Vacuum Line Techniques for Handling Air-Sensitive Organometallic Compounds

Vacuum line techniques for handling air sensitive oganometallic compounds are described. The vacuum line is discussed in six sections: (i) the pumps and main traps, (ii) the main manifold with pressure gauges, (iii) work stations, (iv) the cryogenic traps and Toepler pump, (v) the inert gas purifiers and inlet system, and (vi) the specialty gas inlet system. Use of a swivel frit assembly in the synthesis of air sensitive compounds is described along procedures for the addition of gases, volatile and nonvolatile liquids and solutions to reaction mixtures. High temperature and pressure reactions are discussed in terms of the use of sealed NMR tubes and heavy walled reaction vessels. The procedure for molecular weight determination using the Signer method is also included