Air-free technique

Air-free techniques refer to a range of manipulations in the chemistry laboratory for the handling of compounds that are air-sensitive. These techniques prevent the compounds from reacting with components of air, usually water and oxygen; less commonly carbon dioxide and nitrogen. A common theme among these techniques is the use of a fine (100–10−3 Torr) or high (10−3–10−6 Torr) vacuum to remove air, and the use of an inert gas: preferably argon, but often nitrogen.

The two most common types of air-free technique involve the use of a glovebox and a Schlenk line, although some rigorous applications use a high-vacuum line. In both methods, glassware (often Schlenk tubes) are pre-dried in ovens prior to use. They may be flame-dried to remove adsorbed water. Prior to coming into an inert atmosphere, vessels are further dried by purge-and-refill — the vessel is subjected to a vacuum to remove gases and water, and then refilled with inert gas. This cycle is usually repeated three times or the vacuum is applied for an extended period of time. One of the differences between the use of a glovebox and a Schlenk line is where the purge-and-refill cycle is applied. When using a glovebox the purge-and-refill is applied to an airlock attached to the glovebox, commonly called the "port" or "ante-chamber". In contrast when using a Schlenk line the purge-and-refill is applied directly to the reaction vessel through a hose or ground glass joint that is connected to the manifold.[1]

  1. ^ Duward F. Shriver and M. A. Drezdzon "The Manipulation of Air-Sensitive Compounds" 1986, J. Wiley and Sons: New York. ISBN 0-471-86773-X.

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