Glove box purging

A standard size glove box purged continuously with such air at this flow rate can maintain an atmosphere whose H20 or C02 content is much below the detection limit of any research grade FUR spectrometer. The operation of an FTIR spectrometer under such conditions provides excellent isolation from C02 and H20 and eliminates the time wasted in waiting for the stabilization of the spectrometer atmosphere after each measurement (as is the case in the normal operation of a purged instrument). 

Depending on their sensitivity, solids are loaded into pressure reaction bottles in the air or in an inert-atmosphere glove box. The bottle is capped and may be carried through several purge cycles by means of a hypodermic needle attached... 

Fig. 2.6. Schematic representation of a dry-box purification scheme. (A) Glove box (B) tank argon (C) purge line for pump container (D) gastight pump container (E), 2.7 ft /min graphite ring pump (F) bubbler (G) purification train consisting of Linde 13X and 4A Molecular Sieves, and Vermiculite-supported MnO at room temperature (see Chapter 3). In some installations an additional drying column follows the MnO column. Approximate column dimensions are 3-in. diameter by 4-ft length. (Unpublished design of T. L. Brown.)...

In a typical batch distillation, the lower bulb of the system is loaded with the solvent and a suitable absorber in the glove box, after which it is connected to the system under flowing argon. The system is purged with argon, the appropriate pressure is adjusted, and the lower bulb is heated to boiling point. The first fraction is taken out, and total reflux is applied. Then the middle fraction, the pure material, is collected in the terminal bulb. As the distillation stops, the terminal bulb is closed hermetically and introduced into the glove box. 

The experimental aspects of ex situ FUR spectroscopic studies of sensitive electrodes (e.g., Li and Ca surfaces) using a purged spectrometer (not in a glove box) have been described in detail in Refs. 36-38, 92, and 93. Briefly, it is possible to analyze thin surface films on active metal, using a reflectance mode, while the active surface is in contact with a KBr or NaCl polished window. In Refs. 37 and 38, a possible organization of the measurement chamber of an FTIR spectrometer for such measurements is described. It should be noted, however, that the performance of such measurements when the spectrometer is placed in the glove box is much more elegant and easier. 

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