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Flash Chromatography-the Simplest Way

Flash chromatography is a rapid and efficient alternative to normal column chromatography on silica gel.' A
modification to make this technique more suitable far the undergraduate laboratory has recently been desc~ibed.~ This
procedure still requires a special adapter and a supply of pressurized gas, which may not he available at every workstation.
We have used a balloon as a reservoir of pressurized gas, adapted to a simple column with glass tubing and a one-hole
stopper, and find this works very well.
We have carried out the separation of a mixture of ferrocene and acetylferrocene, obtained on acetylation of ferroeene
with phosphoric acid and acetic anhydride.3 A sample of 0.5 to 1.0 g of the mixture was separated on a 1M1-mm column of
silica gel4 in a 300- X 19-mm tube. The column was packed, and 25 mL methylene chloride was passed through under
pressure. By using two 5-in. balloons, one inside the other, a pressure of 2-3 psig is provided, producing a linear flow rate of
3 4 cmlmin. Since the volume of the balloon is large relative to the volume of solvent, little pressure change occurs during
the course of the experiment. The sample was introduced in a minimal volume of methylene chloride; elution with 30 mL of
the same solvent removed ferroeene. This was followed by elution with 30mL of a 1:l mixture of methylene chloride and ac-
etone to isolate acetylferroeene.
The chromatographic separation requires less than 30 min. Students appreciate the time saved by this method, and
the occasional balloon that hursts on filling provides some comic relief.

' i t i l l , W. C.: ~ehn.~.:~ A. J. Olg. Ulem. 1978, A?,2923.


lThompson, W. J.: Hanson, B. A. J. Chem. Educ. 19114,61,645.
Roberts. R. M.; Gilbert. J. C.: Rodewald, L. B.; Wingrove. A. S. "Modern Experimental Organic Chemistry", 3rd ed.;Holt, Rinehart, and
Winston: New Yo*, 1979: p 397.
4The silica gel used was 40 r average particle diameter. J. T. Baker #7024-1. The quantity required is -12 g per column.
Wllllam L. Bell
Robert D. Edmondson
Red Rocks Community College
12600 West Sixth Ave.
Golden. C0 80401

Volume 63 Number 4 April 1986 361

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