An Inexpensive, Foolproof Apparatus for Flash Chromatography

Wayne J. Thompson and Bryan A. Hanson

University of California at Los Angeles. Los Angeles. CA 90024

Liauid chromatoaraphv using Silica Gel@adsorbent has glass joints which can be frozen,since the adapter is affixed to the
hecome an indispensable research tool in organic rhemistry. column using O-ring seal joints. We recommend 20-mm O-ring
Ilntortunately, the time required for preparation of the col- seal joints for this pupae. These joints are usually supplied with
a Vitona ring seal and are available for nearly the same cost as
umn, search for an appropriate solvent, collection of fractions, standard taper 24/40 ground glass joints.
and isolation uf r~roducts.
generally. .
prohit~itsits useasan ed- (3) When loading the column,the worker simply removes the plastic
ucational tool. stopper and inserts a long-stem funnel that has been modified
Recentlv, a higblv convenient method of "flash chroma- at the end as shown in the figure. The material to be chromato-
tography"whichtakes much less time for operation was re- 7 ~. is dissolved in a few ml of solvent and then ooured into
ersohed
ported bv Still, Kabn, and Mitra? Consistent with these au- lhc funnrl at a ronwnient rare. 11 WII ntmmdl~rallyrun down
thors' observations, we have found that once a solvent system the wnllofthecdumn ontothe brd of Sil~roC.d*.Th~funnelrrln
has been selected, samples in the 0.01 to 10 g range can be then he- used fur 1mdin.g the chnm~aro~rsphy sulwnt wnhout
purified in about 30 min. Since this method is potentially concern about disturbing the Silica Gel".
useful in any research investigation where pure organic All other details of operation are essentially the same as
compounds are required, we sought to incorporate it into our described by Still e t al: Since the actual time required for
undergraduate laboratory curriculum as a practical, routine elution of the products is eenerallv less than 15 min, we have
method of -~urification.Our own exoerience. however. with
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found that one adapter isiufficieit for several workers, thus
the apparatus described by Still e t ai. revealed certainoper- ..
reducine the overall cost of the apparatus of an instructional
ational difficulties which we felt had to be overcome before . laboratory scale.
it would be suitable for use by inexperienced undergraduate T h e advantages of this new apparatus combined with the
students. These technical flaws are functional virtues of "flash ch;omatography" make this
technique an attractive addition to any undergraduate labo-
(1) The nitrogen inlet adapter had to be removed for loading the
column with either sample or eluant. Occasionally,this operation ratory course.
resulted in breakage or jamming of the adapter in the column.
( 2 ) Loading the column properly without disturbing the Silica Gel"
hed eenerallv reauired a fair amount of experience or practice on
the partof ihe worker.
(5) The use of defective rubber bands or springs for holding the
adapter to the top of the column andlor asudden rise in pressure
often resulted in the adapter joint's becoming hopelessly frozen
in thecolumn. When this happened, theexperiment,thecolumn,
andlor the adapter had to be sacrificed.
- - -
We describe here a new. modified "flash chromatomaphv"
apparatus which overcomks these difficulties and is suitable
for use as an instructional tool in an undereraduate laboratow
course. The main features of this new design are
( 1 ) An expensive Teflon' pressure valve is not necessary. The pres-
sure can be conveniently controlled using a commercial needle
valve connected to the stopcock on the adapter using Tygon'
tubing. For compounds insensitive to oxidation, the laboratory
air line can be used for pressurizing the column. Once in the col-
umn, the sample can be loaded onto the Silica GeP without re-
moving the adapter by holding the plastic stopper in the adapter
wlth one hand and pressurizing the column by opening the
stopcock.
(2) If a sudden rise in pressure should take place, the plastic stopper
in the top of the adapter is ejected as a harmless, unbreakable
projectile. Should the stopper become jammed in the joint, it can
he removed easily with a pair of pliers. There are no other ground
Details of the mcdified apparatus. A, 24/40 plastic stopper: 8. 24/40 oufer joint;
C. 2-mm stopcock;D, downwadfacingears (one on each side);E. 2 0 m m &ring
seal joint: F, top of column: G. 20-mm Vitona ˚(H, No. 35 clamp, not
I Still, W. C., Kahn, M., Mitra, A,, J. Org. Chem., 43,2923 (1978). shown): (I, rubber band, not shown);J. modified funnel; K. 4-mm round hole.

Volume 61 Number 7 July 1984 645