Simple distillation is a deceptive name. This week I conducted a demonstration of a
simple distillation for my honors class as part of the Foul Water Lab from the
ChemComm curriculum. (I don’t use
ChemComm, but I like this lab from the book.)
I used Demo 9.10 Separating Liquids: Fraction Distillation found
in volume 3 of Shakhashiri’s Chemical
Demonstrations, A Handbook for Teachers of Chemistry as a reference for the
set-up and discussion.
Here's the simple distillation apparatus.
The distillation demo was the final step in a water
purification lab conducted by my Honors students. They were challenged to purify a water sample
that contained oil, coffee grounds, garlic powder, and salt. I used the “Foul Water Lab”, which is an
excellent introduction to separating mixtures, chemistry lab techniques, and
the physical properties of matter. The
students did a series of purification steps:
separating the oil from the water, sand/gravel filtration to remove
large particles, charcoal absorption to remove odors, and a distillation to
remove the salt (and the rest of the impurities that they didn’t get out
before). I conducted the final step of
the experiment as my demo this week because my lab tables don’t have sinks (very
annoying) and we don’t have enough condensers (they are useless without sinks,
by the way).
My colleague suggested that I distill Cherry Coke first to
introduce the technique, something I had never tried. This was a lot of fun because the kids always
love testing something they might actually eat or drink. I decided to set up the apparatus during
class (some of the groups were still finishing up the filtration, so half the
class had some down time). Most of the
students had never seen a distillation.
I handed the tubing to a couple of boys and asked them to connect it for
me, while I attached clamps to ring stands.
I asked for more helpers to hold the round bottom flask and condenser in
place while I clamped it all together.
The set-up was a distant cousin to the fractional distillation apparatus
in my college organic chem lab, with glassware that all fits together and bars
in the back of the hood for clamps. After
a lot of adjusting, I managed to assemble the apparatus with the Coke in the
flask, when I realized that I had forgotten to add the boiling chips. So I loosened some clamps, lowered the round
bottom flask, added the boiling stones, and manipulated the apparatus back
together. My students watched, gathered
around the front bench, a few lending a hand to help me steady everything as I
readjusted. At the same time I explained
how the system works to separate liquids with different boiling points. Finally we were ready to light the Bunsen
burner. (As a side note, the first time
they see me light the burner is a big deal every year. Soon enough the magic is gone and this
becomes just part of the regular lab routine.)
The first thing we observed was rapid bubbling as we watched
the carbon dioxide leaving the solution.
I bubbled the gas through limewater to confirm the presence of CO2,
another suggestion from my colleague.
Very cool so far. Then we started
collecting a liquid. I wish that I had remembered
to put a thermometer in the flask to note the boiling point of the distillate,
but I didn’t think about that until it was too late. It’s been a really long time since I’ve done
a distillation. It all started coming
back to me as we were boiling the Coke. Maybe
I should have spent a little longer reading Shakhashiri, because a thermometer is
clearly labeled in the diagram! We
collected a clear, colorless liquid form of the cherry/vanilla flavoring. The strong odor of cherry coke was
overpowering in the small sample we collected.
The second liquid we collected was also clear and colorless with a faint
smell of cherry coke; this time I think we collected water with a small amount
flavoring contaminate. After we had
about 100 mL of distillate, I removed the pot and let the students observe the
smell of the liquid left behind, flat and flavorless Coke. They enthusiastically passed around the three
samples and commented on their odor and color.
Distilling the foul water sample, the last step in the purification lab.
Next we distilled their foul water samples. I combined several groups’ samples into the
pot because we were only going to do this once.
The brownish, electrically conductive water sample in the pot started to
boil vigorously as the bell rang ending the period. No! My
kingdom for 20 more minutes. We were
already collecting distillate, so I decided to let it continue to distill after
the period ended. I saved the purified
water sample into an Erlenmeyer flask and saved the remaining pot liquid. During the next class period, I was a bit
nervous to test the conductivity of the solution. What if it didn’t work? How would we explain the presence of salt in
our purified sample? I decided to let
the anticipation build by showing the class a control test of the conductivity
of distilled water (no light) and salt water (bright light). We were all pumped up when the light did not
come on when we submerged the electrodes in our purified water. The only
disappointment was the lingering garlic odor in our water sample. The purification would have been better with
a fractional distillation set-up rather than a simple distillation (a second
condenser above the pot makes all the difference), possibly separating out the
organic substance in the solution responsible for the lingering odor. However, we did the job we set out to
accomplish; the salt was definitely gone from the final product.
Compare the sample of untreated foul water to our purified sample. Looks nice, but don't smell it!
Here's the distillate we collected and the liquid that was left in the pot at the end of the distillation.