The Glove Box

For the preparation, manipulation and/or analysis of air-sensitive chemicals, the use of a glove box may be necessary. When purged with an inert gas eg nitrogen, the inert atmosphere in the glove box will allow handling air-sensitive substances. 

A sketch of the glove box is depicted in Fig.2.9. The pressure in the box should be maintained at a positive pressure of nitrogen. About 1.5-2 cm of oil on a manometer tube represents a satisfactory pressure and will cause the gloves to become inflated outside the box. The mercury lute acts as a safety valve and will prevent the build up of pressures greater than 1 cm of mercury in the box. 

For filling the box with nitrogen, a large plastic bag is connected at the point a inside the box on the nitrogen inlet tube. The bag is allowed to inflate thus displacing air from the box space. When the bag is full, it is disconnected from a so that the nitrogen will fill the box space. It is advisable to repeat this process twice more. 

It is advisable to deaerate liquids and solutions to be used in the box by passing a stream of nitrogen for 5 minutes. Boiled-out water should be used for solutions. 

The glove box can be also used for handling moisture-sensitive materials which may not be affected by oxygen. In such cases, an efficient desiccant e.g. phosphorus V oxide is placed in large area containers and die box filled with moisture-free gas, keeping a desiccant container in the box s tunnel. For chemicals sensitive to carbon dioxide, soda lime is used instead of a desiccant. 

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The electrolyte used is 1 molar LiPF dissolved in a mixture of 30% ethyl carbonate (EC) and 70% diethyl carbonate (DEC) by volume. This electrolyte IS easy to use because it will self-wet the separator and eleetrodes at atmospheric pressure. The electrolyte is kept under an argon atmosphere in the glove-box. The moleeules of electrolyte solvents, like EC and DEC, have in-plane dimensions of about (4 A x 5 A) to (6 A x 7 A). These molecules are normally larger than the openings of the micropores formed in the region 3 carbons (Fig. 2) as described in section 5. 

Electrochemical cells are assembled in the glove-box. The cell is a 2320-type coin cell (23 mm OD and 2.0 mm thickness) as schematically shown in Fig. 5. The cell includes the electrolyte, the cell cap and can which are stainless steel, a polypropylene gasket used to seal the cell, the two electrodes, the separator between the electrodes, as well as a stainless spacer and a mild steel disc spring which are used to increase the pressure on the electrodes. Once the cell is assembled in the right order, the cell is sealed by a pressure crimper inside the glove-box. 

In the patterning experiments, chlorinated poly(styrene) films were baked at 120 C for 15 mins, in a forced air oven, equilibrated for -12 hrs. inside the humidity-controlled glove box, exposed to deep-UV radiation and treated with TiCU under usual conditions. No significant variation in the lithographic parameters was observed by varying the relative humidity in the 30-60% range in the glove box. 

After removal of the gaseous products, the bomb is transferred to the glove box, opened, and inspected for the presence of solid products. If a residue is found it is weighed and analyzed. The crucible is also reweighed to determine if NiF2 was formed in the combustion, and a correction for this side reaction is applied, if needed. 

In a glove-box, l-(2-methylphenyl)ethanol (1.11, 8.14 mmol), tert-amyl alcohol (16 mL), and EtjN (0.67 mL, 4.8 mmol) were added to a flask containing 16 (27.7 mg, 0.0419 mmol). A septnm was added and the flask was removed from the glove box. After some gentle heating to dissolve the catalyst, the flask was cooled to 0 °C. Ac O (0.46 mL, 4.9 mmol) was added dropwise and after 25.5 h the reaction was quenched with MeOH (5 mL). 

For maintenance or repair the open glove boxes are closed. After completing the work and potential decontamination, the glove box walls are removed and the system can be baked out easily. 

Polymerizations were carried out at 30°C in all glass, sealed reactors using breakseals and standard high vacuum techniques (3). For the calorimetric measurements, a 1 liter sample of a 0.03M solution of each polymeric lithium compound with M of ca. 4,000 was prepared in benzene solution using sec-butyl-lithium as initiator and transferred to the glove box. 

In the glove box, prepare a 0.25 M stock solution of each alcohol (Reactant A) in anhydrous DCE. Note In case of salt, equal amount of equivalents of TEA should be added. 

In the glove box, add 320 p,L (80 p,mol, 1.0 eq) of the appropriate alcohol (Reactant A) solutions into the appropriate predried test tubes. Note The reaction is sensitive to the order of the addition of reagents. 

In the glove box, cover each test tube with a test tube cap. 

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