A Simple Device for Flash Chromatography

Flash chromatography is an important improvement in column chromatography;' use of 40-63 p m silica instead of
W 2 0 0 pm increases the optimal rate of the mobile phase, and thus so that elution is complete within 20 min. This is specially
important for teaching, because column chromatography can he very tedious and time-consuming in a practical lab course
in organic synthesis. With this new technique, preparation of the column, elution, and analysis of the fractions are completed
in two hours.
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The only trouble for s t u d ~ n t ais trse of compressed air. The column must he opened and filled with solvent frequently
and each time the air flow regulator has u,he readjusted. l i t h e pressure is released t m fast, the adsorbent layer is cracked.
If the pressure is tw high, then the air flow regulat<,r,which is expensive, is often ejected and broken. We descrihe her? a
simple. low-cost device whwh prevents all these inconveniences.
Am is admitted into the system through a restrictor. which is specially useful when the pressure available is ton great.
The restrictor is simdv a 8-mma d . alms tuhe, constricted at oneend in order to h a w a 2-mm hole. This admits only a l w
air flow into the device. The restrict& is connected by silicone tubing t o the pressure regulator, which is a T tube immersed
in mercury. Use of a n SVLglass screw adaptor allows a convenient adjustment of the useful height of mercury (a) in order
t o obtain a mobile phase rate of 5 cmlmin.
For a. given column diameter (a) needs only t o calibrated once. Excess of sir flow evacuates very safely by bubbling
through the mercury. T o avoid mercury vapor in the lah, the outlet was connected t o a h w d by rubber tuhing.
The pressure reservoir that is connected to the pressure regulator is a 3-1 flask or tube, wrapped with a safety grill. Once
the whole device is a t the right pressure, it is possible to have a very low air flow which bubbles through the mercury. Two
columns can he connected simultaneously t o the pressure reservoir, if each can be insulated from the device with an ordinary
glass tap.

Air comes on the column by a bent pound-glass joint, firmly attached with rubber hands. The shape of the bottom
of the column and its diameter are identical ta those recommended hv Still. At the too of the column. we added a solvent
reservoir (500 ml for a 4-cm column, 1 I for n 5-rm rolumnl which allows to complete the whole evolution w ~ t h w opening
r
the rolumn. Introduction <,fthe mlwe and the solvent mixture was achieved with a long miled funnel which had n mwtrictpd
end, to avoid pertwhation of the sand surface ( w e msert in figure).

' Still, W. C., Kahn, M., and Mitra, J. J. Olg. Chem.,43,2923 (1979).
A. Feigenbaum
bboratoire de Photochemie
UER Sciences
ERA 688.51082 Reims. France

Volume 61 Number 7 July 1964 649