Safe and convenient procedure for solvent purification

Organometallics

Volumn 15, Issue 5, 1996, Pages 1518-1520

  Pangborn, Amy B ^a   Giardello, Michael A ^a   Grubbs, Robert H ^a   Rosen, Robert K ^b   Timmers, Francis J ^b  

^a California Institute of Technology ^*  (United States)

^b DOW CHEMICAL COMPANY   (United States)

Author keywords

[No Author keywords available]

Indexed keywords

EID: 5244370033     PISSN: 02767333     EISSN: None     Source Type: Journal    
DOI: 10.1021/om9503712     Document Type: Article

References (8)

1. Shriver, D. F.; Drezdon, M. A. The Manipulation of Air-Sensitive Compounds, 2nd ed.; John Wiley & Sons: New York, 1986.
2. Gordon, A. J.; Ford, R. A. The Chemist's Companion; Wiley: New York, 1972; pp 429-438.
3. Dietrich, A. Am. Lab. 1994, 26, 33-39.
4. Solvents available in Kilo-Lab cylinders include acetonitrile, benzene, diethyl ether, dimethoxyethane, heptane, hexane, methylene chloride, pentane, tetrahydrofuran, and toluene. Empty cylinders are also available. Kilo-Lab cylinders are rated for 240 psi and have fusible plugs for overpressure situations.
5. Care should be taken during the activation step to prevent water vapor in the vent gas from condensing and running back into the column.
6. Heating tape may also be used. For large columns at least two heating zones are needed with separate thermocouples and controls. We found it convenient to wrap the thermocouple between the column and heating mantle.
7. Valves rated for higher temperatures are available at ap-proximately 3 times the cost of the valves suggested (high-temperature two-way valve for use with hydrocarbons, Whitey 83KS4, with halogenated and ethereal solvents, Nupro SS-4BG). If these valves are used, they may be installed before column activation, and the columns may be cooled under dynamic nitrogen pressure with the exit valves closed.
8. Any disposal practice must be in compliance with all federal, state/provincial, and local laws and regulations.