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Published November 24, 1987 | public
Book Section - Chapter

Vacuum Line Techniques for Handling Air-Sensitive Organometallic Compounds

Abstract

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.

Additional Information

© 1987 American Chemical Society. Received July 31, 1987. Published in print 24 November 1987. The authors wish to thank members of the Bercaw group, past and present, who have contributed to the development of the procedures and equipment described in this chapter. JEB wishes to thank Professor Hans H. Brintzinger (presently at the University of Konstanz, West Germany) for inspiring many of the original concepts when the two of us were at the University of Michigan.

Additional details

Created:
August 19, 2023
Modified:
January 14, 2024