A Simple Method for Producing Efficient Concentric Tube

Distillation Columns

Sherrel Smith
Texas A & M University, College Station, TX 77843

Comparison of simple and fractional distillation is a com-

mon experiment in organic chemistry laboratories. For sev-
eral years we have been using columns packed with glass
beads for demonstrating fractional distillation. While these
columns performed well, their use had some disadvantages.
They display a relatively large holdup and are quite differ-
ent from the equipment used in the simple distillation. The
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large holdup made it difficult to scale down the pot charge

below 5 to 6 mL. Also, as a more effective teaching tool, we
desire to use the same equipment for both the simple and
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fractional distillation but markedly change the efficiency of

the column in some simple fashion for the fractional distilla-
tion. The Ace Glass Inc. Hickman-Hinkle spinning band
still serves this purpose fairly well but has some drawbacks. Figure 1. Cross-sectional view of an insert. Dimensions are in inches.
The spinning band would seem to be excessively expensive
when used for only one experiment. Also we have experi-
enced some difficulty in operating these units with the heat-
ing mantles that we use in our laboratories. The use of the
heating mantle interferes with the spinning of the band.
These disadvantages were overcome by converting the Hick-
man-Hinkle column to a concentric tube column. This was
accomplished by machining a plastic insert to serve as the
inner tube of a concentric tube column. We have used Delrin,
UHMW polyethylene, and Kel-F for this purpose. These
materials are suitable for a wide range of temperatures and
distillates. The use of Kel-F for the insert provides the best
chemical compatibility but is much more expensive than the
other two plastics. The construction of these inserts is shown
in Figures 1,2, and 3. They are machined to provide approxi-
mately 0.03 in. clearance between the wall of the column and Figure 2. End view of top of insert showing slots for vapor and liquid passage.
Dotted line indicates positioning ring. Dimensions are in inches.
the insert. To keep the inserts properly positioned in the
columns, rings were machined at the top and bottom of the
inserts. These rings were sized to fit the inside diameter of
the column loosely. Another ring was machined at the top to
hold the insert in the column. Slots were cut in the rings to
allow passage of vapor and liquid. The distillation assembly
with insert is shown in Figure 4. The Hickman-Hinkle distil-
lation heads that we have received from Ace have shown
slight variation in length and inside diameter. The dimen-
sions shown for the inserts provided a reasonable fit for most
of the heads. Air condensers and Liebig condensers have also
been converted to efficient fractionating columns by ma-
chining an appropriate insert for them. A 14/20 condenser,
with the water jacket evacuated, sealed, and fitted with an
insert, had an effective column length of 18 cm. This column Figure 3. End view of bottom of insert. Most of the positioning ring is cut away
produced 16 theoretical plates when operated with a distilla- to allow vapor and liquid passage.
tion head that allowed reflux ratio adjustment.

Experimental
Comparisons of separation efficiencies were made using two test
mixtures. Both mixtures were made up 50/50 by volume. The first
mixture was hexane/heptane, which has a boiling point difference of
29 °C. The second mixture was 2-methylpentane/cyclohexane with
a 20 °C difference in boiling point. Distillations were performed
using 2 mL of the test mixtures in conical vials equipped with the
Hickman-Hinkle head. Heating was provided by a sand bath that
was maintained at the same heat setting throughout the study. This
provided essentially the same boilup rate for all distillations. Ap-
proximately 0.1-0.2-mL fractions were collected with Pasteur pi-
pets from the well of the Hickman-Hinkle still. Composition of the

616 Journal of Chemical Education

fractions were determined by gas chromatography using Vg-in. X 5-ft of the mixtures. Analysis of later fractions showed little change in
columns packed with 8% Superox 20 on 80-100 mesh Chromosorb P- composition until a fairly significant portion of the pot charge had
AW. The chromatography was performed with a Perkin Elmer 8410 been distilled.
gas chromatograph. The results reported are the raw peak area
percents as determined by the GC integrator. While these values are
not true weight percentages, they are adequate for comparisons Results of Distlltallons with the Hlckman-Hlnkle Still
between the different setups. The values reported are for the first
fractions collected of 0.1-0.2-mL volume. distillation hexane bp 69 2-methylpentane bp 60,3
Spinning band columns can provide about twice the efficiency mixture3 heptane bp 98 cyclohexane bp 80,7
that concentric tube columns can produce. However, since the insert
utilizes the full length of the tube in the distillation head, it pro- no insert 82.3b,c 67.5
duces essentially the same resolution as the spinning band provided Delrin 97.4 98.0
by Ace Glass, which uses only about half of the total tube length. Kel-F 97.2 94.8
The table shows a comparison of distillation results using the Hick- HMWPE 95.0 93.4
man-Hinkle still by itself, with a spinning band, or with the inserts. spinning-band 98.8 94.2
The results shown are for the first fraction collected. Since it is very 3
The test mixtures were made up 50/50 by volume.
difficult to duplicate collection volumes with the Hickman still, the b The
results shown are for the first fraction with a volume of M).1 mL.
results cannot be rigorously compared. However, both spinning c
The values are the area percents of the lower boiling component as reported by the
band and inserts consistently demonstrated high resolution for both integrator.

Volume 68 Number 7 July 1991 617