gases can be vacuum transferred from one flask to another or several reactions may be run at the same time.

These lines may be of a dual or single manifold design. In a single manifold design, the manifold's main purpose is for vacuum. Here is an example of a single manifold design which uses all-Teflon(tm) valves and O-ring joints to ensure a good vacuum seal. Each port has its own independent bubbler, so up to three reactions can be stirring under nitrogen at one time.

A dual manifold design provides one manifold for vacuum and another for nitrogen or a reactant gas. A connection between the two manifolds permits the nitrogen manifold to be easily evacuated. Shown below is a diagram of a dual manifold high vacuum line. Note that the lower manifold is for vacuum and the upper one is for nitrogen.

Two features worth noting in this drawing are:

1. Main Trap. When the line is running, this trap is immersed in a liquid nitrogen dewar. This stops volatile or corrosive vapors that have escaped the pre-trap and prevents them from entering the pump. New pumps can cost one to two thousand dollars, so protecting the pump is its ONLY role. NEVER PULL SOLVENTS INTO THE MAIN TRAP! 2. Pre-Trap. This is an additional liquid nitrogen trap to condense vapors or gases from the vacuum line. It is also used to collect solvents that are removed from reaction flasks. If you are removing a lot of solvent from a reaction the nitrogen level will drop quickly, so be sure to keep an eye on it. Click on any of these manifolds for more information or to order:

Dual Manifold Line

Single Manifold Line

Dual Manifold, Souza Design

Single Bank Manifold

Double Bank Manifold 4-port Vacuum/Inert Line